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S10200089 DruAtvo jedrskih strokovnjakov Slovenije / X Nuclear Society of Slovenia X International Conference Nuclear Energy in Central Europe'99 Proceedings Volume 2 Embedded Meeting Neutron Imaging Methods to Detect Defects in Matericls Portoroz, Slovenia f1a, A31 A '0 6 to 9 September, 1999

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Page 1: International Conference Nuclear Energy in Central Europe'99 ......CIP -Katalozni zapis o publikaciji Narodna in univerzitetna knjilnica, Ljubljana 621.039(4-014)(063)(082) NUCLEAR

S10200089

DruAtvo jedrskih strokovnjakov Slovenije / X

Nuclear Society of Slovenia X

International ConferenceNuclear Energy in

Central Europe'99

ProceedingsVolume 2

Embedded Meeting

Neutron Imaging Methods toDetect Defects in Matericls

Portoroz, Sloveniaf1a, A31 A '0 6 to 9 September, 1999

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CIP - Katalozni zapis o publikacijiNarodna in univerzitetna knjilnica, Ljubljana

621.039(4-014)(063)(082)

NUCLEAR energy in Central Europe '99: international conference,Portorol, Slovenia, 6 to 9 September, 1999: proceedings /[organisation] Nuclear Society of Slovenia; [editors Oton Gortnarand Andrej Stritar]. - Ljubljana: Nuclear Society of Slovenia,1999

ISBN 961-6207-13-X1. Gortnar, Oton 2. Dru~tvo jedrskih strokovnjakov Slovenije. - 1.Nuclear Society of Slovenia glej Drustvo jedrskih strokovnjakovSlovenije105053696

For the symbol of this meeting we have chosen a drawing of a wind pump in old saltworks close to Portoroi.This is an old technical device, much more primitive than the technology we are dealing with today. However, itis a symbol of human inventions that are simplifying our life.

The museum of salt-making is located in the formerly used salt-pans to the right of the Giassi channel close toSedovlje. The museum is comprised of a salt-maker's dwelling with a collection of artifacts, and salt-pans nearthe Giassi channel, supplying fresh seawater.

Editors:Oton Gortnar and Andrej Stritar

The contents of papers published in this book is the responsibility of the authors concerned, organisersare not responsible for the facts published and the technical accuracy of the data presented. All thepapers were peer-reviewed by at least two reviewers. However, final texts in this volume were setindividually by authors.

Meetings organised by Nuclear Society of Slovenia:

* First Meeting of Nuclear Society of Slovenia, Bovec, Slovenia, June 1992

* Regional Meeting: Nuclear Energy in Central Europe, Present and Perspectives, Portoroi,Slovenia, June 1993

* PSA-PRA and Severe Accidents '94, Ljubljana, Slovenia, April 1994

* Annual Meeting of NSS '94, Rogaska Slatina, Slovenia, September 1994

* 2nd Regional Meeting: Nuclear Energy in Central Europe, Portoroi, Slovenia, September 1995

* 3rd Regional Meeting: Nuclear Energy in Central Europe, Portoro2, Slovenia, September 1996

* 4th Regional Meeting: Nuclear Energy in Central Europe, Bled, Slovenia, September 1997

* Nuclear Energy in Central Europe '98, Catel, Slovenia, September 1998

II International Conference Nuclear Energy in Central Europe '99

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ORGANISATION

Nuclear Society of SloveniaJamova 39, SI-1000 Ljubljana, Slovenia

E-mail: nss(~iis.siTel.: + 386 61 1885 450Fax: + 386 61 161 22 76

SPONSORS

European Nuclear SocietyMinistry of Science and Technology of Slovenia

Ministry of Economic Affairs of SloveniaInstitute "Joief Stefan"

Slovenian Nuclear Safety AdministrationAgency for Radwaste Management

ENCONET Consulting GmbH, ViennaSIAP d.o.o., Pesnica pri Mariboru

S-NET, Internet Provider

International Conference Nuclear Energy in Central Europe '99

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PROGRAM COMMITTEE

Andrej Stritar, Slovenia, Chair

Pavel Balai, Slovakia Irena Mele, SloveniaHelmut Bock, Austria Martin Novsak, Slovenia

Teodor ChiricA, Romania Stojan Petelin, SloveniaLeon Cizelj, Slovenia Dubravko Pevec, Croatia

Francesco D'Auria, Italy Joze Rant, Slovenia

Milorad Dusic, lAEA Matjai Ravnik, Slovenia

Danilo Feretic, Croatia Stane Rozman, SloveniaBogdan Glumac, Slovenia ZoltAn Szonyi, Hungary

Miroslav Gregoric, Slovenia Joze Spiler, Slovenia

Carolyn D. Heising, USA Bojan Tomic, Austria

Silviu-Aurel Idita, Romania Andrej Trkov, SloveniaAlojz Franc Kodre, Slovenia Wolfgang Volkenbom, Germany

Jure Marn, Slovenia Marko Cepin, Slovenia, Young GenerationBorut Mavko, Slovenia Network

Organising Committee of the Embedded Meeting onNeutron Imaging Methods to Detect Defects in Materials

Joze Rant, Slovenia Piero Chirco, Italy

Marton Balasko, Hungary Helmut Rauch, Austria

AWARD COMMITTEE

Andrej Likar, Slovenia, Chair

Jirgen Knorr, Germany Nikola Cavlina, Croatia

ORGANISING COMMITTEE

Oton Gortnar Tomaz SkobeLeon Cizelj Ivan SpilerIgor Jencic

http://www2.i js.si/-ic jt/dis/port99/

IV International Conference Nuclear Energy in Central Europe '99

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FOREWORD

The International Conference Nuclear Energy in Central Europe '99 was held inPortoroz, Slovenia, from 6th to 90 September 1999. This was the sixth international meetingentitled "Nuclear Energy in Central Europe" and organized by Nuclear Society of Slovenia.The event had already been recognized as a traditional yearly meeting of European nuclearprofessionals in which several hundred experts participated since the year 1993.

The meeting in Portoro2 aimed to connect the Central European nuclear community justbefore entering the third millennium. This is the region of Europe, where new nuclear powerplants are still being put into operation (Mochovce, Cernavoda). This was the reason for theslogan printed also on the cover of these Proceedings: Expanding nuclear capacity in theregion.

Special attention was devoted to the exchange of operational experiences between CentralEuropean nuclear power plants. 147 participants from 18 countries attended the conferenceand 109 papers were presented in two parallel sessions and a poster session. Introductoryspeech was given by Pat Upson, president of the European Nuclear Society. Each of the threeworking days started with plenary session intended for invited lectures.

The conference has also hosted the meeting Neutron Imaging Methods to DetectDefects in Materials, which was organized in the frame of the project EC COST 524, andthe meeting of the European Neutron Radiography Working Group.

Call for papers for the conference was issued at the end of the year 1998. Papers werecollected by May 1999. Program Committee held a meeting in June and determined the finalprogram of the conference. Due to the very large number of submitted papers the conferencewas run with two sessions in parallel and with additional poster session.

Award was given for the best contribution prepared by first author aged no more than 32years. An international award committee has reviewed papers and awarded Ms. Elke Pichl(Austria) for presenting the paper "Siemens Argonaut-Reactor Graz: A Method to Determinethe Bum-up of Fuel Elements".

During the conference every paper was peer-reviewed by at least two reviewers. Finally, afterthe conference, authors had to submit final, camera-ready papers, which are printed in theseProceedings. Final number of printed papers is exactly 100.

Due to the large number of papers these Proceedings are printed in two volumes. Volume 1 isthicker, containing almost 700 pages, while Volume 2 contains about 110 pages and isentirely devoted to the embedded meeting Neutron Imaging Methods to Detect Defects inMaterials. Table of Contents and Index of Authors are identical in both volumes.

Dr. Andrej StritarProgram Committee Chairman

International Conference Nuclear Energy in Central Europe '99 v

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Table of Contents

TABLE OF CONTENTS

Volume 1

Invited Lectures . ............................................ 1

Assuring Nuclear Energy's Future through International Co-operationPat Upson ................................................................. 3

Mochovce NPP Unit 1&2 Completion ProjectJaroslav Holubec ................................................................. 9

Current and Future Neutron Radiography StandardsJack Brenizer ................................................................. 17

Harmonisation of Slovenian Nuclear Legislation with EUMiroslav Gregoricn ................................................................. 25

Krsko Modernization ProjectStane Rokman ................................................................. 33

Reactor Physics .............................................. 47

The Integrated Code System CASCADE-3D for Advanced Core Design and SafetyAnalysisAlfred Neufert, Antoine Van de Velde ................... .............................................. 49

Definition of Pseudo Fission Product Data for Reactor CalculationsAndrej Trkov, D. Aldama ................................................................. 57

Radiation Dose Rates in the Vicinity of the NPP Krsko Spent Fuel PoolMile Bace, Dubravko Pevec, Kregimir Trontl ............................................ ..................... 63

Power Feedback Effects in the LEM CodeMarjan Kromar .................................................................. 69

Validation of SCALE Code Package on High Performance Neutron ShieldsMile Baie, Radomir Jejmenica, Tomislav Smuc ................................................................. 75

The Energy Released by Neutron Capture in Thermal ReactorsAndreja PerWic, Andrej Trkov ................................................................................................. 83

Analysis of TRIGA Reactor Thermal Power Calibration MethodToma Zagar. Matia± Ravnik, Andreja Per ..ic. 91

Research Reactors .99

Development of a New Safeguards Method for Research ReactorsUwe Filges, Alexander Ellinger, Jfirgen Knorr .. 101

Neutron Beam Utilization at the TRIGA Mark II Reactor ViennaMario Villa, M Baron, G. Badurek, Helmut Bock, R. Buchelt, M Hainbuchner, S. Ismail,Sonja Korner .. 105

International Conference Nuclear Energy in Central Europe '99 V1I

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Table ofContents

Siemens Argonaut-Reactor Graz: A Method to Determine the Burn-up of FuelElementsElke Pichl, Waldemar Ninaus ....................................................................... 13

Fast Neutron Fluence Monitoring in the Exposure Channel F19 of the TRIGA MARK IIReactor in LjubljanaEdvard Krigof ....................................................................... 121

Neutron Measurements at the TRIGA Reactor Ljubljana for Core Inventory VerificationUwe Filges, Alexander Ellinger, Jurgen Knorr, Maojaz Ravnik, Robert Jeraj, Tomai Zagar,Radojko Jacimovic ....................................................................... 129

Upgrading the Siemens ARGONAUT Reactor Graz with a Digital Monitoring System0. Frohlich, Waldemar Ninaus .................... .................................................... 137

SSR TRIGA 14 MW Thermal Hydraulic AnalysisGheorghe Negut, Mladin Mirel .................... .................................................... 145

Thermal Hydraulics ............................................... 151

Reanalysis of Some Key Tranzients with MAAP Code for Krsko NPP after SGReplacement and Power UprateBozidar Krajnc, Bruno Glaser, Ivica Bagi6, Martin Novgak, Joze Spiler ............ ......................... 153

NPP Krsko Natural Circulation Performance EvaluationVelimir Segon, Tomislav Bajs, Nenad Debrecin ....................................................................... 161

Analytical Verification of the Cool-Down Procedure in the WWER-440/213 ReactorVessel Head under Natural CirculationJan Szczurek, Piotr Marks, Peter MikloviJ ....................................................................... 169

Modeling of Subcooled Boiling in the Vertical FlowBostjan Koncar, Borut Mavko ................... .................................................... 177

Response Surface Use in Safety AnalysesAndrej Prosek ....................................................................... 185

Modelling of the Rod Control System in the Coupled Code RELAP5-Quabox/CubboxVesna Bencik, Dani/o Feretic, Davor Grgic ....................................................................... 193

Simulation of the Instability in the Stratified Two-Fluid SystemGregor Cerne, Stojan Petelin, Iztok Tiselj ........................................................................ 201

On Counterflow (Reflux) Modelling using MELCOR and FIDAPJure Marn, Marjan Delic, Zoran Zunic . ........................................................................ 209

RELAP5 Analysis of Subcooled Boiling Appearance and Disappearance in DownwardFlowRisto Ristevski, Iztok Parzer, Dusan Spasojevi6 ................................... 2......1.......... .. 217

Influence of the Upper Head Nodalization on the "BETHSY" 6.2 TC TestStojan Petelin, Boltian Koncar, Samo Hrvatin ...................................................................... 225

A Combined Single-Multiphase Flow Formulation of the Premixing Phase Using theLevel Set MethodMatjaz Leskovar, Jure Marn ...................... 233

VIII International Conference Nuclear Energy in Central Europe '99

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Table of Contents

Structural Analysis .............................................. 2 41Can We Simulate the Development of ODSCC Defects in Steam Generator Tubes?Leon CizelO, Marko Kovaj, Tomaz Dvorek . .................................................................. 243

Piping Reliability Improvement through Passive Seismic SupportsRobert Baltus, Antoine Rubbers ................................................................. 251

Numerical Analysis of Interacting Cracks in Biaxial Stress FieldMarko Kovae, Leon Cizelj ............. ............................. . ...................... 259

About Criteria of Inadmissible Embrittlement of Zirconium Fuel Cladding duringLOCA in the PWRsVitaly Osmachkin ................................................................. 267

Flaw Evaluation ChartsDarko Korogec, Jelena Vojvodic Tuma ....................... .......................................... 273

Probabilistic Safety Analysis . .................................... 279

Integrated Use of PRIMAVERA and ORAM Codes in Outage 1999 at NPP KrskoJanez Krajnc, Franc gkaler, Ivica Basic, Roman Ko(cnar .......................................................... 281

Deterministic and Probabilistic Methods to Assess the Safety Level of OperatingNuclear Power PlantsHeinz Berg ........................................... . .................... 289

A Risk-Informed Approach to Optimising In-Service Inspection of PipingAnthony Billington, Philippe Monette ...................... ............................................ 297

A New Approach for Estimation of Component Failure RateRomana Jordan Cizelj, Ivo Kljenak .................. ............................................... 305

Probabilistic Analysis of Allowed Outage TimeMarko Cepin ................................................................. 313

Severe Accidents .............................................. 321

Modeling of Hydrogen Stratification in a Pressurized Water Reactor Containment withthe CONTAIN Computer CodeIvo Kijenak, Alja LSkerlavaj, Iztok Parzer ............................... 323

Plant Specific Severe Accident Management - the Implementation PhaseRobert Prior ........ 331...................... 331

USA Experiences in Conducting and Implementing the Protective Measures in a Case ofthe Nuclear Accident and their Possible ImplementationInes Ana Jurkovi6 .............................. 339

Modeling of Krgko NPP Engineered Safety Features with MELCORMarjan Delkc, Jure Marn .............................. 347

Modeling of Aerosol Condensation and Evaporation during a Severe Accident with theCONTAIN Computer CodeA ljaz Skerlavaj, Ivo Kijenak, Iztok Parzer .............................. 355

International Conference Nuclear Energy in Central Europe '99 1X

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Table of Contents

Role of the Exercises in the Training of the Technical Support Center Members inCroatiaInes Ana Jurkovic, Davor Grgic, Dejan Skanata ..................................................................... 363

NPP Operation ............................................... 371

Outages 1999 and 2000, Investments in Safety and Long-Term Operation of NE KrskoPredrag Sirola, Janez Krajnc. Ferdo Androjna ..................................................................... 373

Backfitting of Nuclear Power Plant Bohunice V1 in SlovakiaMilan Ferenc ..................................................................... 381

The NPPRI Trnava Participation in the NPP V-2 Modernization and SafetyImprovement ProjectVladimir Michal, Blaiej Logonsky, JozefMagdolen ................................................................. 389

Status of Siemens Steam Generator Design and Measures to Assure ContinuousLong-Term Reliable OperationGfinterHoch ..................................................................... 397

Steam Generator Replacement Project in 2000Janko Cerjak, Richard Holz, Jorg Haus, Christian Gloaguen ...................... .............................. 407

Mochovce NPP Experience in the Certification and the Use of Full Scope SimulatorLubomir Krenicky ..................................................................... 415

Diagnosis Methods Based on Noise Analysis at Cernavoda NPP, RomaniaConstantin Bdnica, Dumitru Dobrea ......................... ............................................ 423

Safety Upgrading Program in NPP MochoveePavol Baumeister ..................................................................... 431

Probabilistic Determination of Neutronic Trip Setpoints at Cernavoda NPP, RomaniaConstantin Banicd ...................................................................... 439

NEK Containment Integrated Leak Rate Test at Full PressureFranc Skaler, Vinko Planine. Dam/an Gregoric, Darko Cievarij ................. .............................. 445

Implementation of Motor Operated Valves (MOV) Program in NE KrskoVladimir Butkovi6, Janko Cerjak, 2eljko Mide, Marko Nikolic, MatoaS Prah .......... ..................... 453

Implementation of Procedures to NPP Krgko INTRANEKDun/a Gradisar, Marjetka Kran jc, Roman Koinar, Jozie Spiler ................... .............................. 461

Nuclear Energy and Public ........................................ 465

Legislation in Hungary, Implementation of the Act on Atomic EnergyZoltan Szonyi .................................................................... 467

Configuration Management at NEKMarijan Podhraski ..................................................................... 475

Physical Protection of Nuclear Facilities and Materials, Safeguards and the Role of theIAEA in Physical ProtectionMiroslav Smolej .................................................................. 483

X International Conference Nuclear Energy in Central Europe '99

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Table of Contents

Cernavoda - Unit 2: A Strategic Project for RomaniaJohn Saroudis, Teodor Chirica, Giovanni Villabruna ............................................................... 491

Future of Nuclear Power is PromisingAndrej Stritar ............................................................... 497

New Devices for Better Understanding of Radioactive Waste by General PublicAndrej Stritar, Oton Gortnar, Jelislav Kovacdid, Matjai Kofelj, Irena Mele,Nadja Zeleznik .............................................................. 505

Public Opinion About Nuclear Energy - 1999 PollAndrej Stritar, Radko Istenic .............................................................. 511

Radioactive Waste .......................................... 519

PAISA for Slovenian LILW RepositoryNadja 2eleznik, Irena Mele .............................................................. 521

Croatian Repository Construction Project - Present Status & Main ObstaclesSavka Kujar-Dragitjevic, Damir Subasic, Antun Schaller, V. Lolner,Mirjana Cergkov-Klika .............................................................. 529

Tunnel Type Radioactive Waste Repository Performance AssessmentDejan Skanata, Davor ginka, Saga Medakovic ..................................... ......................... 535

Reassuring the PublicNadja Zeleznik, Irena Mele ............................................................... 543

Radiological Protection and Environmental Issues ............... 547

Strengthening ALARA Approach in Work Management at Krsko NPPBorut Brezuik, keljko Kovae, Predrag Sirola ................................ .............................. 549

Environmental Monitoring Program at Cernavoda Nuclear Power Plant, EnvironmentalRadiation Monitoring Data for Cernavoda NPP March 1996 to December 1998Elena Bobric, Vasile Si~nionov ......................................... ,.,,.,,.,.....,,,,.,.,,.,,,.,.555

The Chernobyl NPP Accident: Social and Psychological Rehabilitation of thePopulationOlga Joukovskaia, Igor Rolevich .......................... 563

Activity Levels of Cs 137 and K 40 in the Skin and the Associated Structures of a CowFollowing the Chernobyl AccidentElke Pichl, H. Rabitsch .......................... 569

Future Needs in Radiation Protection Training for NPP Workers in SloveniaMaijaS Kozelj, Terezija Bogovcii .......................... 5/5

Nuclear Methods ................ 583

Ion Beam Analysis (IBA) at J. Stefan InstituteMilog Budnar, M Kavcii5, A. Mahleisen, Primoz Pelicon, A. Razpet, J SimciC,Benjamin Zorko, kiga 9mit. Matjai Zitnik ................... ....................................... 585

International Conference Nuclear Energy in Central Europe '99 XI

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Table of Contents

Characterization of Thin Films and Surfaces by Ion-Beam Analytical TechniquesPrimoz Pelicon, Milog Budnar, Benjamin Zorko, A. Razpet .................... .............................. 595

The Effect of, within the Sphere Confined, Particle Diffusion on the Line Shape ofIncoherent Cold Neutron Scattering SpectraBruno Cvikl, UfDahlborg, Monique Calvo-Dahlborg ............................................................. 603

Collector Floating Potentials in a Discharge PlasmaMilan Cerciek, Tomai Gyergyek .................. ................................................... 611

Time Development of the Electron Distribution Function after the Application of aPositive Voltage Step to an Electrode Immersed in a Weakly Magnetized DischargePlasma ColumnTomai Gyergyek, Milan 6er6ek .................. ................................................... 619

Monte Carlo and Deterministic Transport Calculations ......... 627Sensitivity Studies of the TRIGA Benchmark Critical ExperimentRobert Jeraj, Andreja Pergij, Toma.V Zagar, Matai Ravnik ........................ .............................. 629

Cross-Section Data Uncertainty and How Such Information is Used in Fusion AnalysisIvan Kodeli ...................................................................... 637

Simulation of the Si-Ball and the RoSiB Silicon Detector ArraysSaleh Ashrafi, Matej Lipoglavsek, Andrej Likar, J. Nyberg, A. AxeIsson, H. Grawe,Tim Vidmar, R Schwengner ..................................................................... 645

Simulation of the TRIGA MARK H Benchmark Experiment with Burned FuelTomai 2 agar, Andreja Pergid, Robert Jeraj, Matjaz Ravnik ........................ .............................. 651

Using Vega Linux Cluster at Reactor Physics DepartmentBojan Zefran, Robert Jeraj, Jure Skvarcj Bogdan Glumac ............................ ............................ 659

Determination of the Neutron Flux Characteristics and Personal Dose Equivalents inthe Thermal Column of the SAR-GrazIgor Koprivnikar, Waldemar Ninaus, Ewald Schachinger ................................ ......................... 665

Validity Test of the n-Particle Transport Code MCNP 4B in the Low Neutron EnergyRegionIgor Koprivnikar, Walde mar Ninaus, Ewald Schachinger ................................................ ........ 673

Index of Authors ................................................................................................................ 681

Volume 2

Neutron Imaging Methods (Embedded Meeting) ................ 685Image Quality: Signals and Information (Invited Lecture)Hisao Kobayashi .......................................................... 687

Neutron Diffraction Studies for the Measurement of Strains and StressesGerard Swallowe, R. Wimpory .......................................................... 695

XIl International Conference Nuclear Energy in Central Europe '99

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Table of Contents

Investigation of Microporosity in Die-cast A1Sil2(Cu) Alloys by Neutron- and X-rayRadiographyZsolt Szalay, Mirton Balask6 . ...................................................................... 703

Application of 10B Entrapped PEG-Liposome to Boron Neutron-Capture Therapy forPancreatic Cancer Model In VivoHirinobu Yanagie, K. Maruyama. T Takizawa, 0. Ishida, K. Ogura, T Matsumoto, Y. Sakurai,7 Kobayashi, K Ono, Joze Rant, Jure Skvarc, Radomir Ii6, A. Shinohara, M Chiba. MEriguchi, Hisao Kobayashi ........................................................................ 709

Fast Neutron Radiography Using Photoluminescent Imaging PlatesJo&e Rant, Mdrton BalaskM, Edvard Krigtof, Jfirgen Stade ......................... ............................... 717

Investigation of Perspectives of Fast Neutron Radiography on the Basis ofNon-Traditional Neutron Sources: Neutron Generators with Accelerating and "PlasmaFocus" TubesVitali Mikerov, A. Zhitnik, Ju. Barrnakov, A. Isakov, E. Bogolubov, V. Ryzhkov, T Khasaev,V. Tukarev, A. Ignatcev, V Korneev, A. Pertsov, V. Samarin, Ju. Ivanov, V. Sevrjukov ........ ......... 725

Calibration of Quantitative Neutron Radiography Method for Moisture MeasurementToma2 Nemec, Robert Jeraj ....................................................................... 731

A New CCD-Camera Neutron Radiography Detector at the Atominstitute of theAustrian UniversitiesSonja Korner, Helmut Bock, Helmut Rauch, Eberhard Lehmann ................. .............................. 739

Artefacts of Fast Neutron Radiography Concerned with Neutron ScatteringVitali Mikerov, A. Isakov, A. Koshelev, A. Bykov, V Tukarev, A. Khodeev,W. Waschkowski ........................................................................ 747

Application Fields for Neutron Radiography and Tomography in Industry andTechnological DevelopmentEberhard Lehmann, P. Vontobel, Burkhard Schillinger ............................................................ 755

X-Ray Radiography Inspection of Core Model of the CODEX AIT-2 FacilityMarton Balask6, Z. H6zer. Lasz/6 Mar6ti, P. Windberg ................................ ........................... 763

Performances of some Mobile Neutron Radiography SystemsPierre Bach ....................................................................... 771

Detection of 10B Distributions in Histological Samples by NCAR Using Thermal andCold Neutrons and Photoluminescent Imaging Plates: New ResultsJoze Rant, D. Gabel, GuY Bayon, Hirinobu Yanagie, Hisao Kobayashi,Eberhard Lehnzann, G. Kuehne. Jure Skvarc~, Radomir iW ........................ ............................... 777

Neutron Radiography at the "Institut de Maintenance Aeronautique"Serge Cluzeau ...................... ,,............. 785

Index of Authors ........... 791

International Conference Nuclear Energy in Central Europe '99 XWI

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S10200090Nuclear Energy in Central Europe '99Portoro2, Slovenia, 6 to 9 September, 1999

Invited Lecture

Image Quality: Signals and Information

Hisao KOBAYASHI

Institute forAtomic Energy, Rikkyo University, 2-5-1 Nagasaka, Yokosuka, 240-0101 JapanPhone: +81-468-56-3131, fax: +81-468-56-7576, e-mail: [email protected]

AbstractAmong many parameters relating image quality, neutrons and observed signals prior to

handle observed signals are considered in this report. A relation between signals and theirqualities on neutron images is studied considering on neutron intensity and its statisticalcharacter, effective energy, and characteristics of neutron detection systems. Geometricalparameter of neutron beam is discussed as the other importance to characterize image quality.

1. IntroductionSince 1965, several texts, handbooks, and monographs have been published in fields of neutron

radiography [1-4]. Principal bases are described and it seems to be completed in those literatures.Recently, however, several new technologies have been extensively developed and their capabilitieswere advanced in many fields such as converters, detection systems, electronics, and relatedperipherals. In addition, variety of neutron sources were also installed and newly constructed forneutron radiography in world. Those advanced tools and facilities were reported in many papers andProceedings mainly such as this series of World Conferences, another series of Topical Meetings, andWorkshops on neutron radiography [5-12].Those advanced technologies became to be able to applied in variety of research and industrial fieldssuch as dynamic analyses of liquid, particles and heat flow phenomena, architectural and geo-technicalfields, biological and medical fields, and industrial applications for measurements and inspections aswell. As results of recent development, potentialities of quantitative analyses are more and moreenhanced in those research and applied fields.

Qualifications of obtained images are especially important to realize such quantitative researchfields relating to statistical fluctuations and to spatial uncertainties. Qualities of neutron beams,characteristics of detection systems are considered mainly in this lecture. Many parameters and manyitems of data processing to be considered in image quality determinations are summarized in Table 1.Items discussed in this lecture are shown as highlighted terms by bold faces in the table.

2. Parameters to Determine Image QualityAn image of neutron radiography includes information as a material thickness and a

transmittance. The transmittance is described mainly by a parameter which equivalent to an integratedvalue of a quantity of linear attenuation coefficient (macroscopic cross section) multiplied bydifferential transmission length. Then the transmittance has a possibility to determine a size and toidentify the material. The obtained image itself of course has a principal information and valuable todetermine shape and size of object.

Many grade of image can be obtained depending on facility and imaging system. In this study,however, two extreme cases are considered. One is the case to seek a condition to get the highestquality of the image and to find its extent. The other is the case to study what is the lowest intensityrequired to extract image information.

International Conference N'uclear Ene&Zy in Central Europe '99 687

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Neutron Imaging Methods to Detect Defects in Materials

Table 1Parameters Relating Image Quality Determination

REQUIREMENT OF THE HIGHEST QUALTY OF IMAGESUAnearity and latitude (number of neutrons versus signal out put)

Linearity: Linear (C-CCD, IP) and non-linear devices (SIT, X-ray film)Range of linearity / Latitude

Signal fluctuationQuantum noise (8n)Electronic noise : Readout noise: white noise(& ) and Shottky noiseInhomogeneous sensitivity : Position dependent sensitivity fluctuations(&)Character of detection system:

Grain noise on film (6g) and inhomogeneity of converter (6d)Relating parameters: Relations of film-converter, camera-converter,

imaging plate-conversion materials, etc.Spatial resolution and deformation of Image

Geometrical uncertainty (U,, 1, LID ) and inherent uncertainty (Us)Geometrical deformation (L ) and system deformations

Transmission characterEffective total macroscopic (EM) cross sectionEffective energy for continuum spectrum

REQUIREMENT OF THE HIGHEST SENSITIVE IMAGINGThe lowest limit of n Intensity

Requirement of data smoothing and edge enhancement (image recognition)Enhancement of sensitivity of imaging device

Sensitizing and single neutron counting

(Notice: Items highlighted by boldface are discussing In this report)

2.1 Requirement of The Highest Quality ImagesRange of Linearity: Figure 1 shows photostimulated luminescent (PSL') signals as a

function of neutron fluence with the most recent results of neutron sensitive imaging plates (NIP). Thefigure is composed by two series of experimental results [13, 14). Neutron beams are extracted fromthe tangential beam port in the TRIGA-II with controlling the reactor power from 100 W to 100 kW.The beam fluxes were also controlled changing the collimator opening D from 2.9 cm-+ (L/D=1 10) forthe first experiments (open circles) [13] and 10 cm-0 (L/D=32) for the second experiment (solidcircles) [14]. Furthermore, the beam intensity was adjusted by using suitable thickness of Pb filters.Systematic differences were found the two series of results. The reason may be due to the fluxmeasurement for the second series of experiment and should be reevaluate in the near future.

The figure proves that the NIP covers the range of linearity at least 7 decades. The highest PSLsignals to be able to memory image information is limited again by the readout system. However, ifafter ten times higher fluence 2 x101 1 n/cm2 was exposed than the upper limit, whole imageinformation was completely reproduced by the repeated readout process [141. The evidence shows theupper limit should be extent at least up to 2 x10l2 n/cm2 namely 8 decades of linearity range.

Traditionally, ranges of linearity were 2.5 decades for almost of detection system such as filmsand converter systems and imaging camera (SIT, II etc.) and converter systems except a cooled CCDcamera and converter system which has five decades of linear range. Anyway, the NIP has the widestlinearity range in the whole available detection systems to date.

' PSL is some time called also as OSL (optically stimulated by luminescence).

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Neutron Imaging Methods to Detect Defects in Materials

1.E+06X P5L: No.081 -501 (BASSOOO: S4000-530000) ___.t_____ii.1a

*PSL:No.1003-1270(BAS2SOO,Sl00-Sl000) _ _T _ . l . _ 11lll

1.E+05

E 1.E+04E

- 1.E+03

0 E0

C)

L 1E+00

11.E-01

1.E+03 11 .+04 1 .E+05 11 .E06 1+07 1 08 1E+09 1M M+1 0 111 1

NUTRON FLUENCE, n/CM 2

Fig.1 PS+Imnir as a function of neutron fluence. Measured by the low sensitivePSL reader BAS2500 (C) [14] and the high sensitive reader BASSOOO (0) [13].

Statistical Character To determine image quality, a character of statistical fluctuation isplay main role on the density signals. Figure 2 shows summary of measured statistical characters forvarious imnaging systems. The upper part of this figure is multiple scales to found fluences fromneutron flux and exposed time intervals. The lower part shows standard deviations for four typicaldetection systems; (1) a unit cell of 0.1 mm square of the Gd2O3 sensitized NIP, (2) a cooled CCDcamera with a fluorescent converter (NRC: 6 LiF+ZnS(Ag)), (3) an image intensifier (II)+NRC, and(4) an industrial X ray film (Kodak SR)+an evaporated metal Gd. For references, standard deviationsof NIP are also summarized for additive three different pixel sizes (0.05 mm, 0.5 mm and 5 mm-squares).

(1) In the results of NIP, the statistical character was confirmed up to 2x109 n/cm2 [13].Unfortunately, the analyses for the most recent results is not finished until now. Then, the datacouldn't given here for the most interesting region higher than 2x109 n/cm2 .

(2) The cooled CCD camera is known as one of sophisticated system. However, three signalfluctuation sources are observed for the used cooled CCD camera (Hamamatsu C3140) [15]. Relativestandard deviation shows linearly decreases on fluence in a low fluence range less than 5x10' n/cm2

and a low signal intensity region. Then, the region tells us that a fluence-independent instrumental-noise is a main source. The second narrow region appears at around region of 108 n/cm2 . The regionobey the statistics of neutrons and have nearly n 12 dependence. After that the constant relativestatistics is observed in the higher fluence region. The region shows the imaging device hasinhomogeneous sensitivity between unit CCD cells on the tip.

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Neutron Imaging Methods to Detect Defects in Materials

EXPOSURE TIME (SEC) -

1000 fps 30 fps for Real Time Imaging

\0' le 10o\ -1l- 100 101 102 103 104 sec

104 u 0 \ - \ UTR-KInki

N

,E10 5 -- _

RUR/N2(L/DM110)X 10- ;-SK_ _.\_.K..........B

107- A <A \ A \ \ <RUR/N2(L/D=30)

JR -3M/T (L/D=150)FLUEUCE (nicm2) >-*

101 102 103 104 105 106 107 108 109 1010 10o 1012 n/cm2

100% - WE-

<:NIP~~~~~ ( 5 mmsur)0N~ al

z

0~~_ ..,. BA oo(:~i~~

x __

Film bGdVi+u DC Sst u Varo E squar

6LiF-Z S(Ag)

different opNIP (5 mm square) o th c e (.e1 statcNP(0.5 mm square). nt ~ur

z ~~~~~NIP (0.1 mm square)NIP (0.05 mmn souare)

cn0. 1 % _

- (S300-100

(S] 000-S IDO)

Fig. 2 Expected Statistical Character in Neutron Radiogram forVarious Detection System under Various Exposure Condition

(3) The measured statistical fluctuation of the film-converter system has similar in shape butdifferent origin of complicated character to the cooled CCD. In this case, the statistical fluctuationmainly consists of a constant noise region, which is due to film granularity of fluence independent fogregion in a low fluence region, and an exponential region due to electronic noise at transmitted photon

2.2 Other Important Parameters on Transmittance MeasurementsNon-Linearity of System Response: The non-linear characteristics is frequently

observed on the film-converter system especially combinations with light emission type converterssuch as an NRC, a sheet of GdOS(Tb) etc., and many electric imaging systems.

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Neutron Imaging Methods to Detect Defects in Materials

Table 2 Measured Scattering Neutron Component [16]

Reactor'/Facility Neutron flux Scattered Comments(Beam quality') n/cm2-s component

JRR-3MtNRF2TIN) 1.5x108 17 - 6 % Non-filteredWRR-3MICNRF(CNIG) 2.3x108 4 ± 2 Guide tube

RUR/N2(TN) 1.5x106 15 ± 5 Non-filteredKUR/E2(CN) 1.2x106 14 Thin Pb filterKUR/CN2(CN/G) l.x1107 4 Guide tubeSAPHIR(IN) 3.5x 105 3 14 Pb + Bi filterHHB8(1N) 3.4x105 *3 9 Si + cooled BiHFR/HB8(CN/F) 2.6x105

*3 7 Cooled (Be + Bi)

* 1 Reactor: JRR-3M: Japan Research Reactor No,3 Modified, JAERI, 20MW.RUR. Rikkyo University Reactor, TRIGA-11, 100kW.KUR Kyoto University Reactor, 5MW.SAPHIR: Light water moderated material test reactor,

Paul Scherrer Institute, Switzerland, 10MW.JIFR: High Flux material testing Reactor, Petten, Netherlands.

*2 Beam Quality: TN: thermal neutron,CNIG: cold neutron with a guide tube,CNIF: cold neutron with cooled filters.

*3 Estimated from a relation between optical film density and exposed fluence measuredat RUR/N2.

Traditionally, the non-linearity is frequently described by a slope y. For y >1 for example a filmwith a light emission type converters, the system is characterized as a narrow latitude system. Thesystem is automatically enhancing the contrast. On the contrary, a wide dynamic range is expected fory <1 system.

Studies to expect quantitative analyses require suitable correction for the non-linear system. Inthe case, a system having y =1 relation is preferable. But, recent detection system have a potentialityeasy to correct those non-linear relations if the image data are stored in a memory of a personalcomputer.

In fact, the IP has wide range of linearity, then the IP readers usually analyze 4 or 5 decades ofsignals. In the case, measured PSL signals are compressed to a data length of 16 bit after a logarithmtransformation. Therefor, the compressed data must be retransformed to linear relation.

Collection of Background Component: It is well known that the measured signalsinevitably include components of scattered neutrons and gamma ray background and sometimeinclude instrumental offset signals. A 20 % of background components are sometime observed.Measured scattered components are summarized for some neutron beams including outputs of coldneutron guide tubes in Table 2 [16]. A few correction methods have been reported to correct thebackground component. The Cd shadow method [17] is one of practically useful technique. Recently,some materials such as hydrogen rich objects is expected to include a systematic error in the Cdshadow correction for gamma ray components [18].

2.3 Geometrical CharacteristicsInherent unsharpness U, gives ultimate capability of the imaging system. As shown in Table 3

[13,15,16,j, the best U, was given to bel 1 um. However, usually 20,um was given for typical film-Gdconverter system, and greater than 100 Asm typically 200 um for electronic imaging. Recently, Ui ofNIP was measured and found to be 59 ± 8 ,um [13].

The importance of geometrical parameter LID has been discussed elsewhere [2], becausegeometrical unsharpness U, becomes frequently larger than inherent unsharpness of converter itself forU, < l / (LID). Where I is distance of object from an imaging plane. The geometrical unsharpness givesfrequently appreciable blur on an image.

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Neutron Imaging Methods to Detect Defects in Materials

Table 3. Measured Inherent Unsharpness for Converter-Film System [13,15,16]

Film No Converter Detector' Edge' 1(rm)' Slit/cell size FWHM(um)

H725 Gd-12.5um SR Gd 0.2 5pumWxso0umH 13.7 ± 6.3H655 Gd-25 pm SR Gd 0.2 17.5 * 1.3H740-1 Gd-25 am D30 Gd 0.2 19.1 2 1.8H740-2 Gd-25,um D35 Gd 0.2 11.1 _2.1H889 PBN SR Cd 0.2 22 * 5

H770 K0500 Dry Gd 0.2 lOumwx50,umH 265 * 5H769 NRC Dry Gd 0.2 @ 207 t 22

NRC C-CCD Cd 2.0 17,umHxl3umV 160 - 10'

- GdO, NIP Gd 0.0 25,umwx25,um' 59 ± 86

1. [Converter] Gd: Gd metal converter, PBN: 20,um pyrolytic boron nitride plate.K0500: Gd202S:Tb, converter, NRC: 6LiF/ZnS:Ag type converter.

2. [Film] SR: Kodak single coated film, D30: Dupont double coated film,D35: Dupont single coated film, Dry: 3M INSPEX-H dry film.

3. [Edge] Gd: 50pm Gd foil. Cd: 0.5 mm Cd plate.4. Separation between the edge and the converter (film thickness) plus the thickness of Al lid.5. Data from reference [15]. 6. Data from reference [13].All data except the last two lines are taken from reference [16].

The shape of diaphragm D is also important parameter. If the diaphragm has asymmetric shapesuch as square or rectangular opening. Images given by such a beam observed unsharpness becomesalso asymmetric [19].

Spatial deformation (magnification) of image is resulted by a finite L value. The effect has beenless considered as an important parameter. However, the parameter becomes serious result fordimensional measurements especially results of tomograms.

2.4 Transmission Character and Effective EnergyAt the stage of beginning in radiography studies, differences of transmission character were

ignored for thermal neutron beam without any experimental evidence and considered to be equivalentto 25 meV. Later, a quantity effective total macroscopic (ETM) cross section was proposed as anapproximated attenuation coefficient for a fixed continuum beam [17]. It was found that transmissioncharacters of various materials was slightly differed from one beam to an other. Table 4 showsmeasured effective total macroscopic (ETM) cross sections of 14 elements, 7 alloys and inorganiccompounds, 5 chemicals, and 3 biological materials for four different beam spectra with effectiveenergies of 9.8 meV, 17.0 meV, 28.9 meV and 1.46 eV [20]. The first two beams were obtained byinserting 10 cm and 5 cm thick Pd filters, respectively. The third beam was non-filtered beamextracted from No.2 tangential beam port in the Rikkyo TRIGA-I. Final one was given by a Cd filterwith thickness of 1 mm, and the attenuation coefficients at the resonance energy were measured by atransfer method using an In foil with thickness of 0.3 mm thick. Thus, appreciable difference of theETM cross sections were observed between beam to beam especially between filtered beams.

It is concluded that transmission characters must be considered to describe at least as a functionof a parameter describing a continuum spectrum. The concept of effective energy was proposed as therequirement. Effective energies as above mentioned were determined by a beam quality indicator(BQI) which was recently developed [21]. Many thermal and cold neutron beams with and withoutusing filters have been measured using the BQI, and summarized elsewhere [20].

3. Requirements for The Highest Sensitive ImagingAs shown in Fig.1, the image quality is limited by statistical fluctuation due to the quantum

noise of incident neutrons. However, if a leading term of the noise origin is an instrumental one which

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Neutron Imaging Methods to Detect Defects in Materials

is normally independent of number of neutrons, lowest detection limit is defined by the noise term.Such imaging systems are shown in Fig. I as the case of the cooled CCD and the film-Gd systems. If10 % of statistical fluctuation for the unit cell of 0.1 mm square is acceptable, the lower limits arefound on the Fig.1 to be 1O' n/cm2 for the cooled CCD and 108 n/cm2 for the film+Gd system. Toextend the lower limit, an averaging or a smoothing in more wider area of unit cell must be applied atthe sacrifice of spatial resolution.

Table 4 Effective Total Macroscopic Cross Sections of Various Materials for Four NeutronBeams with Different Effective Energies from 9.68 meV to 1.45 eV(unit: 1/cm) [20].

Beam Sub-thermal Sub-thermal Thermal In Epi-thermalFilter Pb = 10 cm Pb = 5 an none Cd= 1 mm Comment

Ecff 9.68 meV 17.0 meV 28.9 meV 1.46 eV

Al 0.0989 ± 0.0008 0.0986 ± 0.0007 0.1002 ± 0.0006 0.0887 ± 0.0012

Au 6.976 + 0.127 6.088 ± 0.089 5.619 ± 0.112 1,925 ± 0.021 Dental

Ag 4.545 + 0.057 4.066 ± 0.066 3.602 ± 0.048 1,055 + 0.009 Dental

Cd 114.58 + 1.38 109.64 ± 1.90 96.74 ± 1.50 0.577 ± 0.008 Dental

Cu 0.921 ± 0.016 0.899 ± 0.009 0.849 + 0.014 0.586 ± 0.006 Dental

Dy 35.64 ± 0.97 31.35 ± 0.91 28,01 ± 0.55 7.700 ± 0.137

Graphite 0.380 ± 0.008 0.398 ± 0.009 0.389 ± 0.007 0.3172 ± 0.0042

Fe 1.022 ± 0.028 1.043 ± 0.021 1.040 ± 0.020 0.5308 ± 0.0161

In 9.42 ± 0.31 8.23 ± 0,33 7.45 ± 0.22 88.70 ± 47.64 t<0,28 mm

Ni 1.648 ± 0.072 1.592 ± 0.048 1.604 ± 0.040 1.150 ± 0.029

Pb 0.259 ± 0.006 0,293 ± 0,004 0.312 ± 0.003 0.2620 ± 0.0055

Rh 11.19 ± 0.34 9.86 ± 0.18 9.11 + 0,16 36.352 ± 0.149 t=<0.025

Ti 0.637 + 0.010 0.553 ± 0.010 0.517 ± 0.005 0.239 ± 0.002

Zn 0.356 ± 0.005 0.346 ± 0.006 0.331 ± 0.004 0.2302 ± 0.0030

Ag-alloy 4.184 + 0.064 3.814 ± 0.037 3.416 ± 0.060 5.70 ± 1.12 Dental

Au-Pd 3.808 + 0.091 3.243 ± 0.062 2.965 + 0.077 3.26 ± 0.25 Dental

Brass 0.724 ± 0.011 0.670 + 0.007 0.652 ± 0.008 0.3477 ± 0.0081

LiF - + + 0.771 ± 0.000

PBN 30.20 ± 1.58 28.19 + 1.18 19.83 ± 1.39 5.451 ± 0.041

Pb(Te) 0.236 ± 0.005 0.274 ± 0.004 0.304 + 0.004 0.3035 ± 0.0051 Te=0.02%

SUS 1.013 + 0.022 1.022 0.011 1,006 ± 0.012 0.5208 ± 0.0085

H,0 3.557 ± 0.030 3.380 + 0.047 2.800 + 0.018 0.489 ± 0.053

D20 0.598 + 0.005 0.567 0.008 0.497 _ 0.004 0.360 ± 0.009

Teflon 0.318 + 0.006 0.321 ± 0.004 0.323 ± 0.003 0.2165 ± 0.0046

Poly 4.729 ± 0.121 4.398 + 0.053 3.541 ± 0.085 1.3284 ± 0.0480 t=<0.6cm

Acryl 3.541 + 0.032 3.254 + 0.035 2.717 ± 0.040 1,0521 ± 0.0288 t=<0.6cm

Tissue 3.504 + 0.059 3.183 + 0.069 2.247 ± 0.125 0.8654 ± 0.0425 t=<1.19cmTiss(new) + _ + 1.1202± 0.0679 t=<1.4cm

Bone 2.729 ± 0.075 2.106 ± 0.143 1.663 _ 0.130 0.6064 ± 0.0574 t=<2.07cm

Neutron beam: Rikkyo TRIGA-II (10OkW) - Beam port No.2 with Pb filter (0,5 and 10 cm).Measurements of effective energies: BQI with Imaging Plate for neutron detection (BAS NR2025).Measurements of ETM cross sections: Average slopes of transmission curves after scattered component corrections.

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Neutron Imaging Methods to Detect Defects in Materials

To seek the lowest limit of neutron fluence is another interesting point. Our previous studyshowed that the 100 % standard deviation was found at 4.5x104 n/cm2 for 50 pum square unit pixel(=1.1 neutrons/pixel) [13]. The analyzing unit area was widened from 50 um square to 1 mm square.The result shows at the left side point in the Fig.1. Thus, it is proved that the lower limit should beextended by the averaging over the suitably extended area.

To get the highest sensitivity of imaging device should be attained by realizing a single neutroncounting technique. For instance, the neutron sensitive imaging plate seems to fulfill the requirement.For electronic imaging, an image intensifier may be one of effective tool. Anyway, the imaging ofsuch a low level neutron field should be carried out taken into considering the statistical character.

4. ConclusionsSignals obtained by neutron radiography are discussed relating with image quality using

parameters of range of linearity, statistical character, geometrical character, and transmission character.In the discussions, some useful data were given by figures and tables.

In this study, many items are not discussed relating enhancement of image quality, usingvaluable traditional and advanced data processing.

This study only considered thermal and cold neutron radiography. However, it is not intended togive less importance to other neutrons such as a high energy neutron radiography including transfermethods and mono-energetic neutron radiography using nuclear reactions and TOF techniques. A partof those items will be discussed in another lecture in this conference such as a fast neutron radiography,an energy selected neutron radiography etc.

5. AcknowledgernentsThe author would like to express their thanks to Dr. S. Iwai, Dr. K. Takahashi, Dr. S. Tasaki

and Mr. M. Etoh Fuji Photo Film Co., Ltd., for their many discussions and kind help to supply ofimaging plates, and permission to use of the BAS5000 and the BAS2500. The work was supported inpart by a Grant-in-aid from the Ministry of Education, Science and Culture (No. 11691202).

References[1] Harold Berger, Neutron Radiography: Methods, Capabilities and Applications, (Elsevier Publ., Co.,

Amsterdam 1965); (Photocopy Edition: Industrial Quality, Inc., Gaithersburg, 1995).[2] P. von der Hardt and H. Rottger eds., Neutron Radiography Handbook, (D. Reidel, 1981).[3] J. C. Domanus compiled, J. F. W. Makgraf ed., Collimators for Thermal Neutron Radiography - An

Overview, (D. Reidel PubL., Dordrecht, 1987).[4] J. C. Domanus ed., Practical Neutron Radiography, (Kluwer Acad. Publ., Dordrecht, 1992).[5] J, P. Barton et al. eds., Neutron Radiography, (Reidel, 1982) [lst World Conf., San Diego (1960)].[6] J. P. Barton et al. eds., Neutron Radiography, (Reidel, 1987) [2nd World Conf., Paris (1986)].[7] S. Fujine et al. eds., Neutron Radiography (3), (Kluwer, 1990) [3rd World Conf., Osaka (1989)].[8] J. P. Barton ed., Neutron Radiography (4), (Kluwer, 1993) [4th World Conf., San Fransisco (1992)].[9] C. 0. Fischer ed., Proceerings - 5th World Conference on neutron radiography (1996), (DGZfp, Berlin,

1997) [Equivalent to "Neutron Radiography (5)"][10] G. M. MacGillivray and J. S. Brenizer, Jr. eds., Neutron Radiography System Design and Characterization,

(AECL Res., Chalk River, 1994) [1st Topical Meetings, Chalk River Nat'l Lab. (1990)].[11] H. Kobayashi and K. Mochiki eds., Nucl. [nstr. Methods, A377 (1996) 1-181 [2nd Topical Meetings,

Rikkyo Univ. (1995)].[12] E. Lehmann et al. eds., Nucl. Instr. Meth. A424 (1999) [3rd Topical Meetings, Luzerne (1998)].[13] H. Kobayashi and M. Satoh, Nucl. Instr. Meth. A424 (1999) 1-8.[14] E. Kobayashi, "Basics of Imaging Plate for Radiograms" (6th WCNR) Paper number 120.[15] It Kobayashi, in reference [10] pp.189-208.[16] H. Kobayashi, Radiation Detectors and Their Uses, KEK Proc. 93-8 (KEK, 1993) 174-185.[17] H. Kobayashi et al. J. Nucl. Sci. Tech., 29 (1992) 1045-1053.[18] H. Kobayashi, "Study for ETM Cross Section Measurements" (6th WCNR) Paper number 116.[19] H. Kobayashi, Nondestr. Test. Eval., 11 (1994) 77-85.120] H. Kobayashi, Nucl. Instr. Meth. A424 (1999) 151-157.[21] H. Kobayashi and Y. Kiyanagi, Nucl. Instr.

Meth. A377 (1996) 52-57.

r , /_0A__R;AA ?-Ar ,,,~I;r F,,rolv in Funtral EuroDe '99

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S10200091

Nuclear Energy in Central Europe '99Portoro2, Slovenia, 6 to 9 September, 1999

Neutron Diffraction Studies for the Measurement of Strains and Stresses

G. M. Swallowe and R. C. WimporyDept. Physics, Loughborough University, LEL I 3TU, U.K.

ABSTRACT: This paper describes the neuron diffraction method for the measurement ofresidual strains and stresses and illustrates the method with examples of measurements ona mining chain link and a Single Lap Shear (SLS) Joint. It is shown that compressivestresses in the chain surface contribute to the fatigue resistance of the link. Results for theSLS joint cast doubt on current finite element models of joint stress distributions andquantify the stress redistribution which occurs in the joint with ageing. The extension ofthe method for the measurement of dislocation densities and dislocation cell sizes isillustrated with an example of a plastically deformed copper sample.

1. IntroductionResidual stress distributions arise in many manufactured engineering components due toinhomogeneous heat treatments such as welding or quenching or inhomogeneous plasticdeformation. The magnitude and type of stress (tensile or compressive) vary from point to pointwithin the material and large stress gradients may arise. In the absence of external forces theoverall stress balances to zero when integrated over the whole volume of the component. Thesestresses can alter the components useful service life since they add to externally applied forcesand therefore alter the fatigue life of the material. It is now common practice to use finiteelement methods in order to calculate the expected values of residual stresses in manufacturedcomponents. It is highly desirable that such calculations be checked by direct experimentalmeasurements and diffraction methods provide the most reliable non destructive method ofcarrying out these measurements.

Residual stresses are elastic forces and therefore alter the spacing of crystalline lattice planesof the material. High resolution X-ray or neutron diffractometers can detect these small latticespacing changes and hence can in principle be used to measure the strain at specific pointswithin the material. In order to measure the strain two measurements of the lattice spacing arerequired, a measurement of the spacing in the region of interest and a zero strain referencemeasurement. The strain at the point of interest is the determined from the shift in the Braggreflection peak position AO using the equation £ = - O.5(cot 0) AO. The sensitivity of thetechnique depends on the diffraction angle 20 and it may be tempting to choose the neutronwavelength so as to maximise 0 but considerations of spatial resolution, as described below,lead to a value of 20 - 9d0 being generally favoured. In order to be useful for stress analysis thediffractometer must be capable of determining the peak positions with a relative accuracy of theorder of 5x I5. Instruments capable of this resolution are available at all major neutronsources. The advantage of using neutrons rather than X-rays lies in the penetrating power of theneutron. Using neutrons useful measurements can be made at depths several cm. in steelsamples while X-rays are effectively limited to, at most, tens of microns. The availability ofhigh intensity synchrotron X-ray sources such as the ESRF at Grenoble has increased the depth

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Neutron Imaging Methods to Detect Defects in Materials

to which X-ray measurements can be made but, at a fraction of a mm, X-rays are stillessentially useful for surface and near surface measurements only.

A neutron diffraction measurement provides a value of strain in a particular direction atspecific points within a component. The direction is that of the scattering vector, see Figure 2.In order to obtain the full stress tensor it is necessary both to make strain measurements in atleast 6 different directions at the point and also to use the appropriate elastic modulus toconvert strain to stress. Because of crystal anisotropy the elastic constant and Poisson's ratiowill vary with the lattice planes being used in the measurements. The Kroner model (1,2) isnow frequently used to determine the appropriate elastic modulus but texture in the material ofinterest can lead to inaccuracies in the predicted modulus value. It is often best to make a directmeasurement of the modulus by loading a sample in a stress rig in-situ in the neutron beam andmaking a plot of crystal plane strain as a function of applied stress. However, in a sample thathas undergone severe plastic deformation the accuracy of measurements of residual stress usingjust one set of lattice planes can be open to question. This is because some crystal grainswill deform first due to their being in an 'easy' orientation for slip compared to neighbouringgrains and the resulting intergranular stresses complicate the situation and add to themacroscopic residual stresses that are the items of interest. Figure I illustrates a neutron stress-strain curve for a 99.9% pure polycrystalline copper sample where the Bragg planes aremeasured in the loading direction. It can be seen that at the yield point (- 40 MPa) the curve forthe I I l and 200 planes deviates from linearity while that of the 3 I I plane remains essentiallylinear. It is therefore desirable to make measurements using several different sets of latticeplanes though time constraints often make this difficult at reactor sources. However in manymetals there are one or more lattice planes that are relatively little effected by plasticdeformation and these are commonly used to give reliable measurements of lattice strain inhighly deformed samples examples are the 311 plane in copper and the 211 or 110 in iron.

100Soiler Detector

At ? Scn , Lattice k:f,., 0 ' ~~~~~~~~~~~~~~~~ ~PlanesMPa *

50 o o 2 -I

~~~~~~~~ ~~~~~~Volue s pe d

0 *2 .4 .6 8 1e x103

Monochromator

Figure 1: Applied stress- neutron measured Figure 2: Schematic of strain scanning systemstrain in 99.9% Cu. A II 1, * 31 1, 0 200 after Hutchings (in reference 5)

The high intensity and high resolution required for neutron residual stress measurementsmean that they are almost invariably carried out at reactor or large spallation sources. Recentlythere has been some effort in the UK by Oxford Instruments to develop a portable source foruse in strain measurements but work on this has now been suspended. From the point of viewof residual stress measurements the difference between reactor and spallation sources lies in thefact that at a reactor source one neutron wavelength is chosen and measurements are carried out

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Neutron Imaging Methods to Detect Defects in Materials

by scanning 0, whereas at a spallation source a white beam is used with the detectors fixed at afixed angle relative to the neutron beam. Different neutron wavelengths arrive at the detector attimes given by t = L/v = (Xm/h)L with m the neutron mass, h Planck's constant, v the neutronvelocity and L the distance from source to the detector. The strain is given by E = At/t. Themajor advantage of a spallation source is therefore that many diffraction peaks can besimultaneously collected. This allows the use of Rietveld methods to determine strain anddeviations from random orientation of crystal grains, which effects the calculated values of themodulii, in the component to be detected.

2. Experimental arrangementA typical arrangement for a neutron strain scanning system is schematically illustrated in

Figure 2. The size of the incoming neutron beam is limited by a set of slits so that a 'slice' ofthe component under investigation is illuminated by the beam. A further slit, in the case of asingle detector, or radial collimator when a Position Sensitive Detector (PSD) is used, defines asecond slice through the component from which neutrons may reach the detector. Theintersection of these two slices defines the volume, the gauge volume, from which themeasurements are made. The measured diffraction angle is an average of the diffraction anglesfrom all the crystallites within the gauge volume which are oriented so as to diffract neutronstowards the detector. In principle the smaller the gauge volume the more accurately can thestrain distribution in sample be defined but the resulting reduction in diffracted neutron beamintensity due to the use of very small gauge volumes considerably worsens the signal to noiseratio and lengthens the experimental time. At current reactor and spallation instruments theminimum slit sizes which can be used to produce diffraction data on a reasonable timescale aretypically Imm x 1 mm. This leads to a minimum sampling volume of - 1 mm3 . Gaugevolumes of the order of 1 mm3 are generally accepted to be a reasonable compromise inneutron diffraction work. The size and shape of the sampling volume will clearly depend on therelative orientation of the incoming and diffracted neutron beams. The volume will be aminimum when they are at 900 to each other and measurements are usually carried out with thebeams as close to 900 as possible in order to improve the spatial resolution of the strainmeasurements. For reasons of efficiency in the collection of data the detectors used now atvirtually all strain scanning installations are PSDs. Most instruments are now equipped with astress rig which allows a sample to be loaded in tension or compression while it is in theneutron beam. Facilities to carry out tests at elevated temperatures are also available.Components are mounted on sample stages so that they can be moved in the x, y and zdirections relative to the fixed sampling volume. In this way the component can be moved in a3D grid pattern and measurements made at positions throughout the component. Stagescurrently available (e.g. at Dla at ILL or ENGIN at ISIS) have capabilities of carrying samplesof up to ~50kg weight and allow movements of - 40cm. However, new strain scanningfacilities are currently in the planning stage at both ISIS and the ILL which will increase boththe size and weight of the components that can be investigated.

3. Strain Measurement ApplicationsThe neutron method is the most time consuming and expensive of all current methods of

residual stress measurement. Components must be taken to large research facilities and the sizeof component that can be investigated is restricted. The next generation of facilities, the first ofwhich (ENGIN-X) is expected to come on stream at ISIS in 2002, will considerably reduce thecost of measurements per data point to about the same as holedrilling or sectioning methodsand will also reduce the time required to obtain a comprehensive set of measurements. Themajor advantage of the neutron method over all others is its combination of deep penetrationdepths and the fact that it is non-destructive. In view of these points the neutron method has

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Neutron Imaging Methods to Detect Defects in Materials

found most of its applications in components for the aerospace and transport industries. Weldedjoints and cold expanded holes are frequently the source of fatigue cracks and much effort hasbeen put into the measurement of residual stresses around them (3,4). References 3 and 4 alsocontain many other useful papers on the neutron strain measurement technique and the resultsthat can be achieved using it. Another area in which the neutron method has found wideapplication is the measurement of stresses in the interior of metal matrix composites (5). Theseare frequently SiC reinforced Al, or WC reinforced Ni. Since both components are crystallinethe neutron method enables the strain in both matrix and reinforcement to be measured andpredictions of thermal stresses and the variation of residual stresses with fibre ratio can beinvestigated. In the following the results from two sets of measurements carried out by stafffrom Loughborough are briefly presented.

3.1 High Tensile Steel Chain Link:Chains manufactured from high tensile steel are used in many applications where it is vital

that their load carrying capacity is assured. The final stage of manufacture involves applying aload which is sufficient to plastically deform the chain and imparts the final dimensions to eachlink (6). The residual stresses produced in this process are believed to be beneficial to thechains performance and the idea of the experiments was to measure the magnitude anddistribution of these stresses. The chain link was manufactured from 19 mm diameter steelformed into a link 63.4 mm wide and 98.2 mm long. Figure 3 illustrates the definition of the x,y and z directions and the orientation of the link in the neutron beam used to obtain strains inthese directions. Measurements were carried out on the Dl a diffractometer at ILL and thesampling volume used was 2x2x2 mm. The 211 reflection was used with a neutron wavelengthof 0.191 nm giving a value of 20 close to 900.

ian)

a,.5

Figure 3: Orientations of chain link for neutron diffraction measurements

The results are illustrated in Figure 4 together with a finite element calculation of the zdirection stress. The finite element calculation was carried out using the ABAQUS code with asimple linear elastic region followed by a linear work hardening model for the metal and a yieldstress of 89OMPa. It can be seen that reasonable agreement between the FE and neutronmeasured values of residual stress is obtained. It is also clear that the surface of the chain link isin compression in the z direction with relatively little residual stress in the x and y directions.Since, when in use, the chain is loaded in tension in the z direction this residual stress patternwill oppose the formation of surface cracks from the flaws that inevitably occur during use.These results explain the origin of the improvement in chain performance obtained by thetraditional last stage in manufacture.

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Neutron Imaging Methods to Detect Defects in Materials

50lo

0~ ~~-100<-300 / / *

0 2 t 6 a 10 12 1L 16 18 20Y POSIlION mm Z

Figure 4: Residual Stress measurements Figure 5: Origin and directions of the co-ordinate systemwith a comparative FE calculation of a. for the SLS joint. All dimensions in mm.

3.2 Single Lap Shear (SLS) Joint:Adhesive joints are now frequently replacing riveted joints in transport applications since

they provide a much more even load distribution across the join and avoid the dangers inherentin riveted structures of cracks initiating at the rivet holes. These joints are commonly used tojoin sheet metals and a great deal of work using both analytic and finite element techniques hasbeen carried out to predict the distributions of stresses and strains within and around the joint(7,8). However, other than surface measurements, no measurements of the stresses in a loadedmetallic joint had been made. Experiments were carried out, again using the 211 Braggreflection on the Dla diffractometer at ILL to verify the FE calculations and to study the effectof environmental ageing on the joint.

The joints were prepared using 50 mm x 16 mm x 3 mm CRI mild steel adherends whichwere grit blasted and subsequently degreased and vacuum annealed prior to assembly. Theadhesive used was Araldite AVI 19 and the bondline thickness was controlled by the additionof 1 % 250 micron "Ballotini" glass spheres. Figure 5 illustrates the appearance of the joint andthe co-ordinate system used in the stress measurements. Aged samples were prepared byimmersing a joint in deionised water at 60 °C for 10 days while simultaneously applying a loadof I kN. Measurements were carried out to determine stresses in the y direction with the jointssubjected to an axial load of 2.5 kN. A subsidiary experiment in which a piece of the steel usedto make the joints was loaded incrementally was carried out to determine the diffraction elasticconstant in the direction of interest for the Bragg plane used.

50 .--. .. . ..-----.. - -.....

40 4030 < | + z = 2mml 1 30 if \ + z- 7~~~~~~~~~~~~~~~~~z =4rmm

X ~~~~~~~~~~ -2 0 m + z = 7 ~ 1 2 . . | \ a c~~~~~~~~~~~~~ 20~ ~ ~ ~ ~~~~~~~~~i'2

10 -20

20 -, 2 4

yposition (mm) yxoixcn(mm)

Figure 6. Plot of the stress difference between Figure 7. Stress in the adherend as a function ofunaged and aged SLS joints for x = 0 (glue line) longitudinal position in an unloaded SLS joint.

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Neutron Imaging Methods to Detect Defects in Materials

Figure 6 and 7 illustrate some of the major findings to emerge, the full results are presented inreference 9. Figure 6 illustrates the difference in stress between an unaged and aged sample andclearly shows a redistribution of load occurring with ageing. The load carried by the agedsample is considerably decreased in the material along the upper surface of the glue line (x = 0,z = 2, y = 2,4,6,8) and in consequence increased in the central region (x = 0, z = 8, y = 2,4,6).This is likely to be due to plasticisation of the adhesive in the outer areas of the joint and aconsequent reduction in load carrying capacity and relaxation in the strain of the adjacentmetal. These results provide direct evidence for load redistribution during the ageing of joints.

Figure 7 presents the results for the curing stress close to the glueline in the joint and can becompared with the modelling results presented by Adams (8). The results of these experimentsdo not agree with the predictions of Adams et al., the stress close to the interface is not uniformalong the central region for either z = I or z = 4 and in fact tends to be tensile in the centre andcompressive at the edges. The data obtained has therefore cast doubt on the results of recentfinite element models and further work will be needed to resolve the discrepancies.

4. MicrostructurePlastic deformation introduces defects into the material and these give rise to microstrains

which result in a broadening of the diffraction peak. At higher plastic strains dislocations formcell structures which effectively divide the material into small coherent scattering volumes,these also cause peak broadening as described by Scherrer. Coherent size broadening isindependent of diffraction order but strain broadening is dependent on diffracting angle andhence diffraction order. In principle it is therefore possible to distinguish between broadeningcontributions due to size and strain. This is normally carried out by examining a completediffraction pattern and studying the comparative broadening of different diffraction peaks (10).However this traditional method is impossible when only one diffraction order is available, asis the usual case in reactor based neutron residual stress studies. Since the microstrain relatedcomponent is directly related to sample plastic deformation and the size broadening componentto the dislocation cell structure it is desirable to make use of information already gathered instudies of internal strain to evaluate these parameters. Estimates of plastic strain are potentiallyvaluable to the engineer since the variations in plastic strain at points within a sample will bemirrored in variations of yield stress. The single peak method of de Keijser et al (11) may beused to separate size and strain effects and the results presented here illustrate how the datafrom residual stress measurements may be used to study microstructure.

The samples used were polycrystalline cylindrical rods with diameters in the range 3 to 4mm and gauge lengths in the range 20 to 30 mm. The copper and samples were manufacturedfrom 99.9% pure metal. the iron samples from 99.8% material and the nickel 99.98%. Allsamples were annealed after manufacture to minimise residual strains. Measurements werecarried out on the TKSN-400 spectrometer at Rez. This system produces very narrowinstrumental line widths which make it particularly suitable for studying peak profiles. Thereflections studied were the copper and nickel 002 and 111, and the iron 110 peaks. At leasttwo samples of each metal were tested.

The single peak method of de Keijser et al. describes the measured peak profile as aconvolution of a standard profile (which incorporates the instrumental effects) with the samplepeak profile. The sample profile is itself regarded as a convolution of a Gaussian functionwhich is related to microstrain with a Cauchy function which is determined by coherent volumesizes. The method is therefore to use a standard instrumental peak profile to deconvolute themeasured peak and produce the sample peak data. This data is then analysed to obtain theGaussian fig and Cauchy Pc peak breadth components. There is of course an assumption in the

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Neutron Imaging Methods to Detect Defects in Materials

method that the Cauchy component is solely due to size effects and the Gaussian due tomicrostrain. This assumption seems to be supported by theoretical and experimental evidenceand is discussed by Delhez et al. (12). In these experiments broadening was dominated by theGaussian component with evidence of the Cauchy contribution becoming apparent only by thepresence of the tails at high strains. Figure 8 shows plots of the Gaussian and Cauchy breadthcomponents of Cu peak profiles as a function of applied strain. The data is well fitted by a

simple power law of the form iOg = a + b F-c where a, b and c are material parameters. These

parameters vary not only from material to material but depend also on the annealing or othersample history in a similar manner as do the parameters in the stress strain curve. The figurecontains data from the same Bragg peak from two samples. It is clear that the same fittingparameters can be used to describe the data for both samples. From reference 11 the averagemicrostrain is given by <E> = 13g/4 TanO and the coherent scattering region size by

D = XIIc CosO where Pg and Pic are the Gaussian and Cauchy components of the integral

breadth.Since the microstrain is a function of defect densities which may in turn be considered to be

a result of the relative amounts of plastic deformation, evaluation of microstrain does not initself provide information on the amount of plastic deformation experienced by various regionswithin the material. However the width of the Gaussian component of the peak profile canprovide a simple empirical measure of the local plastic deformation if a calibration is carriedout in which peak profiles of samples with known plastic strains and made of the same materialas the test sample are also measured. This need not increase the total experimental timerequired by more than a relatively small amount.

2.4

0

2.0 -~ ~o2.0 2.0

pp 0] PC%4 X 1l x10 4 ~- 1.6

a I 1 ~~~~~~~~~~~~~1.2 a...- x

1 ~~~~~~~~~~0.81 0 0.1 0.2 0.3

0 o*1 02 03Strain Strain

Figure 8: Width parameters for 002 reflections from Figure 9: Derived dislocation cell size as aCu samples.* Cauchy sample 1 0 Gaussian sample I function of strain in copper. 0 data from* Cauchy sample 2 o Gaussian sample 2 this work, * data from Gracio (13)

Derived values of D, the effective coherently diffracting region size, as a function of strain inCu are illustrated in Figure 9. The electron microscope based observations of Gracio et al (13)on Cu indicate that these metals form closed dislocation cell structures at strains greater than afew percent with cell dimensions of the same order as the derived coherent region sizesreported in this work. The reduction in coherent region size with increasing strain observed in

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Neutron Imaging Methods to Detect Defects in Materials

this work also follows their reported trend. The similarities are such that it may be concludedthat the coherent diffracting volume sizes derived from the diffraction data are measures of thedislocation cell structures in the deformed metal

The data presented in Figures 8 and 9 is from the Cu 002 reflections. A limited amount of datafrom one sample of Cu and Ni observing the 11 1 reflection was also gathered. The same trendin reduction of cell size with strain was observed but for both the Cu and Ni samples no cellstructure was observed until the applied strain exceeded 0.2. In both cases the cell dimensionsmeasured using the 111 reflection were approximately a factor of 2 greater than those measuredusing the 002 reflection. Dislocation densities can be derived from the microstrain using therelationship p = k<F>2/Fb 2 where p is the dislocation density, b the Burgers vector, F a factordescribing interaction between dislocations (F =1 in this work), k a constant and <E> theaverage microstrain. It is generally accepted that dislocation densities scale with plastic strainwith a relationship of the form p = A + B ep where A and B are material constants and Fp is the

plastic strain. If the dislocation density estimates derived from the single peak analysis areaccurate it would be expected that the experimental stress strain data and the dislocation densitystrain data estimates should fall on the same (suitably scaled) curve. Good agreement wasfound between these two sets of data. A fuller description of the results of these experiments ispresented in reference 14. The results of this work indicate that much more use could be madeof the data that is routinely gathered to determine residual stress in engineering components.Generally it is only analysed to determine macrostrains from shifts in the diffraction peakposition and other than an estimate of microstrain no use is made of the information containedin the peak profile.

References1. E. Kroner, Z. Phys 151, 504, (1958)2. Behnken, H., Hauk, V., Z. Metallkunde, 77, 620, (1986)3. L. Edwards and A.T. Ozdemir, in Measurement of Residual and Applied Stress Using Neutron

Diffraction eds. M.T. Hutchings and A.D. Krawitz, NATO ASI Series 216, 545, Klewer(1992)

4. Th. Nitschke-Pagel and H. Wohlfahrt, Proc. Fifth Intl. Conf on Residual Stress, Linkoping,Sweden 1997

5. P.J. Withers in Measurement of Residual and Applied Stress Using Neutron Diffraction eds.M.T. Hutchings and A.D. Krawitz, NATO ASI Series 216, 545, Klewer (1992)

6. 'Short link chain for lifting purposes, Parts 1-6', BS 4942, (1981).7. M.Y. Tsai and J. Morton, J. Strain Analysis, 29, 137, (1994)8. R.D. Adams, J. Comyn and W.C. Wake, Structural Adhesives Joints in Engineering, 2 nd ed.,

Chapman and Hall (1997)9. G.M. Swallowe, G.W. Critchlow, R.C. Wimpory and T. Pirling, J. Adhesion, 70, 1, (1999)10. C. Barrett and T.B. Massalski, Structure of Metals 3rd edition (Pergamon, Oxford, 1980) see

chapter 16.11. T.H. de Keijser, J.I. Langford, E.J. Mittemeijer. and A.B.P. Vogels, J. Appl. Cryst. 15, 308,

(1982)12. R. Delhez, T.H. de Keijser, J.1. Langford, D. Louer, E.J. Mittemeijer and E.J. Sonneveld in The

Rietveld Method ed. R.A. Young, chapter 8, TUCr Monographs No 5, OUP (1995)13. I.J. Gracio, J.V. Femandes and J.H. Schmitt, Mat. Sci.and Engin. A118, 97, (1989)14. G.M. Swallowe, J.C. Osborn, P. Lukas and M. Vrana, Proc. 4 rh European Conf On Residual

Stress, Cluny (1996)

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11 111t IIi1 l lii lS10200092

Nuclear Energy in Central Europe '99Portorol, Slovenia, 6 to 9 September, 1999

Investigation of Microporosity in Die-cast A1SiS2(Cu)Alloys by Neutron- and X-ray Radiography

Szalay Zsolt*, Balask6 MArton***Ph.D. Student, Department of Materials Sciences,

Technical University of Budapest H-i 111 Budapest, Hungary**KI`KI Atomic Energy Research Institute, P.O.Box 49, H-1525 Budapest, Hungary

ABSTRACT - The porosity of the castings can dramatically reduce the solidity and reliabilityof the objects made from aluminum alloys. The X-ray radiography is able to find theplacement of the porosity of the aluminum devices. After a special "water saturation" processthe dynamic neutron radiography is available to discover the "dangerous" - surface near-porosity in the aluminum samples. The X-ray and neutron radiography were used ascomplementary examination techniques to study the porosity of the aluminum castings.

Keywords: porosity, aluminum castings, X-ray radiography, neutron radiography

1. IntroductionThe different kinds of the die-cast aluminum alloys contain porosity by the production

process. The porosity is very dangerous for the solidity of the objects, mainly if it is locatednear to the surface of the casting. Some non-destructive-testing methods (NDT) are able tostudy the porosity of aluminum alloys. It seems that the suitable combined application of X-ray radiography (X-RR) and ultrasonics is very effective in this field, however, thedetermination of the depth of the error area is not easy task by these methods. A "watersaturation" procedure on the defective samples and dynamic neutron radiography (DNR) wereapplied. It was found that in the samples the water was infiltrated in the porosity.

2. Experimental facility

The experimental work was carried out at the Dynamic Radiography Station (DRS) [1] ofthe Budapest (10 MW) reactor. This facility is able to use the neutron-, gamma-, and X-rayRadiography as it is seen in the Fig. 1. The neutron - and gamma beams are obtained througha horizontal thermal channel of the reactor using pin-hole type conical collimator. Thecollimation ratio was 170, the beam diameter 150 mm and the neutron flux at the detectorposition 108 n cmf2 sec-'. Objects with a surface area of 700 x 1000 cm2 and weights of up 250kg can be investigated and are manipulated into the correct position of the beam by means ofa remote control mechanism. The X-rays was generated by a large scale of portable, industrialX-ray generators. Their power is changeable from 50 kV; 5 mA to 300 kV; 5 mA. Thetransmitted neutron image of the objects is converted into light by a scintillation converterscreen (type NE 426) - this task is solved by ZnS converter screen or a NaCs single crystal forX- and gamma - ray imaging and the "light image" is detected by a low-light-level (LLL) TVcamera (104 lux for type TV 1122). The imaging cycle is 40 msec, thereby providing thepositioning for visualizing medium speed movements up to about 2.5 rn/sec inside theinvestigated object. The resolution of the detected radiography image is about 150 grm forneutrons and about 100 pm for X-rays. The schematic block diagram of the imaging system is

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Neutron Imaging Methods to Detect Defects in Materials

shown in Fig. 2. The radiography images are displayed on a monitor, stored by an S-VHSrecorder and for further analysis, an image processing system is used (type Sapphire 5.05 byQuantel). A hard copy of the picture is provided by a video printer. In addition to theradiography image other parameters characterizing the operation of the investigated object -such as operating time, pressure, temperature, flow velocity, power consumption - aremeasured and controlled.

9- .: . - t1^, ~~~~~Reactor -

Inside collimator Investigated object withC) Iron shutter system remote control mechanism(Y Beam diameter changer and filter unit ® Imaging system with

low light level TV camera) Reactor shielding ma Working parameter indicators

B) Outside collimator sl Background TV camera(C) Biological shielding (a BeamstopA) Position of portable X-ray generator () Contrl cabin

Fig. 1. Arrangement of the Dynamic Radiography Stationat the Budapest research reactor

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Neutron Imaging Methods to Detect Deuss in Materials

X-ray Backgroundand Temperature TV cameras

neutron Pressure Control monitorsradiation7_

Heat poweretc.

3. Invesbject i e obje

NE 426ZnSNa~s l I

Te i e Converter screen Low-light leveli _ _ ~~~TV camera_

The fLi t o a Image t is msymbol_"" optswidhs 26 m, isprocessilg t% _ + ' ~~~~~~system covre

specialflangserie for the hi r r ity T Videoprinterc SIl i

Fig. 2. Imaging system of the Dynamic Radiography Station

3. Investigated objectThe investigated objects were choozen from the mass production of alunlititil industry.

The first element is a part of an air bag system in a motor car. It is marked in the Hgi. 3- withsymbol "A". (Its width is 26 mnm, its length is 205 mm and its thickness is 2 mmi). It contals, aspecial flange series for the higher releability. The second object of our investiat~ion is theyoke of the scaffolding system in the building industry. In the Fig. 3. it is denoted by symbol"B". (Its width is 36 mm, and its length is 9% mm and its thickness is 'X mm). Ta, pcOsity ofthe aluminum castings reduces the solidity of the objects.

Fig. 3. Samples made from aluninum castingsA.. Frame of an awi bag systemB: Yoke of scaffolding in the building industry

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Neutron Imaging Methods to Detect Defects in Materials

4. Experimental resultThe large number of castings were investigated by X-RR to select the samples withporosity content. In order to increase the quality of the picture 500 images were integratedby the Quantel video processor. The X-ray pictures of the "A" is shown by the Fig. 4. andthe "B" sample is shown by Fig. 6.

af al It F- t C It OF Q 8 v

Fig. 4. X-ray radiography of the porosity in the frame of the air bag system

Fig. 5. Dynamic neutron radiography of the frame of the air bag system after the"water saturation" process

The porosity of the castings, characterized by the bright areas, are marked by arrows. Aspecial "water saturation" process was used before we applied the DNR. The essential idea ofthis procedure is to substitute the residual gas with water in the porosity of aluminumcastings. The neutrons are very sensitive to the water because of its high hydrogen content.The DNR is an appropriate method to determinate the "waterized" porosity. In the first stepthe aluminum samples were taken in an excicator and the samples were filled up by water.The vessel was closed and was evacuated by a rotating vacuum pump for 120 minutes. Thesamples stayed under the water for further 1 5 hours. If the porosity of the casting was situatednear the surface of the sample, the water was able to ooze into the cave of aluminum. Thiseffect was observed for both "A" and "B" specimens, as shown in Figs. 5 and 7 as exposed byDNR.

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NVeutvOn tmar~girnt .hods Do Detec Defeces in Maer,1l7

Fig. 6. X-ray radiography of the yoke of the scaffolding

Fig. 7. D~ynanilc neutron radiographx of the yoke of the scaffolding after the"cwater saturation` process

The "waterized' porosity of the aluminum castings are characterized by dark shade, markedby arrow~ss. Figure 8. shows the cut surfiice of 'W' sample at the place of the porosity. It isclearly observable the smxall material t.hickness (12120 piin) between the porosity and thesurface of sample.

Fig. 8, The position of the porosity int the yoke after cutting

ffhrnanO)1aI _ _l.~~r~n~e.?&:(cl .n.r.3.............A.....

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Neutron Imaging Methods to Detect Defects in Materials

5. Conclusion

The X-ray radiography is an advanced NDT method to discover the placement of theporosity in the alurninum castings. Applying a special "water saturation" process the dynamicneutron radiography is able to show the "dangerous"- surface near - porosity of the aluminumdevices by their water contain. Both X-ray - and neutron radiography techniques were usefulcomplementary examination methods to study the porosity of the aluminum castings.

6. References

[1] M. Balask6, E. SvAb "Dynamic neutron radiography instrumentation andapplication in Central Europe" Nucl. Instr. Methods A 377, 140, 1996

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Iill IzilB llS10200093

K t Nuclear Energy in Central Europe '99Portoro2, Slovenia, 6 to 9 September, 1999

Application of `0B Entrapped PEG-liposome to BoronNeutron-Capture Therapy for Pancreatic Cancer Model In vivo

H. Yanagie ', K. Maruyama2 , T. Takizawa2 , 0. Ishida2 , K. Ogura3 ,T. Matsumoto4 , Y. Sakurai5 , T. Kobayashi5 , K. Ono5 , J. Rant6,

J. Skvarc6, R. Ilic6 , A. Shinohara7 , M. Chiba7,M. Eriguchil and H. Kobayashi8 .

'Dept of Surgery, Institute of Medical Science, University of Tokyo, Tokyo,2Dept. of Pharmaceutics, Teikyo University, Kanagawa,3College of Industrial Technology, Nihon University, Chiba,4 0miya Research Laboratory, Nikken Chemicals Co. Ltd., Saitama,5Kyoto University Research Reactor Institute, Osaka, JAPAN,6Jozef Stefan Institute, Lublijana, SLOVENIA,7Dept of Epidemliology, Juntendo University School of Medicine, Tokyo,fnstitute for Atomic reactor, Rikkyo University, Kanagawa, JAPAN.

ABSTRACTThe cytotoxic effects for tumor were evaluated with intraveneous injection 10B

PEG-liposome(Stealth liposome) on human pancreatic carcinoma xenografts in nudemice with thermal neutron irradiation. After thermal neutron irradiation of mice injectedwith B bare-liposome or B PEG-likosome, AsPC-1 tumour growth was suppressedrelative to controls. Injection of B PEG-liposome caused the greatest tumoursuppression with thermal neutron irradiation in vivo. These results suggest thatintraveneous injection of B PEG-liposome can increase the retention of ' 0B atoms bytumor cells, causing tumor growth suppression in vivo upon thermal neutronirradiation.

Key words: Boron neutron capture therapy (BNCT), Neutron capturealpha-autoradiography, CR-39 track detector, Drug delivery system,PEG-liposome (Stealth liposome)

1. INTRODUCTIONBoron neutron capture therapy ( BNCT ) is aimed at inhibiting the growth of

various cancers [1]. The cytotoxic effect of BNCT is due to a nuclear reactionbetween B and thermal neutrons. This nuclear reaction is as follows:

`B+ 'n 71i + 4He (a) + 2.79 MeV (6.3 %)7Li* + 4He (a) + 2.31 MeV( 93.7 %)7- L + 4He (a) + 0.478 MeV

The resultant lithium ions and a particles are high linear energy transfer particles withrelatively high biological efficiency. These particles (a and 7Li) destroy cells withinabout 10pim path length from the site of capture reaction. It is theoretically possible to

* Corresponding author: Phone: +81-3-5449-5352, fax: +81-3-5449-5439,e-mail: [email protected] / [email protected]

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kill tumour cells without affecting adjacent healthy cells, if 1 atoms can be selectivelyaccumulated in tumour cells. BNCT has been used clinically in patients withmalignant brain tumours and melanoma.

Liposornes have been investigated extensively as carriers for anticancer drugs inattempts to direct active agents to tumors or to protect sensitive tissues from toxicity.We have reported that ' 0B atoms delivered by immunoliposomes are cytotoxic to humanpancreatic carcinoma cells (AsPC-1) with thermal neutron irradiation in vitro [2]. Theintratumoral injection of boronated immunoliposomes can increase the retention of ' 0Batoms in tumor cells, causing tumor growth suppression in vh'o under thermalneutron irradiation [3].

In this study, we prepared the polyethylene-glycol binding liposomes (PEG-liposome) as the effective '°B carrier to avoid the phagocytosis by reticuloendotherialsystems (RES) and the bare liposome. We performed a technique of prompt y-spectroscopy to quantitatively determine the '0B concentration in the organ of mouse.And also we used a technique of neutron capture autoradiography using Solid StateNuclear Track Detectors (SSNTDs) in order to qualitatively determine the '1Bbiodistribution in whole body samples of mice.

2. MATERIALS & METHODS

2.1. Materials prepareingChemicals: Sodium salt of undecahydro-mercaptocloso-dodecaborate

(Na2`1B12 H2l SH) was obtained by Wako Chemical Co. Ltd. (Tokyo, Japan).Dipalmitoyl phosphatidylcholine (DPPC), distearoyl phosphatidylcholine (DSPC)

and distearoyl phos-phatidylethanolamine (DSPE) were kindly donated by NOF Corp.,Tokyo. NOF also provided a monomethoxy polyethyleneglycol succinimidylsuccinate (PEG-OSu) of average molecular weight, 2000.

Target Tumor Cells and Mice: The human pancreatic carcinoma cell lineAsPC-1, which produces carcinoembryonic antigen (CEA) was obtained from DainihonSeiyaku Co. Ltd. (Osaka, Japan).

Male BALB/c nulnu mice were obtained from Nihon SLC (Shizuoka, Japan)and used at 6 to 7 weeks of age. The procedures for tumor implantation and sacrificeof the animals were in accordance with approved guidelines of the Institution'sAnimal Ethics Committee.

Preparation of PEG binding liposomes containing B-compound:Liposomes were prepared from DPPC/DSPC/CH (7:2:1, m/m) and an appropriateamount of DSPE-PEG by the reverse-phase evaporation (REV) method and extrusionmethod [4]. The lipid mixture (5 mg in total lipids) was dissolved in 600 , 1 ofisopropyl ether/chloroform (1:1, v/v) and one-half ml of 120 mM B-compound(Na 2 'B2 1HItSH ) solution was added.

Liposomes were formed by the REV procedure and extruded more than ten timesthrough polycarbonate filters (Nuclepore, Nomura Science, Tokyo) to control size.Uiposomes were sized to 100-120 nm in mean diameter by extrusion, which werereferred to as SUV. The extrusion was performed at 509C in a thermostatic extrusiondevice (EXTRUDER, Upex Biomembrane, Canada). Liposome size was measuredby dynamic laser light-scattering measurements using a ELS-800 particle analyzer(Otsuka Photonics, Tokyo). This admixture was heated at 60WC for 10 min withintermittent vortex mixing and chromatographed on a BioGel Al. 5m column (2 cm x 20cm, Bio-Rad). The ' B-entrapping liposomes were finally sterilized by passagethrough a membrane filter of 0.45 ym pore size. B entrapped bare liposomes wereprepared as same way without polyethylene glycol.

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2.2. Experimental procedureMeasurement of accumulated B concentration in each organ in vivo.

AsPC-1 cells (1 x 10 ) were injected subcutaneously into the back of male BALB/cnu/nu mice. At 10 - 14 days after injection, when the estimated tumour weight reached100 - 300 mg, the recipient animals were injected intravenously into the tail vein witheither '0B entrapped bare liposome ('0 B bare-lip.) or '(B entrapped PEG-liposome( B PEG-lip.) under anesthesia The ' 0B concentration of 10B PEG-lip. and '`B bare-lip. were 116 ppm and 160 ppm, respectively. Tumors of this size never regressedspontaneously. The animals were sacrificed 3, 6 and 24 hours after injection and thetumors and organs were removed so that B concentration was determined bymeasuring the gamma ray at the peak corresponding to a 478 keV area [5, 61. Tissueswere weighed immediately after dissection and recorded as "wet weights". Resultswere expressed as [g B / g tissue.

Preparation of sliced mice samples At 10 - 14 days after injection ofAsPC-1 cells, when the estimated tumour weight reached 100 - 300 mg, 0.2 ml of Bentrapped-liposomes (10B bare-lip. / 10B PEG-lip.) were injected to the tumor bearingmice intraveneouslly. The mice were sacrificed 3 and 6 hours after the injection of

B-tiposome solution, and the mice were frozen at -60 C. Subsequently, the frozenmice were cut suggitally into 40 Apm thick sections putting on the mending tape, andfreezed dried at -20 C in 2 weeks, and air dried in one more week. Thus, the driedsamples were prepared [71.

Neutron Capture Autoradiography using Track Etch DetectorsIn order to examine the biodistribution of the B entrapped liposomes after

intraveneous injectios, we performed the Neutron Capture Auto Radiography(NCAR).After intraveneous injections of B-liposomes, the tumor bearing mice were sacrified andfrozen. The mice were cut into 40 pm thick sections mounted on a thin 3M Scotchtape. The whole-body sections (40 pm thick) of pancreatic cancer tumor bearingmouse were put in close contact with the CR39 detector plate and exposed to a flux ofthermal neutrons in the dry cell of the Thermal Column Neutron radiography facility ofthe Ljubljana TRIGA Mark II reasearch reactor of the Jozef Stefan Institute. Thegamma rays were filtered by a provisional 16 cm thick Pb filter made of lead bricks andthe irradiation facility was not optimal regarding the neutron beam intensity and gammaray background. The thermal neutron fluences varied regarding the objectives of theexperiments and were as follows:

For B concentration measurement: 6.8 x 1010 neutrons / cmFor Imaging: 4.4 x 10 12 neutrons / cm

For a-autoradiographic imaging including proton of tracks produced by '4N (n, p)reaction, where '4N is the biogenically abundant nuclide, the CR-39 detector plates wereetched in a 6.25 N NaOH solution at 70 'C for 60 minutes to reveal tracks. Thetracks were automatically measured by the TRACOS track analysis system of the JozefStefan Institute [8].

Evaluation of tumor growth suppression on experimental BNCT: Inorder to evaluate the tumor growth suppressive effects of BNCT with 10B liposomaldelivery, we prepare 10B PEG-lip. (6600 ppm) and '0 B bare-lip.(6850 ppm). Afterfour times intraveneous injections were performed with 6 hrs' intervals, tumor bearingmice were irradiated for 37 min with the irradiation rate of 9 x 10i ns-1 cm 2 thermalneutrons (total fluence: 2 x 1012 n cm- 2) at the TRIGA-II atomic reactor of Institute forAtomic Energy of Rikkyo University. After irradiation, the effect of BNCT was

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estimated on the basis of tumor volume and morphological findings of the tumors at 3-day intervals [3].

3. RESULTSComparison of B accumulation in each organ after injection of B

bare-lip.! B PEG-lip.: AsPC-1-bearing mice (n = 3) were given i. v. injectionjO~~~~~~~~~~~~~~~n

with 0.2 ml of solution of B PEG-lip. or B bare-lip.. The mice were sacrificed at3, 6 and 24 hrs after injection and the boron contents of tissues were analyzed asdescribed. Table 1 shows the B concentrations in various organs (tumor, blood,liver, kidney and heart) after injection of 10B PEG-lip. or 10B bare-lip. B uptake in

10tumor was higher than the uptake in the liver at 6 to 24 hr after injection of B PEG-lip.The uptake in the liver was higher than the uptake in the tumor at 6 hr after injection of

B bare lip. and decreased to less than 1.40 ppm 24 hr later. The concentration of Bin tumor after injection of B PEG-lip. was two times higher than that of B bare-lip.at 24 hrs. The boron content in tumor reached a maximum value at 24 hr, andincreased slightly by retention due to the of circulation with PEG after injection. Ourdata indicated that the selective accumulation of B atoms in tumor was achieved byusing B PEG-lip.

Table 1. Measurement of accumulated '0B concentration in each organ aftersingle intraveneous injection of '0B PEG-liposome in vivo

Boron distribution following injection of `0B PEG-Organ liposonle / ' 0B bare-liposome (ppm) after:

3h 6h 24h

' 0B PEG-lip tumor 1.57 1.95 2.37blood 3.41 2.92 1.22liver 2.52 1.18 1.43kidney 3.34 1.91 2.45heart 1.59 1.34 2.20

°B bare-lip tumor 1.09 1.67 1.13blood 3.41 1.23 1.17liver 4.41 4.37 1.35kidney 5.81 1.38 3.03heart 3.26 1.41 1.76

The boron concentration was measured by prompt gamma-specroscopy method The original 'nBconcentration of `B PEG-liposome and 10B bare-liposome were 116 ppm and 160 ppm, respectively.

Neutron Capture Autoradiography using Track Etch Detectors:In order to examine '0B-biodistribution in mice, we performed NCAR of sliced

mice samples using CR-39 track etch detector. Proton and a-tracks were measured bythe TRACOS track analysis system. TRACOS is capable of accurate measurements ofdimensions, shape, grey level intensity and accurate position of individual tracks on alarge CR-39 plate. On the basis of local track densities obtained from positionalinformation of tracks having different origin it is thus possible to make separate digital

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tumor__liv~lier_

of r~iver -a

Fig. I a-autoradiographic imaging by NaOH method NCAR images ofwhole-body boron distribution obtained by neutron capture autoradiography after 6 hoursintraveneous injection of 3B-Iiposomes. Neutron capture autoraiograph was preparedfrom the whole-body section ( 40 gm thick ) of a pancreatic cancer-bearing mouse. Theneutron fluence needed to produce this image was 4.4 x 10`2 nlcm2 . After the irradiation,CR-39 detectors were etched in 6.25N NaOH solution at 70 'C for 60 minutes. Upper:'0B-PEG liposome injection, Lower: 'SB bare liposonme injection.

radiographic images. Images of whole body mice by neutron capture autoradiographywere shown in Figure 1.

At 6hr after intraveneous injection of '0 B bare-lip./ tOB PEG-lip., the accumulationof 10B was found only in the tumor, but not in the liver or kidney. It has thepossibility to escape the uptake of reticuloendotherial systems (RES) in the liver usingPEG-lip.

Growth inhibition of tumor treated with 'OB PEG- liposome: The effectof ' 0B PEG-lip. and `OB bare-lip. on tumor growth suppression was examined withthermal neutron irradiation.

The boron concentrations in tumor tissue after injection of '0 B PEG-lip. was 37.3ppm with four times i. v. injection of '0 B PEG-lip. by plasma emmision sp ectroscopy.After thermal neutron irradiation of mice injected with '0B PEG-lip. or Bbare-lip.,AsPC-1 growth was suppressed relative to controls. Intraveneous injection of '0B PEG-lip. caused the greatest tumor growth suppression and necrosis with thermal neutronirradiation in Figure 2.

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Yt

Fig.2 Tumnor growth suppression or I3NCT with 'WB delivery using PEG-liposore :Six hours inravencous injection of '13 PEG-liposomes or '30 bareliposomes,tumor bearingitmice wereirradiaed with thermal neutron (total fluencc: 2 x 1012 nlcm2 ) at theTRIGA-il atomic reactorin Rikkyo University. (a) Non-treated, (1,) '0B bareliposome treted,(c) ' PEG-liposome

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4. DISCUSSIONOne of extremely important concerns in BNCT is the '0B delivery system, for

which liposomes are very attractive and interesting. It is commonly told that the sizeof multilamellar liposome (MLV) is about 300 nm, so these MLV liposomes are easilyphagocyted by reticulo-endotherial system (RES). So it is very difficult to accumulatethe content of liposome into the target cancers. To escape these phagocytosis of RES,we have tried to prepare single unilamellar boronated polyethylene glvcol bindingliposomes which is become to use in chemotherapy. We found that the taB PEG-lip.have the possibility of retention to the tumor cells and providing sufficient '1B atoms forthe BNCT. Maruyama et al have demonstrated that polyethylene glycol bindingliposomes (about 100 nm mean diameter) and rigid lipid composition showedsignificantly greater accumulation in solid tumor [9].

The track etch method was applied to observe visually qualitative distribution of1'B [7]. The image with NaOH etch method is effective to identify the position of tumor,and can also describe organs in the whole body section by means of proton tracks withdifferent contrast in comparison to the a track image. The correct ' 0B concentration isalso calculating now using PEW etch method [7] andlor computing automatic imageanalysis system TRACOS [8].

BNCT with intraveneous injection of PEG-lip. with a high content of ' 1BSH hasthe ability to destroy malignant cells of the tumor mass. The PEG-lip. can easily reachthe tumor tissue with enhanced permeability and retention (EPR) effect than the bare-lip.We try to prepare boronated transferrin binding PEG-immunoliposomes (stealthimmunoliposomes), and to perform BNCT experiments in vitro and in vivo.Experiments using systemic injection of inteligent 1 B delivery systems are in progressfor selective targeting of '°B atoms in tumors in the application of clinical BNCT.

REFERENCES

[1] H. Hatanaka,et al., Int J Radiat Oncol Biol Phys 28(1994) 1061 - 1066.[2] H. Yanagie, ei al., Br. J. Cancer, 63(1991) 522 - 526.[3] H. Yanagie, et al., Br. J. Cancer, 75(1997) 660 - 665.[4] K. Maruyama, et al., Proc. NatI. Acad. Sci. USA 87(1990) 5744-5748.[5] H. Yanagie, et al., J Cancer Res Clin Oncol 120(1994) 636 - 640[6] T. Kobayashi, etal., NucI. lnstr. Methods, 204(1983) 525 - 531.[7] H. Yanagie,et al., Nucl. Instr. Methods, A424(1999) 122- 128.[8] J. Skvarc, etal., Nucl. lnstr. Methods, B 152 (1999) 115 - 121.[9] K. Maruyama, et al., Biochim. Biophys. Acta 1234(1995) 74 -80.

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*5 ~~~~~~~~~~~~~~S10200094Nuclear Energy in Central Europe '99Portoro2, Slovenia, 6 to 9 September, 1999

FAST NEUTRON RADIOGRAPHYUSING PHOTOLUMINESCENT IMAGING PLATES

J. Rantl*, M.Balasko2 , E. Kristof1 , J. Stade3

l J. Stefan Institute, Ljubljana, Slovenia2 KFKII-AEKI, Budapest, Hungary

3Bundesanstalt fuir Materialforschung und -prfifung (BAM), Berlin, Germany

Fast neutron radiography (FNR) and resonance neutron radiography (RNR) are complementary to theconventional radiography with high energy gamma-rays or brems-strahlung radiation used for the inspection ofthick metal objects. In both non-destructive methods, the contrast sensitivity and the penetration power can beimproved by using higher energy neutrons. At present direct techniques based either on Solid State NuclearTrack detectors (SSNTDs) or scintillating screens and transfer techniques using activation threshold detectorsand radiographic films are applied for the detection of fast neutron images. Rather low detection sensitivity offilm and SSNTD based fast neutron imaging methods and also rather poor inherent image contrast of SSNTDpose a problem for FNR in the fast neutron energy region 1-15 MeV interesting for NDT. For more efficientdetection of fast neutron images the use of novel highly sensitive photoluminescent imaging plates (IP) incombination with threshold activation detectors as converter screens in transfer imaging technique was proposedby authors and tested at the KFKI research reactor. The conventional IP produced by FUJI Photo Film Co. forthe detection of beta and X-ray radiation were used. The threshold activation detectors were the reactions"5In(in, r)5mliw, 64Zn(nip) 64Cu, 56Fe(np)5 6Mn, 24Mg(nrp)24Na and "Al(n.X) 24Na. These threshold reactionscover the fast neutron energy region between 0.7 MeV and 12 MeV. Pure, commercially available metals 0.1mm to 0.25 mm thick made of In, Zn, Fe, Mg and Al were used as converter screens. The very high sensitivity ofIP , the linearity of their response over 5 decades of exposure dose and the igh dynamic digitalisation latitudeenabled fast neutron radiography of image quality comparable to the quality of thermal NR. In our experimentalconditions (4nt 108 n/cm s, RCd % 2) the neutron exposure and IP exposure periods were still practical andcomparable to the half life of the corresponding reaction products (half an hour to several hours). Even with the27Al(n.ct)24Na reaction having a 23 WU fission spectrum avaraged cross-section of 0.65 mb useful fast neutronimages were obtained. These preliminary experiments clearly demonstrated the useful imaging properties of IPin transfer fast neutron radiography with threshold activation detectors. On the basis of this new fast neutronimaging technique and using an appropriate set of threshold activation converter screens FNR in energy windowbetween the 0.1 MeV to 20 MeV could be conceived.

1. Introduction

Radiography with thermal neutrons in the energy range of 0.01 eV to 0.3 eV is a wellestablished non-destructive method [1]. Neutrons of epithermal energies (0.3 eV to 10 keV)and fast neutrons ( 10 keV to 20 MeV) are used for neutron radiographic examinations inmuch smaller extent. However, the use of fast and epithermal neutrons for neutronradiography is becoming increasingly attractive. The reasons for the increasing interest forfast neutron radiography (FNR) and epithermal neutron radiography (ENR) are:* Neutrons of higher energies, in particular 14 MeV neutrons can penetrate thick layers of

bulk materials (more than 10 cm), offering the possibility to inspect larger objects [2-5].* The radiographic contrasts obtained by FNR are similar and comparable to those obtained

with high energy X- and gamma-ray radiography and in general are smaller than with

* Retired from JSI

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thermal neutron radiography. Poorer discrimination is offset by broader contrast latitudeand low atomic number materials can simultaneously be observed with heavier metals[4]. However, the neutrons at the lower portion of fast neutron region (< I MeV) canoffer radiographic contrast different from either X-ray or thermal neutron radiography [2].

* Availability of mobile or even portable radioactive and modern accelerator based fastneutron sources [6-8] in addition to many research reactor based NR facilities, enablesindustrial applications of FNR.

The increased interest for FNR is promoting also the search for more efficient fast neutronimage detectors. For the detection of fast neutron images direct techniques based either onSSNTDs [9] or scintillating screens and transfer techniques based on activation detectors andradiographic films are in use [1-3]. Rather low detection sensitivity of the film as well as ofSSNTD based fast neutron imaging methods and also rather poor inherent image contrast ofSSNTD pose a problem for the fast neutron radiography in the for the NDT interestingenergy region 1-15 MeV. For more efficient detection of fast neutrons the use of novel highlysensitive photo-luminescent imaging plates (IP) in combination with threshold activationdetectors as converter screens in transfer imaging technique were proposed by the authors[10].In addition to its inherent insensitivity against y-ray background the FNR using transfertechnique with threshold activation detectors has several useful properties:* The threshold detectors are not sensitive for neutrons below the threshold energy of

relevant nuclear reaction and hence are not sensitive for scattered neutrons moderatedbelow threshold energy.

* Each threshold reaction has his own characteristic energy window of sensitivity, insidewhich the neutrons contribute most to the activation of the detector. This energy windowdepends on energy dependent reaction cross-section and neutron spectrum. The neutronabsorption and scattering effects in the investigated objects can significantly distort theinitial fast neutron spectrum and the sensitivity regions depend on the materialcomposition and dimensions of the object.

* In a single neutron exposure a set of foils of different threshold activation detectors canbe irradiated providing simultaneous fast neutron radiographs through different "energywindows". Simultaneously the thermal and epithermal neutrons, which are present in theneutron beam in particular when the fast neutron beams of a research reactor are used, areinducing thermal and resonance neutron absorption reactions in the converter material.This can be sometimes of an advantage, however often the unwanted 'parasitic' activitieshave to be suppresses by filtering out the thermal neutrons using Cd shields and/or byselecting appropriate time of neutron irradiation, waiting time before exposing the imagedetector and the exposure time.

The reaction cross-sections of threshold detectors are in a millibarn region and orders ofmagnitude smaller then the activation cross-sections of conventional converter materials forthermal neutron radiography. A problem encountered in FNR using radiographic films asimage recorders is an adequate fast neutron beam intensity to produce quality fast neutronimage. According to Berger for FNR using 14.5 MeV neutrons in a single screen transfertechnique with common threshold detectors (reactions in Cu and Al) and radiographic filmsthe required fast neutron flux to achieve moderate film density 1.5 at still practical exposureconditions (30 min irradiation time, waiting time 2 min and 'overnight' film exposure) shouldbe at least of about 2. 107 n/cm2 S [3]. The use of novel IPs instead of radiographic filmswould offer several benefits. Compared to radiographic films the IPs have advantages as high

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sensitivity of 102_103 times that of radiographic films, high dynamic range in exposure dose(more than 6 orders of magnitude), high intrinsic spatial resolution, large area and negligiblespatial distortion, reusability and digital output [11]. In exposure boxes well shielded againstnatural background the surface distributions of 14C and 40K radionuclides of few 0.01Bq/cm2 can be detected by autoradiography using IP as reported by Mori et al. [12].

In this contribution we report on the measurements of the response of various available typesof IP to the /ly/) radiation induced in selected threshold activation detector materials by fastneutron irradiation in the dry cell irradiation facility of the Ljubljana TRIGA Mark II researchreactor. The use of IP in FNR was successfully tested in rather limited number of experimentsat the KFKI research reactor [13]. The use of IP in FNR with threshold activation converterscreens is discussed.

2. Experimental

2.1 Threshold activation detectors in transfer technique of FNRThe threshold detectors are based on endotherm nuclear reactions induced by fast neutrons ina suitable materials. They are widely used in reactor physics experiments for fast neutronspectroscopy and many of them have been used also as converter screens in transfer techniqueof FNR [1-3]. Some selected threshold activation detectors, common in FNR and used in ourexperiments are quoted in Table 1. Their nuclear characteristics as threshold energy, theirsensitivity energy region and spectrum averaged cross-sections in 235U fission neutronspectrum and the cross-section values at 14 MeV are presented here. The detectors chosen arethe same as used previously for measurements of fast neutron spectra in Ljubljana TRIGAMark II 'dry cell' irradiation facility [14]. The selected threshold detectors cover the fastneutron energy region from above 0.3 MeV to 14 MeV. The half-lives of the reactionproducts range from few minutes to several hours and are suitable for transfer exposuretechnique. The converter screen materials are pure (0.999) metals and readily available in aform of large area thin sheets or foils. They are of natural isotopic composition and henceduring the irradiation with thermal, resonance and fast neutrons significant activities otherthen targeted activity are induced. For the measurements of the response of IP foils (0 5 cm)of Al, Mg, Zn, Fe and In were used, the same, as for the measurements in fast neutronspectroscopy [14]. The converter screens for FNR were 10 X 10 cm2 foils (0.1 mm thick) ofpure (0.999) Al, Zn and Rh and larger 20 X 20 cm2 screens (0.25 mm thick) of technicallypure Al, Fe and Cu.

2.2 Fast neutron irradiation facilitiesTo measure the response of IP the threshold detector foils were irradiated in the 'dry cell' ofthe Ljubljana TRIGA Mark II reactor in a "broad beam" geometry, since there is nocollimator installed in this facility. The irradiation position was 20 cm from the front end ofthe 60 X 60 cm2 graphite thermalizing column using the existing irradiation rig for theirradiation of the medical samples within BNCT experiments. The integral fast neutron fluxabove 0.1 MeV was 1.93 107 n/cm2s, measured by a set threshold detectors. Thermal neutronflux and Cd ratio (RCd) were 4.9 107 n/cm2s and 34 respectively, measured by Au foils (0.05mm).Few trial experiments in FNR were performed in the NR facility of the radial beam port No. 1of the KFKI research reactor in Budapest [15]. The neutron beam is well collimated (L/D=170) and with a high content of epithermal neutrons. Here the total thermal flux was 1.0108 n/cm2 s, Rcd= 8. Fast neutron spectrum was not measured.

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2.3 Imaging Plate Detection SystemThe imaging system used consists of imaging plates, FUJI BAS 1500 laser scanner andRaytest UV IP eraser. The imaging plates were FUJI Photo Film BAS IIIS for imaging X/y/j3radiation and suitable for X-ray radiography and transfer NR, neutron sensitive IP-ND fordirect thermal neutron imaging and IP type TR for imaging of soft X-rays and P radiation(e.g. for autoradiography of tritium). The IP consist of a plastic support plate covered with0.13 mm (0.05 mm in case of IP-TR) thick layer of crystals of photostimulable storagephosphor BaFBr:Eu2 + combined in a plastic binder and covered by a thin layer (0.02 mm) ofplastic protective cover. With IP of TR type the phosphor layer is intended for theregistration of 3H soft P radiation and is hence unprotected and susceptible for surfacedamage and wetting. In case of IP-ND the storage phosphor is mixed with gadolliniumoxide (50 %). The BAS 1500 He-Ne laser (632.8 nm) scanner has a pixel size 0.1 X 0.1

2mm, scanning speed 14 ps/pixel and 12 bit digitalisation (4096 grey levels). The inherentresolution of the system is lower than the pixel size, only about 0.2 mm (with advancedscanners - 40 pm).The digital images are handled, processed and analysed by a personal computer and printedby Epson Stylus Photo printer. The image handling, processing and analysing software isTINA 2.0 supplied by Raytest (Germany) and Photoshop ADOBE 3.0.

2.4 Measurements of the IP response to the radiation induced in threshold detectorsTo measure the response of imaging plates to the /i3ly radiation induced by neutrons a set offoils (0 5 cm), same as used for fast neutron spectroscopy, was irradiated in the neutron fieldof the 'dry cell' irradiation facility. Set of foils was irradiated in Cd pot (1 mm thick) to filterout thermal neutrons. Three different sets of foils have been prepared: (Al, Mg and Zn), (In,Fe) and (In, Al). The present experiments did not include Rh and Cu foils. Of each detector atleast 2 foils were irradiated to allow simultaneous determination of the specific saturatedactivity of the relevant reaction product by calibrated Ge gamma-ray spectrometer. Tomonitor the variations in the reactor power and to measure the thermal neutron flux bare andCd covered Au (0.05 mm) and diluted 0.1% Au-Al wires were irradiated together with the setof detector foils. The irradiation time was chosen to be approximately of the same magnitudeas the half-life (T1,2 ) of the threshold reactions in the set (15 h, 3 h and 0.3 h). The waitingperiods before the exposure of the IP with the irradiated foils was long enough to allow decayof short living parasitic or unwanted activities. The exposure dose of the IP was controlled byvarying the exposure time. With each irradiation 2-3 exposures of different duration andwaiting period were performed. Each group of IP exposures was performed in exactly thesame experimental conditions and with well known exposure dose (decays/cm2). Allexposures of IP were performed in a light-tight Al exposure cassette, without anyintensifying screens. With each set of foils two different IP were exposed simultaneously in acassette. In these experiments it was assumed that the fast neutron attenuation in thin detectorfoils is negligible. After the exposure and after waiting period of -10 min the IP were scannedfor read-out. Scanned neutron radiographs of detector were analysed to extract an averagephotoluminescent signal (PSL events/mm2) over a large area of detector foil image. From thisvalue the average background (PSL events/mm2 ) signal was subtracted. The result wascorrelated to the exposure dose of the radiation (decays/mm2 emitted in 27r geometry)computed from the measured value of the relevant specific saturated activity taking intoaccount the time corrections factors due to the irradiation time, waiting and exposure time.Due to the small mass thickness of the foils (Al, Zn, Mg) and rather high energy of emittedradiation corrections for self-absorption of the /l'ly radiation in the foils were not taken intoaccount.

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Neutron Imaging Methods to Detect Defects in Materials

2.5 Fast neutron radiographyFew trial experiments in FNR at the NR facility in the radial beam channel No.1 of theBudapest KFKI reactor were performed. The neutron beam was filtered by Cd plate at theoutlet of the beam. The converter screens of Al, Zn, Fe, Cu and In were usually packedtogether in pairs and covered by Cd cover from both sides. Irradiations were performed'overnight' and irradiation times were typically 15-17 hours. Waiting period before retrieval ofthe irradiated screens was about 1 hour to get rid of the short-living unwanted activities in thedetector screens. In case of the 115In(n,n') I5mIn detector the waiting period was greater than15 hours in order to suppress the 54 min activity of l16mIn to the level much lower than theactivity of the 15mIn. Therefore two exposures were made. The first exposure after few hoursof waiting (cooling!) time and of about few minutes in duration produced neutron image dueto the resonance neutrons at 1.46 eV and second exposure after 15-16 hours with IP exposureovernight produced fast neutron image. In the case if the neutron beam has a strongcomponent of epithermal neutrons the choice of In as fast neutron converter for FNR mightnot be the best solution. Since at KFKI there was no IP scanner available, the exposed IP weretransferred to US and read out with a delay of 24 hours!

3. Results and discussion

3.1 IP response functions of some threshold activation convertersThe response functions PSL signal/cm vs. the exposure dose/surface area (in decays/cm 2 )of the 24Na radiation due to the reactions 27Al(na)24 Na and 24Mg(n, p)24 Na are in a log-logscale are presented for the 3 selected types of FUJI Photo Film IP in Fig. 1. The linearity ofthe response curves extends over almost 3 decades. The response of the BAS IIIS type IP isthe highest. Somewhat smaller is then the response of neutron sensitive IP type ND,apparently due to the admixture of insensitive gadollinium oxide. Almost an order ofmagnitude less sensitive are IP designed for the detection of tritium radiation, since theiractive layer of storage phosphor is much thinner than with the other two types of IP. In caseof the 64Zn(n, p) 64Cu reaction the response curve is no more linear and the response dependson the waiting time and exposure time. At prolonged waiting times the response issignificantly lower. In addition to the 64Cu nuclide, which is also a ,3+ emitter there is a strongcontribution of 69mZn (13.8 h) and of more short living Zn (55 mm) if radiation with higherregistration efficiency in the phosphor and which are induced due to the resonance neutrons.In case of performing FNR in the presence of strong contribution of resonance neutrons thecontribution of resonance neutrons to the fast neutron image has to be considered. From theabove measured values of the IP response to the selected threshold activation detectors it iseasy to estimate the required fast neutron flux to obtain a target value of the PSL signal atprescribed irradiation, waiting and exposure time and for a threshold converter screen of agiven mass thickness. In case of the Al screens used in our experiments and for PSL signal at10 PSL events/cm2 and for practical irradiation and exposure time of T12 the required flux offission neutrons is below 1. 107 n/cm2s.

3.2 Example of FNR using transfer technique and IPAs an example of FNR a fast neutron image of a pneumatic consumption meter is presented inFig. 2. Detection system was 2 7 Al(n,)24Na threshold detector (Al 0.25 mm thick) andsensitive IP BAS IIIS. The object is composed of two parts with very different compositionand different thermal neutron attenuation properties. The upper part is relatively hollow cavitywith pistons encased in an Al casing. The lower part contains dented stainless steel wheels

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Neutron Imaging Methods to Detect Defects in Materials

encased in steel casing and is relatively opaque for thermal neutrons. The FNR image hasbroad latitude in contrast and both dense and hollow Al parts can be observed, including fewmm thick Al casing. In TNR the upper part was overexposed and Al casing could be barelydetected even by contrast enhancement, enabled by this IP based digital neutron radiography.The FNR could not reveal oil soaked debris in the upper left corner, which was clearlyobserved in TNR. The TNR was of better image quality and with better image discernment.The overall exposure of FNR is not optimal and could be still improved. Detectors withhigher activation cross-section than Al (0.685 mb), as Mg, Fe or Rh could also improve theimage quality, as verified in our work. The FNR enables better visualisation of much denserlower part made of steel.

4. Conclusions

1. Response of 3 different types of IP has been measured for a set of selected thresholdactivation detectors of interest for transfer technique of FNR.

2. Threshold detectors in combination with IP enable to produce high quality images in FNRat fission neutron flux levels below 1. 107 n/cm2 sec.

3. Using a suitable set of threshold detectors and IP it is possible in a single neutronirradiation to obtain neutron radiographic images at several energy windows, ranging fromepithermal to fast neutron energies.

4. The transfer technique with threshold activation detectors and using IP can greatlyenhance practical applications of FNR.

5. References1. Berger, H., Neutron Radiography, Elsevier, Amsterdam, 19652. Berger, H., Radiography with fast neutrons, Proc. 6th ICNT, Paper M-7, 63-743. Berger, H., Image detection methods for 14.5 MeV neutrons: techniques and applications,

Int. J. Appl. Rad. Isot.,21(1970) 59-704. Beynon, T.D., Constantine, G., Deep penetration radiography using 24.5 keV neutrons,

Nucl. Instr. Meth. Phys., A264 (1988)526-275. Richardson, A., E., Improved images in 14.5 MeV neutron radiography, Mater. Eval.,

April 1977, 53-586. Hawkesworth, M.R., Atomic Energy Review, 15,2(1977)169-2207. Dance, W.E., Cluzeau, S., Mast, H-U., Integration of an advanced sealed-tube neutron

generator into a mobile neutron radiology system and resulting performance, Nucl. Instr.Meth.,B56/57 (1991)907-911

8. Cluzeau. S., Huriet, J.R., New neutron generators for industry: the GENIE family,Ibid., 911-914

9. Berger, H., Track-etch radiography: Alpha, proton and neutron, Nucl. Techn., 19,(Sept.1973),188-198

10. Rant, J., Stade, J., Imaging plates as detector for neutron radiography, Materialpruifung,40 1-2,(1998) 1620-25

11. Miyahara, J., Takahashi, K., Amemiya, Y., Kamiya, N., Satow, Y., A new type of X-rayarea detector utilizing laser stimulated luminescence,Nucl. Instr. Meth., A246(1986)572-578

12. Mori, C. et al., Effect of Background Radiation Shielding on Natural RadioactivityDistribution Measurements with IP, Nucl. Instr. Meth., A369(1996)544-546

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Neutron Imaging Methods to Detect Defects in Materials

13. Rant, J., Stade, J., Balasko, M., Kaling, M., New possibilities in neutron radiography withimaging plates, Proc. 7th European Conference on NDT, Copenhagen, Denmark, May1998, ECNDT (1998), 2763-2770

14. Najier. M., Rant, J., Solinc, H., Set of 7 threshold detectors used as fast neutronsprectrometer, IJS Report R-570, Ljubljana, (Oct 1969)

15. Balask6, M. SvAb, E., "Dynamic neutron radiography instrumentation and applications inCentral Europe" Nucl. Instr. Methods A 377,(1996)140

16. Baard, J.H., Zijp, W.L., Nolthenius, H.J., Nuclear Data Guide for Reactor NeutronMetrology, EUR 12354 EN, Kluwer Acad. Publ., Dordrecht, 1989

17. JEF-PC 2.0, NEA Data Bank, OECD, Paris, 1998

Table 1. Characteristics for some threshold activation detectors for FNR.Data compiled from ref. [16], 14 MeV cross-sections are takenfrom JEF-PC[17]

Reaction Ener. range ofReaction threshold 80% response'

[MeV] E1lp. - Eo% Half-Life <uf>235 0.14[MeV] [mb] [mb]

0 3Rh(nri')flO 3m) < 0.1 0.72 - 5.8 56.1 min 699 45

--- min~,n' 110.3 1.1 - 5.9 4.486 h 177 -

Zn(n,p) Cu 1.3 2.6 - 7.5 12.71 h 35.1 193Al(n~p) Mg 2.6 3.7 - 8.5 9.46 min 4.10 87Fe(n,p) Mn 4.5 5.8 - 10.2 2.577 h 0.989 118

27Al(n,) 24Na 5.2 6.8 - 11.1 14.959 h 0.685 124.724Mg(n~) 2~4 Na 6.0 7.6 - 10.6 14.959 h 1.44 -

-,,C-u(n,2n) Cii 10.0 11. - 17 12.71 h 0.292 93Cu(n,2n) Cu 11.1 12. - 18 9.74 min 0.075 470

Definitions:

+ 100-x = I dE o-(E) Ofiss(E) | J dE oy(E) fi.(E),Ex 0

<0>23 5 = 235U fission spectrum averaged cross-section: dE o(E) fi.ssJ E) / dEj r,(E)0 0

-T4 = reaction cross-section at 14 MeV

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Neutron Imaging Methods to Detect Defects in Materials

10000 - ----- -- -- -- -

1000A

0 ND~~~~~~~~~tE / * , 0 t1 + ~~~~~~~~~BAS IIIS

E 100 - -'ND

tL A ft ' ^ * TR

10,,

1,00E+03 1,00E+04 1,00E+05 1,00E+06

Na-24 decays/cm2

Fig. 1 Measured response of IP as PSL signal/cm2 vs. exposure dose of 24Na ,/yradiation produced in threshold reactions 27Al(n, () 24Na and 24Mg(np)24 Na.IPs: FUJI type BAS III S, neutron sensitive type ND and type TR for 3Hautoradiography. Integral fast neutron flux (above 0.1 MeV): 1.93 107 n/cm2s.

Fig. 2 FNR of pneumatic consumption meter, 27A1 (n,a) 24Na detector (0,25 mm A1 foil)under Cd, KFKI reactor, neutron exposure 1 9h 10 min, waiting period 3 h 35 min. IP exposure 8 h15min.

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Nuclear Energy in Central Europe '99 S10200095Portoro2, Slovenia, 6 to 9 September, 1999

Investigation of Perspectives of Fast Neutron Radiography on the Basis ofNon-Traditional Neutron Sources: Neutron Generators with Accelerating

and "Plasma Focus" Tubes

V.1. Mikerov, A.A. Zhitnik, Ju.N. Barmakovl), A.I. Isakov, E.P. Bogolubovl),V.1. Ryzhkov'), T.A. Khasaev'°, V.A. Tukarev, A.P. Ignat'ev,

V.V. Korneev, A.A. Pertsov, V.A. Samarin'), Ju.P. Ivanovl), V.A. Sevrjukov2 ),

P.N. Lebedev Physics Institute of Academy of Sciences of Russia (LPI), Leninsky Prospect53, Moscow 117924, Russia

All-Russia Research Institute of Automatics (VNIIA), Moscow 101000, Central PostOffice, P.O. 918. Russia

2) NPP -Nauka Servis", Moscow 103473, Volkonsky p/k 11, Russia

ABSTRACT - Radiographic measurements have been carried out with neutron generatorsbased on accelerating and plasma focus tubes. The obtained results have experimentally provedpossibility of application of such generators for non-invasive inspection with fast neutrons.A possibility for imaging with X-ray generated by the same sources has been demonstrated too.

Key words. fast neutron radiography, neutron generator, fast neutron detector

1. Introduction

At present, the prospects of fast neutron radiography application in industry are concernedwith the development of transportable and portable neutron sources. In this respect neutrongenerators with accelerating and plasma focus tubes are distinguished by rather high neutronyield, low weight, operational and ecological safety [1]. The aim of this work was toinvestigate salient features of these sources and perspectives of their application in fastneutron radiography. Due to a rather low life time of a neutron generator with an acceleratingtube it was interesting to estimate low limit of exposure time for radiographic measurementswith such a source. In the case of a neutron generator with a plasma focus tube the aim was tocheck a possibility to get a radiographic image in one pulse.

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Neutron Imaging Methods to Detect Defects in Materials

2. Experimental equipment and conditions

Investigations were carried out with custom made neutron generators developed andproduced by the VNIIA. The ING-103 (Fig.1) is a generator with a plasma focus tube and theING-07 (Fig.2) - with an accelerating tube. Specifications of the generators are presented inTable 1. Fast (14MeV) neutrons are emitted in 4t steradians. Maximum neutron yieldamounts to about 3x109 n/s for the ING-07 and 3x10' 0 n/pulse for the ING-103. It isimportant to notice that the generators emit fast neutrons out of a small area. Its size is about3-5 mm and 1 mm for ING-07 and ING-103, respectively. Thus, in most practical cases thesesources can be considered as point like ones. A short duration of the ING-103 pulse (20 ns)and rather high neutron yield per pulse are especially of interest for imaging quick processes.Besides fast neutrons the generators radiate also X-rays with an average energy of about80 keV.

A low power consumption and dimensions of the generators are very attractive fromthe point of view of their use in industry for on site inspection.

Table 1.

Performance data Generator model

ING-07 ING- 103

Neutron Yield, n/s 3xl1o (3xl0'0)(n/pulse)

Max. Pulse Rate, Hz (20) 0,005(kHz)

Pulse Width, ps 10-200 0,02

Operating Life Time, h 500 (1000)(pulses)

Power consumption, kWh 0,15 0,1

Weight, kg 10 200

Radiographic images were obtained with a CCD detector developed in the LPI (Fig. 3) [2].The detector was of 0150 mm field of view. The fast neutron screen was made ofa composite material consisting of an organic resin and a powder luminophor (Gd 2O2 S:Tb).A thickness of the used screen was 3 mm.

Due to presence of a powder luminophor in the screen the detector is sensitive also toX-rays. The measurement of intensities of the signals produced by fast neutrons andaccompanying X-rays in the CCD-detector placed at a distance of 15 cm from a generatorshowed that these signals are in a 1:5 and 1:1 ratio for ING-07 and ING-103, respectively.A ratio of signals produced by fast neutrons and by X-ray is changeable by shielding thesource with a lead screen of an appropriate thickness.

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Neutron Imaging Methods to Detect Defects in Materials

3. Results of radiographic measurements and discussion

The results of radiographic measurements carried out with the ING-07 are presented inFigs. 4,5. A fast neutron yield was 3x 1 09 n/s and a source-to-detector distance 15cm. In theseFigs a possibility to get images with both fast neutrons (14 MeV) and X-rays is demonstrated.

In Fig. 4 images of a specimen consisting of polyethylene contaminated with boron andlead disks are presented. In Fig. 5 images of a lead container filled to certain level with waterare shown. The neutron images have been obtained when the generator was screened by a1 0 mm thick lead plate. It is seen that light and heavy materials are quite well observed withX-rays when they are separated in space. Fast neutrons have advantages in revealing internalcontent of a specimen when a light material is screened by a heavy one. Exposure time was2 s for X-ray images and 30 s for neutron images.

Bright spots seen in the images are produced in CCD - matrix by fast neutrons due to athreshold nuclear reaction Si28(n,p)A12 . This noise is quite significant for small exposuretimes. To eliminate the noise a CCD-matrix shielding is being designed at present.

In the case of the ING-103 specific problems concerned with a strong electromagneticpickup were revealed and solved. Radiographic images obtained with neutrons emitted in onepulse were more noisy than in the case of the ING-07 because of comparatively low fastneutron output (5x10 9 n/pulse) of the generator in the measurements. The obtained resultsindicate that perspectives of the ING- 1 03 application for quick processes imaging depend onthe progress in further increase of the generator yield or (and) the neutron detector efficiency.

4. Conclusion

The obtained results have experimentally proved possibility of implementation ofcustomer made generators of the VNIIA for fast neutron radiography. A quite low exposuretime, weight, power consumption, rather high neutron yield, and environmental safety makethem very perspective for the use in industry.

Imaging with X-ray from the same sources have been demonstrated too. Makingradiographs both with X-rays and fast neutron with the same source and at the sameconditions allows to make a more reliable conclusion about a specimen content.

Increasing an efficiency of the fast neutron detector can obviously improve the equipmentperformance. Further improvements of the equipment are concerned with adapting ofgenerators design and experimental conditions for radiography measurements.

Acknowledgements

The authors appreciate support of the \ork by the International Atomic Energy Agency (IAEA).(CRP `Bulk Hydrogen Analysis using Neutrons").

References

1. Bobylev V.T, Bogolubov E.P., Hasaev T.O., et. al. Proceedings of the 5-th WorldConference on Neutron Radiography. (June 17-20, 1996, Berlin, Germany). Edited by C.O.Fischer, J. Stade, W. Bock. DGZfP, 1997, pp.5 19-523.

2. V.Mikerov, W.Waschkowski. "Fast Neutron Fields Imaging with a CCD-basedLuminescent Detector", Nuclear Instruments and Methods in Physics Research, Vol. A424,1999, p.4 5-5 2.

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Ne utrort Irmagitng .Afethod to Detect Defects in Mfaterials

fIelsma Focus

:i1 iUr 1. last ricutic3l generator ( NG- 10T3) writh a plsm tIc us tube

, panel we.

tlo e 2. a neulti[ron genetzratorP Q:NG 7) wNithz cr c lemaring rutbe

72; Inzte,'na~crt~{onf eRa IS . .......... ('onh'rencc Nudear t:; r a pe '

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Neutron Imaging Methods to Detect Defects in Materials

i I

H e ~~~54

~~~ .~~~~~~ ~6

1 2 >

Figure 3. 1 CCD-detector design. I -CCD-matrix, 2 - lens system, 3 - mirror,4 - luminescent screen, 5 - sample, 6 - image intensifier

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Neutron Imaging Mfethods to Detect Defects in Materials

B iorated

PE

Hole

Figure 4. X-ray (left) and fat neutron fright) radiography) of a sarrple consisti qg of a boronpolyethylene plate of 10 mm thickness with 3.5 mm thick lead disks 08r mm and 011 mnm)anid a hole. Exposueime: 2s (N-rays); 30 S (FN).

Leadcontainer

Air gap-

Water -

Cylider ~bottom

Figure 5. X-ray left) and fast neutron (righlt) radiography of a lead container (externaldiameter - 52 mm. wall thickness - 1nmm) tilled waithi water. Exposture time: 2s (X-Iays);30s (TN).

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E 1limiiliii Mlii liiiNuclear Energy in Central Europe 699 S10200096Portoroi, Slovenia, 6 to 9 September, 1999

CALIBRATION OF QUANTITATIVE NEUTRON RADIOGRAPHYMETHOD FOR MOISTUE MEASUREMENT

Toma2 Nemec, Robert JerajReactor Physics Division, "JofefStefan" Institute, Jamova 39, 11]] Ljubljana, Slovenia

e-nmail. [email protected]

AbstractQuantitative measurements of moisture and hydrogenous matter in building materials by neutron radiography(NR) are regularly performed at TRIGA Mark 11 research reactor of "Josef Stefan' Institute in Ljubljana.Calibration of quantitative method is performed using standard brick samples with known moisture content andalso with a secondary standard, plexiglas step wedge. In general, the contribution of scattered neutrons to theneutron image is not determined explicitly what introduces an error to the measured signal. Influence of scatteredneutrons is significant in regions \vith high gradients of moisture concentrations, where the build up of scatteredneutrons causes distortion of the moisture concentration profile. In this paper detailed analysis of validity of ourcalibration method for different geometrical parameters is presented. The error in the measured hydrogenconcentration is evaluated by an experiment and compared with results obtained by Monte Carlo calculation withcomputer code MCNP 4B. Optimal conditions are determined for quantitative moisture measurements in orderto minimize the error due to scattered neutrons. The method is tested on concrete samples with high moisturecontent.

1. INTRODUCTIONQuantitative measurement of moisture in porous building materials is important for civilengineering and building materials industry. Qualitative detection of moisture by neutronradiography (NR) is well established. For quantitative measurements recorded neutron imageneeds to be corrected for various contributions of neutron beam components. Quantitativemethod is calibrated by standards with known moisture content. Using the calibration curvewe can convert the corrected signal into hydrogen concentration values [1]. Influence ofscattered neutrons to the image formation has to be determined and subtracted from measuredsignal to obtain the signal of transmitted neutron beam.

Quantitative measurements of moisture and hydrogenous matter in building materials areregularly performed at TRIGA Mark 11 research reactor of "Jozef Stefan" Institute. Ourquantitative method is calibrated with standard samples with known moisture content andwith a secondary standard, plexiglas step wedge. Contribution of scattered neutrons to theneutron image is not measured explicitly but is taken into account through the calibrationcurve. This simplification introduces an error to the measurements due to signal of scatteredneutrons. This error is low enough for thin samples at low moisture concentrations while atincreased concentrations of moisture the scattered component prevails over the transmittedcomponent and then the calibration is not correct. Influence of scattered neutrons to the imageis significant in the regions with high gradients of moisture concentrations, where build up ofscattered neutrons causes distortion of the moisture concentration profile [2].

In this paper a detailed analysis of validity of our calibration method for differentgeometrical parameters is presented. Optimal conditions for quantitative measurements aredetermined by an experiment. The error in the concentration profiles at regions with highgradients is estimated by the experiment and also by Monte Carlo calculation. Improved

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Neutron Imaging Methods to Detect Defects in Materials

method with minimized error due to scattered neutrons is tested on concrete samples withhigh moisture content.

2. QUANTITATIVE METHOD FOR MOISTURE DETECTION

For quantitative determination of the moisture content at position (x, y) in a thin sample ofwell defined geometry and thickness d, the attenuation of a collimated neutron beam (D/(D0 isideally correlated with the mass concentration C, of water:

'$(xy) = I00(xly) exp[- (Vtm + GV Cw(xy) ) pm d ] (1),

where 1-tm and Vt, are the neutron macroscopic mass attenuation coefficients of the materialand water, respectively. Using a detector with linear dependence of observed detector signalon the neutron exposure dose [3] we get:

S=k(t =k(Dotexp[-(I,,m+tCw)pmd] (2),

where S is the detector signal at certain coordinates (in units PSL mm-2 for imaging platedetectors), k is the detector sensitivity and t is the exposure time. However, in a real case, therecorded signal S' includes also the background due to gamma-rays, epithermal neutrons andneutrons scattered in the sample (S,, SCp and S, , respectively):

S' = S + Sy + Sep + Ss (3).

Background components need to be subtracted from recorded signal to obtain S and then logS is proportional to the moisture concentration C,. The effects of the background due to y-rays and epithermal neutrons can be estimated by imaging neutron beam, where thermalneutrons are filtered out with a filter made of boral and gadolinium plates. Results of themeasurements need to be corrected for neutron beam nonhomogeneities. The effect ofscattered neutrons, primarily due to scattering on hydrogen, increases with the mass thicknessof hydrogen. However, the influence of scattered neutrons on contrast becomes small enoughat increased distance between the sample and the detector [4].

2.1. Calibration of quantitative method

Calibration is performed with a series of standard samples with known moisture content (inthe range I to 14 wt % for red brick samples). NR image of the standards is performed in thesame experimental conditions as actual measurements. The homogeneity of moisturedistribution in the standards is checked by NRP and is varying by less than 0.5 wt %. Standardsare enveloped in Al foil to prevent moisture evaporation and the weight control during 1-2days shows that weight loss of samples is negligible. For routine measurements a secondarystandard is used, plexiglas step wedge (0.5 to 5 mm thick, 0.5 mm steps). Standard stepwedge is intercalibrated with the set of standard building material samples.

2.2. Contribution to the NR image of neutrons. scattered in the sample

Contribution of scattered neutrons to the neutron image is not measured explicitly but is takeninto account through the calibration curve. This simplification introduces an error to themeasurements because signal of scattered neutrons is added to the signal of transmittedneutrons and detection sensitivity is decreased. This error is negligible small (compared tocontribution of background) for thin samples at low moisture concentrations (1-10 wt % H20for 2 to 2.5 cm thick red brick samples). However, at increased moisture concentration thescattered component can prevail over the component of transmitted thermal neutrons and insuch conditions the calibration is not correct. Influence of scattered neutrons to the image isimportant in regions with high gradients of moisture concentrations, e.g. at the front ofadvancing water in porous sample where build up of scattered neutrons causes the distortionof the moisture concentration profile. This effect is significant also at low enough moisture

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Neutron Imaging Methods to Detect Defects in Materials

concentration where our calibration procedure is valid. To diminish the contribution ofscattered neutrons to the NR image appropriate distance between the samples and the neutronimaging detector must be taken.

3. EXPERIMENTAL

3. 1. Neutron radiographv using neutron sensitive imaging plates

Neutron radiographic examinations of samples are performed in the NR facility in the thermalcolumn of the TRIGA Mark II research reactor in Ljubljana. Characteristics of neutron sourcewere described in the literature [1, 5]. For neutron imaging FUJI imaging plate neutrondetector (IP-ND), which is very suitable for quantitative measurements because of the linearresponse in wide exposure range, good spatial resolution and high sensitivity, is used.Characteristics of JP-NDs are presented in literature [1, 3]. Exposure times at thermal neutronflux of 4105 cm2 s-' ranged from 1 to 60 s. Contribution of gamma ray and epithernalneutrons to the NR image was found to be up to 14 % of the total signal in the neutron beam.The statistical error in the detector signal ranged from 1.5 to 3 %.

3.2. Monte Carlo simulation

Monte Carlo (MC) simulations of NR experiments are performed using MCNP 4B computercode [6]. A parallel neutron source of the same size as the cross-section area of theinvestigated object was defined, with the counting resolution of 1 mm. The source withMaxwell type spectrum with E=0.025 eV was assumed. Statistical error was below 0.5 % forprimary neutron and increases to a few % for neutrons scattered in the area around the sample.Neutron contributions to the NR image were determined separately as primary (undisturbed ortransmitted) and total neutron flux which is the sum of the primary and neutrons scattered inthe sample. Detected signal was normalized to I source particle.

3.3. Investigated samples and standards

Calibration with standards was performed in investigation of moisture transport in red bricksamples [7]. Standards for calibration were prepared from same material and with the samethickness and moisture concentrations as investigated samples. Standard step wedge was cutfrom commercial plexiglas. Concrete samples were prepared according to standard procedurefor concrete impregnation tests. Samples for MC simulations were defined with the samedimensions as the samples investigated in NR experiments. Composition of plexiglas andconcrete was taken from literature and samples were assumed to be uniform in the volume.

4. RESULTS AND DISCUSSION

4.1. Error in the calibration curve due to contribution of scattered neutronsBy calibration curve the detector response was correlated with hydrogen concentration instandards. Calibration curve with standards of known moisture content is shown in Fig. laand calibration with plexiglas step wedge in Fig. lb. Neutron attenuation profiles (measuredin NR images) were corrected for contribution of background. In Fig. lc calibration curves forplexiglas step wedge obtained by MC simulation are shown. Object-detector distance in Fig.Ia varied from 0 to 10 cm, while in Fig. lb and in Fig. lc this distance was 1 cm. Fromcalibration curves in Fig. Ia it is seen that effect of scattered neutrons build-up increases withapproaching of samples and detector. At distance 10 cm linearity exists up to 10 wt % H20

but at higher concentrations the error in calibration due to scattering is noticed. At shortdistances the calibration curves are not linear. The calibration curve in Fig. lb is linear from0.5 to 4.5 mm thick plexiglas at only 1 cm from the detector. In Fig. lc (MC simulation)linearity is observed both for transmitted (direct) component and also for the total neutron

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Neutron Imaging Methods to Detect Defects in Materials

flux. From Figs. lb and lc we can see that calibration is valid in limited range of hydrogenmass thickness even with scattered component present in NR image. Calibration is valid onlyat specific experimental conditions which need to be determined separately for every type ofscattering samples and precise experimental geometry.

4.2. Resolution degradation due to scattering in area of high gradients of H mass thicknessNR and MC simulation images of plexiglas step wedge covered in part by Gd filter arepresented in Fig. 2 together with the measured profiles of neutron attenuation along the wedgeand below the Gd filter. The signal recorded by the detector below the Gd filter in NR image(Fig. 2a) is caused by neutrons scattered in the plexiglas wedge. Profile of sharp edge of Gd isdistorted due to scattered neutrons. For comparison a MC simulation was performed in thesame geometry as the NR experiment and signals due to transmitted and scattered neutronswere distinguished. Results of MC simulation in Fig. 2b are very similar (distribution ofscattered neutrons below the Gd filter) to the NR measurements. When object-detectordistance is increased this distorting scattering effect vanishes but at same time NR imageresolution is worsened by the geometrical unsharpness caused by divergence of neutron beam.Geometrical unsharpness is not seen in MC simulation where parallel neutron source wasdefined.

4.3. Comparison of NR experiment and MC simulation

In Fig. 3 images by NR (a) and MC simulation (b) imaging of sharp moisture front in aconcrete sample (7.1 by 3.5 cm, 1.4 cm thick) placed 10 cm from the detector are seen.Measurement of moisture in concrete is difficult due to nonhomogeneity of material and highcontent of bound water in concrete. The MC image profiles taken across the border of wet anddry areas are shown in Fig. 3c. At this distance from detector the scattering background isbelow 10% of total signal and is uniform so we can subtract it from the image. Resolutiondegradation is not significant.

This experiment shows the clear advantage of using MC simulation as complementarymethod to NR experiments. By MC we distinguish between transmitted and scattered neutroncomponents and obtain results at better contrast with subtraction of scattered component fromthe image. These MC simulations were ideal cases and did not match exactly the realconditions at NR imaging. Shape of neutron spectrum was not determined and by assuming aMaxwell type spectrum results differ from the NR measurements. Other simplificationsinclude the assumed homogeneous composition of investigated materials and their elementalcompositions, which were not determined by elemental analysis.

5. CONCLUSIONSResults presented in the paper clearly illustrate that neutrons, scattered in a hydrogenoussample, cause the degradation of contrast and spatial resolution of neutron radiographicimage. Contribution of scattered neutrons may not be neglected in quantitative measurementsand it must be determined separately to estimate the error in measured 1I concentration valuesdue to scattering component. One way to lower the influence of neutron scattering on imagecontrast is by increasing appropriately the object-detector distance. When calibration isperformed with standards placed several cm from the detector the detected signal is linearwith the moisture concentration in wide range but with object and detector in contact, thescattering component can be greater than the transmitted component making impossible the Hmeasurement. By MC simulations we found that calibration is valid in limited range evenwhen scattered neutrons are present in the image what allows H measurement without theelimination of scattered neutrons from the NR image. In areas with sharp gradients of Hcontent the resolution is degraded. By increasing the object-detector distance the distortion by

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Neutron Imaging Methods to Detect Defects in Materials

scattering will decrease but the image resolution is worsened by geometrical unsharpness. Ascompromise, an optimal distance has to be determined for every specific hydrogenous sample.

Investigation of scattering in standard hydrogenous objects by NR and MC simulationsshowed that in specific experimental conditions the calibration with standard samples andplexiglas step wedge enables quantitative measurements of H concentration in porousbuilding material samples. Scattering and background contributions limit the sensitivity of themeasurements. This is a problem when concrete samples with high moisture content andnonhomogeneous structure are examined. So far NR imaging of concrete was limited toqualitative or semiquantitative measurements with low resolution. Future work will be todevelop the method to enable NR imaging by subtracting the scattered component what willincrease very much the sensitivity of H detection in concrete and enable quantitativemeasurements. MC was found to be a very useful tool in evaluation of the NR results and willbe used in future for simulation of other NR experiments.

REFERENCES

[I] T. Nemec, J. Rant, M. Kaling, Recent Results of Near Real Time Measurements ofMoisture by Quantitative Neutron Radiography Methods, Proc. 4th Regional MeetingNuclear Energy in Central Europe, Bled, 1997, 314-320.

[2] M.R. Hawkesworth, Neutron Radiography: Equipment and Methods, Atomic EnergyReview, 15 (2), 1977, 169-220.

[3] J. Stade, J. Rant, M. Kaling, Imaging Plates as Detector for Neutron Radiography,Materialpriifuig, 40 (1-2), 1998, 16-20.

[4] F. Peterka, H. Bock, H. Pleinert, Neutron Radiography Standard Testing Method for theMoisture Analysis in Building Materials, Neutron Radiography (4), Proc. 4ah World.Conf, San Francisco, June 1994, Gordon & Breach Pubi. Co., 1994, 75-82.

[5] T. Nemec, J. Rant, E. Kristof, B. Glumac, Characterization of the Ljubljana TRIGAThermal Column Neutron Radiographic Facility, Proc. 2nd Regional Meeting NuclearEnergy in Central Europe, Portoroz, 1995, 161-167.

[6] J. F. Briesmeister, Ed., MCNP - A General Monte Carlo N-Particle Transport Code,Version 4B, LA-12625-M, Los Alamos National Laboratory, 1997

[7] T. Nemec, J. Rant, V. Apih, B. Glumac, Study of Building Materials ImpregnationProcesses by Quasi-real-time Neutron Radiography, Nucl. Instr. Meth. A, 424, 1999, 242-247.

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Neutron Imaging Methods to Detect Defects in Materials

7.0 object - - 0 cm o measured valuesdetector 5.0 ' o s distance -*.. 3 cm

* cm E----- linear regression curve-A, 10 cm E

E 6.5 4.8a. -. ~~~~~~~~~~~~~~.

O 6 0 \V 4C -

4.45 .5 -_ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _

0 3 6 9 12 15 0 1 2 3 4 5moisture content [vt %] wedge step thickness [mm]

a) b)

-1 3.2 - neutrons-13 4 ~~~0.99891 oa

m total

o direct-13.6- R= -0.9999 '3

j, -1 3.8 -

: ~~linear regression curves ) -14.0

y-1 3.1 2-0.180x a) a

-142- --- y= -13.14 -0.21 3x '

0 1 2 3 4 5wedge step thickness [mm]

c)

Figure 1. Calibration curves used to determine the correlation between detector response andhydrogen concentration. Calibration by red brick standards with known moisture content (a),measured at varying distance from IP-ND. Calibration with standard plexiglas step wedge0.5-5 mm thick placed 1 cm from detector, obtained by NR (b) and by MCNP simulation (c).

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Neutron Imaging Methods to Detect Defects in Materials

250- .!- -C-l signal neutrons

200 2.0x0 'total

E d.0x10' - - - direct

1 50 - ...e.g.asscatteredpeiasstep wedge

loo - 1.0x104

50- ___ - -wedge, filtered by Gd

0 20 40 60 0 20 40 60 80position [mmi position ImmI

a) b)

Figure 2. Degradation of neutron image resolution due to scattering in areas with highgradients of H concentration. The object is plexiglas step wedge which is filtered by 100 gmthick Gd stripe in upper part: (a) NR image and neutron attenuation profiles along the wedgeand below single Gd (lower part of wedge is covered by two Gd stripes), b) image by MCNPsimulation. Object-detector distance is 1 cm. Below are shown: (a) the neutron attenuationprofiles and (b) contributions of individual components calculated by MCNP (around theobject the signal is caused only by scattered neutrons).

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Neutron Imaging Methods to Detect Defects in Materials

a)

2.0x10"- detected neutrons-total

- - -direct1.5x10 ----. scattered

1,1 1.0xl 07'4

0.00 20 40 6 80 100

Position [mm]i

I) c)

Figure 3. NR and MCNP images of wet concrete sample at object-detector distances 10 cm,contrast is increased: a) NR image of wet and dry concrete samples in close contact to simulatesharp edge of water front, b) MCNP image of concrete sample wet to 1 half, in c) are shownprofiles of total and scattered contributions. Profiles are noisy due to statistical error.

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. I 1||Rl11 1 PHI ~~~~~~~~~~11111 IlmIIIIIHII l iiillR111 |11Nuclear Energy in Central Europe '99 S10200097Portoro2, Slovenia, 6 to 9 September, 1999

A New CCD-Camera Neutron Radiography Detector at theAtominstitute of the Austrian Universities

S. Korner ), 2), H. B6ck ', H. Rauch `. E. Lehmann 2)

1) Atominstitute of the Austrian Universities, Stadionallee 2, A-1020 Wien, Austria2) Paul Scherrer Institute, CH-5232 J illigen PSI, Switzerland

Abstract - Neutron radiography provides a very efficient tool for non - destructive testing as well as formany applications in fundamental research. A neutron beam penetrating a specimen is attenuated by the samplematerial and detected by a two dimensional imaging device. The image contains information about materials andstructure inside the sample because neutrons are attenuated according to the basic law of radiation attenuation.At the Atominstitute of the Austrian Universities neutron radiographic examinations have been carried out formore than 35 years, mainly with detectors consisting of X-ray films and a Gd - converter enclosed in a vacuumcassette. Presently a neutron tomography set - up is under development. For high quality 3D imagereconstruction, about 200 digitized neutron transmission images from different angles of the object arenecessary. Therefore the first step was the design of an adequate electronic neutron radiography imaging device.The requirements for a detector suitable for neutron tomography are: exact and reproducible positioning, easyhandling, high spatial resolution and dynamic range, high efficiency and a good linearity. The key componentsof the detector system selected on the basis of this requirements consist of a neutron sensitive scintillator screen,a cooled slow scan CCD-camera and a mirror to reflect the light emitted by the scintillator to the CCD-camera.The whole assembly is placed in a light-tight enclosure. In this paper the strategy of the selection of theindividual detector components is described. Comparisons on the influence of the use of different componentson the properties of the whole position sensitive imaging device are demonstrated. Finally the new CCD-cameraneutron radiography detector of the Atominstitute is presented and first results of test measurements performedat the neutronradiography facility NEUTRA at the continuos spallation source SINQ at Paul Scherrer Instituteare shown.

1 Introduction

At the 250 kW TRIGA Mark II reactor at the Atominstitute of the Austrian Universities twoneutron radiography (NR) stations are available. The main characteristics of these twofacilities are shown in Table 1:

STATION 1 STATION 2FLUX DENSITY (cM-2SnY ) 3. 1 05i

L/D-RATIO 50 125

BEAM DIAMETER (cm) 40 9

Cd - RATIO 3 20

Table 1: main characteristics of the NR-facilities at the Atominstitute

Since 1964 , NR-activities at the Atominstitute encompass both research oriented work aswell as non-destructive testing for various users [1]. Presently the point of main emphasis inNR-activities at the Atominstitute is set on the development of an experimental set-up forneutron tomography. For a 3 dimensional reconstruction of the sample interior, 2 -dimensional transmission images taken from different view angles are required [2]. Thequality of the tomography depends strongly on the number of images from different viewangles [3]. Good results can be obtained by rotating the object in the beam by 180 degrees

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Neutron Imaging Methods to Detect Defects in Materials

with 0.9 degree-steps [4]. Hence it follows that for a high quality 3 - dimensionalreconstruction of a sample, 200 2 - dimensional transmission images from different viewangles of the specimen are required. Therefore the experimental set-up for neutrontomography consists of the neutron source with a collimator, a rotary table for the rotation ofthe object, a proper detector and a motion control system which coordinates the rotary tablewith the detector.

The detectors presently mainly used for NR at the Atominstitute consist of X-ray films and aGd-converter enclosed in a vacuum cassette. After each exposure, the film has to bedeveloped and the image is digitized by a scanner. It is obvious that such a detector is not thebest choice if an application requires 200 digitized images per sample. Therefor the first stepof the development of an experimental neutron tomography set-up was the selection andoptimization of a proper detector. This paper shows the requirements for a detector suitablefor neutron tomography. It presents the basic principle of the chosen detector system, thestrategy of the selection of the individual detector components, comparisons on the influenceof the use of different components on the properties of the whole imaging device and resultsof first test measurements.

2 Requirements for the Selection of Detector Suitable for Neutron Tomography

Due to the tremendous influence of the number and quality of the transmission images of theobject on the result of the 3 dimensional reconstruction, the demands for a proper detector asone of the key components of the neutron tomography set-up are extremely high:1. Exact and Reproducible Positioning:It is evident, that for all exposures of one sample (from different view angles), the detectorneeds to be in exactly the same position. Corrections of different detector positions during thereconstruction calculations would be very time consuming, not precise and for many caseseven impossible.2. Easy Handling:The enormous number of digitized images needed for each tomography requires a detectorthat can be controlled according to the rotary table by a computer to automate the whole set ofmeasurements needed for the tomography of each sample. Also the digitization of the imagedata should be automated and not cause additional work.3. High Efficiency:In order to save time it is extremely important to reduce exposure time.4. High Spatial Resolution, Large Dynamic Range. Good Linearity:These items are always very important for the quality of images gained by NR. But theinfluence on the quality of neutron tomography is even higher.

3 Selection of the Detector

A comparison of the above requirements with the performance of x-ray film combined with aconverter immediately shows that another detector has to be developed. Exact positioning isquite difficult as after each exposure the enclosure of film and the converter has to be removedand opened to change the film. Additionally this is quite a time consuming procedure,especially as all 200 films have to be developed and scanned. Also the exposure time by usingfilm is quite high. Dynamic range and linearity are poor. Only the spatial resolution issatisfying. Other detectors extensively used for NR are neutron sensitive imaging plates (IP)[5]. They are made of a storage layer (sensitive crystals) doped with Gd. After the exposure aspecial scanner is used to read out the information stored in the IP. The advantages of IPscompared to film are a higher dynamic range, better linearity and a higher sensitivity. The

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Neutron Imaging Methods to Detect Defects in Materials

spatial resolution is not quite as good as for images taken by film, but it is still reasonable. Butregarding the requirements of exact and reproducible positioning as well as the handling,almost the same difficulties occur as with the use of the film technique.Another neutron sensitive imaging device is a CCD-camera combined with a scintillatorscreen. It fulfills all the requirements for a detector suitable for neutron tomographyinvestigations. As the detector has not to be removed between the exposures the demand ofexact positioning during one set of images is fulfilled. The detector is controlled by acomputer and can easily be connected with a computerized motion control system of therotary table. Image data are digitized and can immediately be used for the 3 dimensionalreconstruction. Compared to film the efficiency is much higher, the dynamic range is largerand the linearity is better. The spatial resolution depends strongly on the lens, the size on thechip and the distance between scintillator and camera. The resolution limit is set by thescintillator screen in the range of 200gm.

4 Design of a CCD-Neutron Radiography Detector

neutronbeam

objectscintillator

lens

CCD-camera

mirror computer

light tight box

Figure 1: set-up of a CCD-camera neutron radiography detector

The neutron beam reaches the neutron sensitive scintillator screen after penetrating thesample. The light emitted from the screen is reflected to the camera by a mirror and focusedon the CCD-Chip by a lens. These components are located in a light shielded tube togetherwith shielding components to protect the CCD-camera from neutron and y-radiation. TheCCD-camera is connected to a computer to read out the information stored by the CCD-Chipand to reconstruct and process the digitized image data obtained with the imaging device offigure 1 [6].

5 Selection of the Key Components for the CCD-Camera Neutron RadiographyDetector

Because the CCD-camera is the most sophisticated and expensive key-component of thisimaging device , it has been selected first and the rest of the components have been selected ormanufactured according to the boundary conditions following from the choice of the cameraand from their interactions with each other.

5.1 CCD-CameraTo fulfill the demands of high sensitivity, a large dynamic range and a good signal to noiseratio, a nitrogen cooled slow scan CCD-camera with a thinned SITe S1502A chip has beenchosen. The pixel array format of this chip is 512 x 512 pixels with a pixel size of (24 x24)pim. The Quantum Efficiency of the CCD-camera is in the range of 80 - 90 % for wavelengthsfrom (350 - 800) nrm, as shown in Figure 3. The high precision CCD driver electronics

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Neutron Imaging Methods to Detect Defects in Materials

provides 16-bit digitization (65535 gray levels). Figure 2 shows the correlation of thetemperature of the CCD-chip with the dark-current. To obtain this curve, images withoutneutrons and with closed camera shutter have been made at different CCD-temperatures. Forthe ideal case for each image a gray-level close to zero in each pixel is expected (due tostatistics, dark current, read out noise and the influence of background radiation, which causeswhite spots in the image, the mean gray-level within a dark picture can never get zero). Figure2 shows that for ,,high" CCD-temperatures this value is far away from zero, but for lowerCCD-temperatures the value of dark-current decreases rapidly.

8r0----- __ --- D -jf 00;00 80 -- m~f''~---~t _-R~ntRF 0 , 60000

70 - - -I- - ~~~Fnmt owminae > 50000t~f~~p:i; i05{ :i09t0;if tt0:0;fi-;X;:if °40000 -

s0 --- n o ::-- -0-Thirmdn-' 3000020000

340 - 100001t J1 -- 0- .b .e .io~~U - hmedUAR

00 0 ;,, 0000 .0d0 o

N f4, VXPi 11 c &000 oh X , 0 0 X g X O- -Figure sensiti:ity ffln~fion of Figure CCD-Temperature

Wavedmot in:S

Figure 3: spectral sensitivity function of Figure 2: dark-current depending on theSITe chips temperature of the CCD-chip

5.2 LensAs the light transmission should be maximized and picture distortion has to be avoided, thehigh quality of the lens is extremely important. The desired image size is about (20-25) cm2.The available space beside the facility is less than 1.3 m. Based on this boundary conditions aNikon NOKT 58 mm F 1,2 lens has been chosen. Figure 4 shows that the light intensitydecreases for smaller apertures. From one aperture to the next one (i. e. from 1.2 to 2) it isabout a factor of two. This means that the sensitivity of the detector increases tremendously ifan open aperture (1.2) is used. But for this case the distance has to be adjusted very carefully,because with a completely open aperture the image is blurred more easily.

40000

35000 itji _ = -_=

Q 30000 -l _ - _

t 25000 =

20000 f _C 15000 =_ . -

E 10000 -

5000 -_-_ --____

0 5 10 15 20Aperture

Figure 4: detected light quantity vs. aperture

5.3 MirrorThe demands for this detector component are a high reflectivity (95 %) of the light emitted bythe scintillator, generation of as few y-rays as possible and no lasting activation of thematerials of the mirror. According to that a 2 mm thick glass plate coated with Al and withTiO2 as protecting layer was manufactured at the Paul Scherrer Institute (PSI) in Switzerland.

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Neutron Imaging Methods to Detect Defects in Materials

5.4 BoxA light shielded tube which also serves as a positioning device for the detector componentshas been designed according to the boundary conditions given by the size and appearance ofthe individual detector components, the desired image size and the space available at thefacility. The material for the whole box is Al to avoid lasting activation. It has beenmanufactured at PSI. Light tightness of the box has been successfully tested. The image sizeis (21 x 21) cm.

5.5 Neutron Sensitive Scintillator ScreenAccording to the spectral sensitivity function of the selected chip, a neutron sensitivescintillator screen with a suitable emission spectrum had to be found. Four adequate neutronsensitive scintillators have been compared:

1. Bicron 705: ZnS(Ag)-6 LiF2. Kasei Optonics3. Levy Hill: ZnS(Ag)-6 LiF4. NE 427: ZnS(Cu)-6 LiF

The detection mechanism is: 3Li + n 3 H + ' 2He + 4,78 MeVAll test - measurements have been performed at the neutronradiography facility NEUTRA atthe continues neutron spallation source SINQ at Paul Scherrer Institute in Switzerland [7].

neutron flux -3x10 6cm~2s-'

mean neutron energy 25 meVCd - ratio 16

L/D 550beam diameter 35 cmy - background 1,5 mSv / h

Table 2: main characteristics of the neutronradiography facility NEUTRA at PSI

The following issues have been investigated separately for each of the four neutron sensitivescintillator screens:

5.5.1 Efficiency and Linearity

To compare the efficiency and linearity of the whole CCD-camera NR detector depending onthe choice of the scintillator, series of open beam measurements with different exposure timesfor each scintillator were made. From each of these images, the mean gray-level wasdetermined (the gray-level is higher for a brighter image, respectively for longer exposuretimes, and vice versa).

60000 *X a

50000

, 40000 : *Bicron

30000 E* * Kasei

cc, 20000 A . * *Levy HillE 10000 XNE

01

0 10 20 30Exposure Time (sl

Figure 5: linearity and efficiency: dependency of the mean gray-level on the exposure time

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Neutron Imaging Methods to Detect Defects in Materials

Figure 5 demonstrates the good linearity of this imaging device independing on the choice ofthe scintillator. Small deviations from the linear increase of the mean gray-level with theexposure time are most likely caused by small neutron flux fluctuations at the facility.Besides, Figure 5 shows that the detector has the best efficiency with the Levy Hill or the NEscintillator screen.

5.5.2 Spatial Resolution:Due to the size of the CCD-chip , (512x24) gm x (512x24) rlm, and the size of the sensitivearea of the detector, (26.3 x 26.3) cm2, the area seen by one pixel is (513 x 513) gm2. As theinherent resolution of neutron sensitive scintillator screens are usually in the range of 200 pm,the choice of the scintillator should not affect the spatial resolution of the whole imagingdevice. With each of the four scintillators a knife edge-object (edge of a Gd foil) has beenmeasured. From these images the modulation transfer functions (MTF) were determined andcompared (Figure 6) [8].

1.0v -

0.8- 0.8 -~ ~ ~ ~ -- BICRON

KASE10.6 -+--LEVY HIL

MTF _NE0.4-

I ~ ' I I

0.0 0.5 1 0 1.5 2.01p [mm

Figure 6: modulation transfer functions (MTF) of the detector obtained with differentscintillator screens

5.5.3 Inhomogeneities of the Scintillator Screens

The four neutron sensitive scintillator screens have been compared regarding the homogeneityof their light-emission. For each scintillator an open beam image has been investigated thefollowing way: The image has been subdivided in small areas of interest (AO). In each of thisarea the mean gray-level had been derived. Figure 7 shows that only the BICRON scintillatoris quite inhomogeneous. The fluctuations of the mean gray-level in the AOIs of the otherscintillators appear periodically and on the same position for each scintillator and thereforseem to come from the beamprofile.

70000

60000

50000 - BICRON

> 40000 - ° KASEIlo <X> O A . LEVY HILL

E 30000 -C, ~ ~ ~ ~ O

20000

10000

0

0 10 20 30 40Number of the AOI

Figure 7: homogeneity of the scintillator screens

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Neutron Imaging Methods to Detect Defects in Materials

5.5.4 After Glow of the Scintillator Screens:

To determine the after glow of the neutron sensitive scintillators, the screens have beenexposed to the neutron beam for one hour. After closing the neutron shutter several imageshave been taken with the CCD-detector to observe how long the scintillator emits light afterexposure. Figure 8 shows that the after glow of the scintillators depending on the time afterexposure is quite fast, especially for the Kasei Optonics and the Levy Hill scintillator screens,and the effect of the after glow as an disturbing effect for the following neutron radiographicimage can be neglected for most applications, as this effect is very small compared to therange of 65535 gray levels of a neutron radiographic image taken with this detector system.

4500 - i 1 1120

> 430_00 =-cro ____n_______ Kasel1100 -500 - 1080-

13000 '_-_ 1_000

0~ 200 400 600 800 200 400 600 8001060

2500

! 1040--(D 2000 -- ____ ___ _ (0

1500 _ __ __1020 -

__ t1000 -

0 200 400 600 800 0 200 400 600 800

time [a] time [s]

2500

2 200 --- _ _ _ _ __ _ _ _ _ _

2000 8200 _______- NEn 100 -- Levy Hill i 2000 h

-j _ 7 .., ~~~~~ ~~~~~~~~~1800 _ _ _ _ _ _ _q1000 -. - 1600

6, D a1400 1200

0 .1000

0 200 400 600 800 0 200 400 600 800

time [hd] time [a]

Figure 8: behavior of the emission of light of the scintillators after the exposure to neutrons

After this large series of test measurements and comparisons of different scintillator screens, aneutron sensitive scintillator by Levy Hill (ZnS(Ag)-6LiF) has been selected for the newCCD-camera NR detector at the Atomainstitute.

6 Conclusions and Outlook

A new CCD-camera NR detector has been designed, optimized and tested with the aim ofproviding a tool for scientific and industrial radiography applications requiring highquantitative precision as well as for neutron tomography investigations. The detector consistsof the following key components: The selected camera is an Astrocam. nitrogen cooledslowscan CCD-camera with a thinned SITe S1502A/T chip of the format (512 x 512) pixelsand a pixel size of (24 x 24) Htm 2 and with a Nikon NOKT 58 mm F 1.2 lens. The highprecision CCD driver electronics provides 16-bit digitization (65535 gray levels). A mirrormade of a 2 mm thick glass plate coated with Al reflects the light emitted by a (ZnS(Ag)-6LiF) Levy Hill scintillator screen to the camera. These components are placed in a light-tightbox, made of Al. The image size is (21 x 21) cm2. One camera pixel faces 410 Vtm 2. Thedetector has an excellent linearity and sensitivity. Based on the test measurements performedat PSI, exposure times of 1-1.5 minutes are expected at the NR facilities of the Atominstitute.This means that all measurements needed for one tomography can be made during oneworking day.If a zoom lens would be used, the resolution could be improved on the cost of light-intensity

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Neutron Imaging Methods to Detect Defects in Materials

and image size. For next year the purchase of a Nikon 180mm F 2,8 lens is planned. With thislens we expect to see an area of about (7 x 7) cm2 (if the distance between scintillator andcamera is not changed). The loss of light intensity compared to the 58mrn F 1.2 lens isexpected to be around a factor of 7. The resolution limit given by the lens / scintillator wouldbe in the range of 140 rim, but for this case the resolution limit would properly be set by thescintillator screen in the range of 200 Elm, or even below.

Due to the results of the first test measurements performed at the NR facility NEUTRA atPaul Scherrer Institute, we are confident of having developed a powerful instrument suitablefor neutron tomography investigations. The imaging device will be transferred to theAtominstitute this autumn.

7 Acknowledgments

The authors would like to thank Dr. Schillinger, Techn. Universitat Munchen, Garching,Germany, for fruitful discussions and his ongoing advice, J. Meyer, Gloor Instruments,Switzerland for his support concerning CCD-cameras, P. Vontobel for exchange of ideas andsupport with the experiments at PSI and finally A. Ellenberger also for his help with theexperiments at PSI.

8 References

[1] S. Kdmer, H. Pleinert, H. Bo5ck, Review of Neutronradiography Activities at theAtominstitute of the Austrian Universities, Proc. Of the 5th World Conference on NeutronRadiography, Berlin 1996[2] A. C. Kak, M. Slaney: ,,Principles of Computerized Tomographic Imaging, IEEE Press,New York, 1988[3] J. C. Russ, The Image Processing Handbook; CRC Press, 1995[4] Schillinger, Neue Entwicklungen zu Radiographie und Tomographie mit thermischenNeutronen und deren routinema3igen Einsatz, Dissertation an der Technischen UniversitatMunchen (Thesis in German)[5] M. Thorns, D. Myles, C. Wilkinson, Neutron Detection with Imaging Plates; NuclearInstruments and Methods A 424 (1999) 26-39[6] H. Pleinert, E. Lehmann, S. Kmrner, Design of a New CCD-Camera Neutron RadiographyDetector, Nuclear Instruments and Methods A 399 (1997) 382 - 390[7] E. Lehmann, H. Pleinert, L. Wiezel, Design of a neutron radiography facility at thespallation source SINQ, Nuclear Instruments and Methods A 377 (1996) 11-15[8] J. T. Lindsay, The MTF Method for Neutron Radioscopy Imaging SystemCharacterization, Proceedings of the 4 th World Conference on Neutron Radiography, USA,1992

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j ~~~~~~~~~~~~~~S10200098Nuclear Energy in Central Europe '99Portoro2, Slovenia, 6 to 9 September, 1999

Artefacts of Fast Neutron Radiography Concerned with Neutron Scattering

V.1. Mikerov', A.I. Isakov', A.P. Koshelev 2 ), A.A. Bykov 3 ), V.A. Tukarev',A.I. Khodeev 3 ) and W. Waschkowski 4 )

'P.N. Lebedev Physics Institute of Academy of Sciences of Russia (LPI),Leninsky Prospect 53, Moscow 1 17924, Russia

2A11-Russia Research Institute of Automatics (VNIIA), Moscow 101000, Central Post Office,P.O. 918, Russia

3Russian Research Center "Kurchatov Institute",Moscow 123182, Russiaunich Technical University, D-85747 Garching, Germany

ABSTRACT - The paper considers peculiarities of fast neutron radiography with a two-dimensional detector. Effects produced by scattered neutrons was simulated for various neutronsources. Contribution of y-rays generated in the sample was estimated for a fission spectrum offast neutrons. Feasibility of fast neutrons collimating by a honeycomb collimator wasconsidered.

Keywords: neutron radiography, scattered neutrons, fast neutrons

1. Introduction

Application of a two-dimensional detector in fast neutron radiography makes it muchmore productive. However in this case an image can be effected by scattered neutrons andaccompanying y-rays emitted from the source or produced due to fast neutrons interactionwith the sample and surroundings.

One of the tasks of this work was to get a quantitative estimation of the effects producedby scattered neutrons and y-rays induced in the sample taking into account salient features offast neutron sources which are available at present. The other task was to investigate afeasibility of effective screening of fast neutrons scattered in the sample by a honeycombcollimator.

The following neutron sources were considered: the converter facility of the reactorFRM-1 (Munich Technical University), a neutron generator based on an accelerating tubeING-07 (VNIIA) [1] and a neutron generator with a plasma focus tube (VNIIA).

The following simulation were carried out:

1) Spatial distributions of the detector response to neutrons of different origin:

* non-collided (primary) beam.* beam collided in the sample,* beam collided in the walls of the experimental room,

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Neutron Imaging Methods to Detect Defects in Materials

* beam collided in the source.

2) Distribution of mean energy in the detector plane for the above defined neutrons.

To analyse the problem of fast neutrons beam collimation, the effects produced bysamples, collimators and theirs consequent assemblies were considered. The angulardistribution of the neutrons going forward out from the sample and collimator were evaluatedin the performed calculations. It was assumed that both the sample and the collimator wereunlimited in the plane perpendicular to the primary beam direction.

Effect of y-rays on the radiographic image in the case of the FRM-l source was estimatedtoo. y-rays of inelastic scattering and radiation capture y-rays generated in the sample wereconsidered.

2. Calculation Procedure and Input parameters for Simulations

The calculations - in the case of the FRM-l - were carried out for the real experimentalconditions of radiographic measurements described in [2]. The neutron beam of fissionspectrum was filtered by a combined filter consisting of lead (12.5 cm) and polyethylene(2 cm). A source-to-detector distance L was 5.9 m and a so called L/D (where D is the sourcedimension) ratio was about 80.

In the case of neutron generators, the calculations were performed for mono-energetic(14 MeV) neutrons and a point source. The detector, the generator and the sample were placedin a room (4 m height and 2 m in diameter) along the room axis. It was assumed that the roomwalls were of a 0.5 m thickness and made from concrete. The detector position was fixed at adistance of 0.5 m above the room flour. The calculations were carried out for two source-to-detector distances (15 and 150 cm).

The test sample used in simulations was a cylinder made of polymethylmethacrylate(CH 802) of 4 cm in diameter and 10 cm at height. A sample-to-detector distance in all thecases was 5 mm. Due to the cylinder symmetry a linear detector was used for simulating asample image.

Neutrons scattered both in the sample and in some parts of experimental installations ofdifferent kind were differentiated.

It was assumed that sample imaging was carried out by a luminescent detector based onrecoil protons [3]. The screen of this detector is made of a composite material consisting of anorganic polymer and a pownder luminophor Gd2 0 2 S:Tb.

Simulation of the spatial distributions was carried out in the following way. First, spatialdistributions of fast neutrons of different energy groups in the detector plane was calculatedusing the MCNP-3b code (F5 detector). Second, a response of the screen lx was calculated asl.=ZN.(Ei)a(Ei), where x is the detector co-ordinate, i is energy group, N(Ei) is flux of fastneutrons of energy Es and a(Ei) is cross section of the emitting recoil proton.

A mean energy was calculated as a ratio of energy flux (*F5 detector) to total particlesflux defined as YN,(Ej). To estimate a y-rays contribution to the detector signal energydepositions in the screen material of the detector coursed by fast neutrons and 7-rays werecompared.

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Neutron Imaging Methods to Detect Defects in Materials

3. Results of simulations

3.1. Neutron generator

The results of simulations for a custom made portable neutron generator ING-07 arepresented in Figs. l and 2.

As the neutron beam is a divergent beam the image of the sample edge is not sharp. Theregion of the edge smearing depends on L. It is about 2 mm for L=150 cm and -25 mm forL=15 cm. It can be seen that at a distance of L=15 cm a major contribution of scatteredneutrons is concerned with the sample. At a distance of l =50 cm neutrons scattered in theroom walls prevail. Their contribution in the sample shadow exceeds even the contribution ofnon-collided neutrons.

Spatial distributions of neutrons scattered in the sample and the room walls are rathersmooth. At the same time it can be seen that neutron scattered in the generator influence theimage too without, noticeably, spoiling it.

An image contrast of the sample determined as (Imax-rnin)/(Imax+Imin) in the both cases isthe same (about 0.25). A contrast in the absence of scattered neutrons could be considerablyhigher: about 0.5 for L=150 cm and :0.43 for L=15 cm.

In Fig. 4 a spatial distribution of a mean energy of neutrons scattered in the sample ispresented. It can be seen that a mean energy of scattered neutrons outside the sample is lowerthan inside the sample. The reason is that outside the sample there are neutrons which arescattered at comparatively larger angles and which loose at a collision more energy. Due tothat mean energy of neutrons decreases with an increase of the distance from the sample axis.Comparing a mean energy at the sample edge and its axis one can see that the mean energy atthe edge is higher than at the axis. This is a result of transformation of neutrons spectrum inthe sample due to two processes: 1) scattering in the sample and 2) escaping the sample. Onehas to take into account that the probability to escape the sample is higher for neutronsscattered at larger angles and nearby the sample edge.

The results for the neutron generator with a plasma focus tube are analogous to those forthe ING-07 despite of a different design. Due to that they are not presented in the paper.

3.2. Nuclear Reactor

The results of the calculations show that the contribution of neutrons scattered in thefilter, biological shielding and experimental room is negligible small. Spatial distributions ofthe detector response in this case are presented in Fig. 3. It is very similar to that in the case ofthe ING-07 and L=150 cm. The difference is in the contrast value and in the edge width. Thecontrast of the sample image is about 0.81. It could be 0.87 in the absence of scatteredneutrons. The edge width was found to be tl mm.

The mean energy distribution presented in Fig. 4 demonstrates effect of neutron spectrumhardening behind the sample due to reverse dependence of scattering cross-section on neutronenergy.

3.3. y-rays Contribution

Contributions of radiation capture and inelastic scattering gamma rays concerned with thesample in the case of the FRM-l source were estimated. Energies of y-rays were 2.3 MeV(radiation capture by hydrogen), 4.4 MeV (inelastic scattering by carbon) and 4.7 MeV

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Neutron Imaging Methods to Detect Defects in Materials

(inelastic scattering by oxygen). These V-rays generate in the screen Compton electrons andelectron-positron pairs. An energy deposition of Compton electrons and pairs was comparedwith an energy deposition of recoil protons generated by fast neutrons. Calculation gave thefollowing values of mean energies for the particles: -0.96 Mev and rz2.62 Mev for Comptonelectrons, 1.3 MeV and ,3.4 MeV for pairs, respectively. A mean energy of a recoil proton is1.67 MeV (half of a neutron mean energy, see Fig. 4). The results of calculations shows thatcontribution of radiation capture y-rays to the detector signal can amount to about 20% of thetotal neutron signal. It was found to be about 1,5% for y-rays of inelastic scattering.

3.4. Feasibility of Fast Neutrons Collimating by a Honeycomb Collimator

Evaluated tallies in the performed calculations were angular distribution of the neutronsgoing forward out from:

* a sample unlimited in the plane perpendicular to the primary beam direction,* a honeycomb collimator of reasonable opening made of densely packed tubes,* a sample and collimator placed in consequence along the beam direction.

Table 1. Parameters of honeycomb collimators.

Wall thickness,

Material Length, mm Tube opening, mmmm Type A Type B

Polyethylene 300 2 1 5

Iron 300 2 1 5

PE & Fe collimators 150 (PE) + 150 (Fe) 2 1 5in succession

Simulations of angular distributions were carried out for samples made of iron andpolyethylene of thickness in the range frorn 5 to 15 cm and collimators listed in the Table 1. Itwas assumed that samples were illuminated by a non-divergent beam of fission neutrons.

The obtained results are very similar for any combinations of a sample and a collimator.They are demonstrated in Fig. 4 for a polyethylene sample of 10 cm thickness and ahoneycomb collimator of B type made of iron. It is seen that the angle distribution of neutronsscattered in the sample is very wide. At the same time a thickness of the collimator wallsalong a scattering angle direction is too small to screen these neutrons.

4. Conclusions

The following general conclusions have been drawn out from the obtained results:

* Scattered neutrons influence a contrast and practically do not spoil a spatial resolution ofthe image.

* A contribution of a particular source of scattered neutrons depends on experimentalconditions.

* A honeycomb collimator of any reasonable opening has too thin walls for effectivescreening of neutrons scattered in the sample.

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Neutron Imaging Methods to Detect Defects in Materials

* A primary beam in the case of a two-dimensional detector can be effectively collimatedonly due to a larger collimator-to-detector distance and a smaller angle aperture of thebeam intercepted by the detector.

* All potential sources of scattered neutrons should be taken into account when planningradiography measurements with fast neutrons or interpreting an image.

* Evaluated y-rays contribution is noticeable. The measurements of intensity of y-raysemitted by the sample are necessary to qualify the value of this contribution.

Acknowledgements

The authors appreciate support of the work by Deutsche Forschungs Gesellschaft and the InternationalAtomic Energy Agency. (Co-ordinated Research Program "Bulk Hydrogen Analysis using Neutrons").

References

[1] V.T. Bobylev, E.P. Bogolubov, T.O. Hasaev, et. al. Pulsed Neutron Generators (ING) ofthe VNIIA and Systems on their Base, Proceedings of the 5th World Conference on NeutronRadiography, (June 17-20, 1996, Berlin, Germany). Eds C.O. Fischer, et. al. DeutscheGesellschaftfur Zerstorungfrei Prufung, 1997, pp. 519-523.

[2] V. Mikerov and W. Waschkowski. A Two-dimensional detector for fast neutron fieldsimaging, Proc. V Int. Sem. Interaction of Neutrons with Nuclei, Dubna, 199 7, pp. 269-2 75.

[3] V. Mikerov and W. Waschkowski. Fast Neutron Fields Imaging with a CCD-basedLuminescent Detector, Nucl. Instr. and Aleth., Vol. A424, 1999, pp. 45-52.

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Neutron Imgn eh~cto Detect Dafct in Materials

Total

F :ue1 Spat i :a .^ 9:tf- Gistributial ::,x p00000:00::-P tile ricti:i0-l00: a th: detctoplan fo di:0n, 12; 1 ;;00.4-50A> f-;T- : - -m Crttbuin of.' rieuti-oiis cofie ii t e

6 .*.........

i: t; t [k}.S~~- --- ------------- 0 - f -- 0 ------- ..... .

,0: : : ................................. .. 0et$'.050~'0S:00.: .. ;. :. .;:; 0~~~~~~~~~~~~~~~~~~~~~- ---- - $- -t--X---;--:3--------- :

-C ~ ~ ~ ~ ~ ~~~~~~~CU

L.... X .J. .1-- $--- -- .... '

U.1 a~~~~~~~V4 $t -eyV1 l

Co 1 1i dd b ~ r p~e 0 1 2 3

Figure 1. Spatial distribution (lfxi) of ~tvarious. comnipofnents o00(.}f thle 0neutron lbs ~ in the detectorplane for51 sSour~e- to 0 detecvtor 000dist ance^0 L::15 t$) 0D{)00cm.t 0 Conltribution!ls 0 of lrt icutu s coll i dedl in the

t00 sampllte0, geute:E>rwtr, ank~d room w,400shail3s:; tand:50 o? tl~Hf no-cllidedl neCutron:s jand sum &i co it - 1 ded3 and noan-c00o-t i~tded eurstion1s are pres-tfle0 med. 0 ; 0

1~0 : :

:::: ~ ~ D. ::-.

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Fiure 2. Sptial distrib ion lvx) of vaji ous cornpoenmof th sami trnC g ina the deltectorpliane for sontrce>-so ~deteictor dt~i~stance Ltl 5 c~Tu~~tm. Con~~itributinoets ofa-Vf nleu~tronrs>0 colg0lided in tXXhQXlie Xsampl}e,0 gerlerator, tand rom walSsrilis; adof non0k-Jo~l^Glsded neutronlis and tsuma of tcoi-llided 0and tnon-t collided~ neuterotns are presen~ted. t 0 tt00 tlttllt000900 \tlt 0 \ ; t

752 Jnterniitinnnl Con krcnce Nut few- Ln;000000000000000X0f000000ft 'u ( gnu at Encore '990t~ft00 0

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Neutron Imaging Methods to Detect Defects in Materials

'--TotalA ' 1- _ Non-coll.

es ..; i 4 Sample

_ * * A A A As t

0.0 1 i1.8 1.9 2.0 2.1 2.2

x, cm

Figure 3. Spatial distribution 1(x) of various components of the sample image in the detectorplane for the FRM-1. Contributions of neutrons collided in the sample, non-collided neutronsand sum of collided and non-collided neutrons are presented.

4.0

3.8 -.3' - . . . .. _ : ,,

> L~~~~~~~~ L150 cm ~,3.26- t e Add

3.0 - -

2.8 (-0

2.6-

2.4- 9 \5

2.2- -A-Total

2.0 ' Non-coil. ?.0

1.8 I Coll.0 1 2 3 4 5 6 7 8

x, cm

Figure 4. Spatial distribution of mean energy E(x) for neutrons of different origin in thedetector plane. Left axis - mean energy of neutrons collided in the sample, non-collidedneutrons and their sum for the FRM-1. Right axis - mean energy of neutrons collided in thesample for the ING-07.

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Neutron Imaging Methods to Detect Defects in Materials

02 ,0 0,,00

0~~~~~~

O 3 0------- - - …

5) ° ., C7 10 cm PE&Coll.O -] -- .l- D 10 cm PE. ____

i o

1 054 -.- 4t-

0 110 20 30 40 50 60

Scattering angle, degrees

Figure 5. Angular distribution of fast neutron beam behind a 10 cm thick PE sample and anassembly consisting of this sample and a honeycomb collimator.

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Nuclear Energy in Central Europe '99 S10200099Portoro2, Slovenia, 6 to 9 September, 1999

Application fields for neutron radiography and tomography in industryand technological development

E. H. Lehmann, P. VontobelPaul Scherrer Institut, CH-5232 Villigen PSI, Switzerland

B. SchillingerTechnical University Munich-Garching, Germany

ABSTRACT

Based on the present status of neutron radiography facilities and techniques in Europeancountries, some new options and developments in this field are described. Although someof the applied methods are very common in the different labs, new detectors and newdemands from industry might bring a "renaissance" in neutron radiography by its inherentpossibilities. It depends on the facilities' users effort to take this opportunity byimplementation of the right and adapted solution of the industrial problem.

1. Introduction

The inspection of material samples by neutrons is a technique successfully applied in differentbranches for many years. Most efficient is the study of moisture and corrosion in aircraftcomponents, the inspection of nuclear fuel and the observation of explosives concerning theiradequate functioning [1].As tool for non-destructive testing neutron radiography (NR) is in competition with otherestablished and improved methods such as X-ray, ultrasound and eddy current. Because highresolved images can only be obtained at strong neutron sources, the applications in NR aremostly immobile, i.e. have to be performed at the source site. For future developments in thefield of NR it will become very important to exploit the inherent methodical advantages ofneutrons: high penetrability through thick layers of metal (especially heavy metals such aslead and uranium) and the high sensitivity for detecting hydrogen. For some otherapplications, also the high absorption rates can be used efficiently (boron, gadolinium,cadmium, indium).On the other hand, new detection systems based on imaging plates, high efficient scintillatorsin connection with sensitive camera systems are improving the obtained information about theobserved objects in qualitative and quantitative direction [2]. Due to the wide dynamic rangeand the high linearity of such systems, hydrogen contents in the ppm range can be measured.The improvements in the field of computer technique made it possible to provide computedtomography with neutrons as standard tool at different facilities in Europe. Although theobtained spatial resolution will be in the order of 0.3 mm only, this method becomes animportant tool for reverse engineering (to make technical drawings from an existing object)and rapid prototyping of special objects in industry [3]. In the field of time resolvedmeasurements, advantages will also be obtained for weak neutron sources using highly

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Neutron Imaging Methods to Detect Defects in Materials

efficient intensifiers. With a flux level of 1(6 neutrons cm-2 s_ about 50 frames per second canbe measured in good quality [4].It is an important task for scientists and technicians active in NR to transmit the mentionedadvantages and improvements to the industry in the right and efficient way. This should bedone by publications in the specific journals, lectures for special industrial communities anddirect contacts to the development departments of companies. During the visits of branchexhibitions the demands of industry can easily be observed.This article describes some of the industrial related problems in more details and gives someinsight into the specific solutions.

2. The Situation in Europe

In 1998, a framework was founded for the small groups in Europe which are active in NR.Initiated by different specialists, the COST-524 programme represents now a formal basis forco-operation among the 10 participating countries (IT, FR, DE, AT, SI, CZ, UK, SP, CH, HU)under the "umbrella" of the European Commission [5]. Although not all countries are able tooperate their own neutron source and NR facility it is possible to be active in this field bymaking investigations and developments at other places utilising them as "user lab". On theother side, some NR (DK, SV, NO) stations with good performances have not yet joined theaction.The NR stations operated by the COST members have very different performance parameters.As an example, this situation is illustrated by a comparison of the collimation characteristics(UD) and the neutron flux level in Figures 1 and 2, respectively.

LD-values

500

400

300

200 --

100

01

fl . , , X ' _ ,

_ _ :. 6' ;' 6' 6" 6" i: iP i : f., .D

~~~~~~~~~~~~100 _ -a

Fig. 1: Comparison of the collimation ratio at different neutron radiography stations in Europe

Therefore, it becomes clear that limitations exist at different sites concerning the obtainablespatial (via low collimation) or time (via low flux level) resolution. Differently spoken, thespecial facility should be optimised for those applications for which the properties of thebeam will be advantageous.The second aspect for practical NR beside the beam performance is related to the detectorproperties. Some new developments as imaging plates [61 or camera based systems [7]provide the possibility of improved sensitivity (compared to traditionally used film), dynamic

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Neutron Imaging Methods to Detect Defects in Materials

neutron flux [cm 2 s 1]

1.E+09

1.E+08 0 -

1.E+05

1.E+04

1.E+03

I.E+02

? ? sf~~~~~OC oc.

Fig. 2: Neutron flux levels for thermal beams for different European radiography stations

range and digitised information. Due to the good reproducibility for obtaining images in a

reasonable time, it becames possible to make tomography with neutrons with good quality.

However, there is a strong demand to improve the application range of existing detector

systems, to understand all of their inherent properties and to look for other new options, as

semiconductor based detector arrays.

3. Application Range of Neutron Imaging

The majority of the NR facilities apply thermal neutrons for investigations, only a small

amount of systems is designed for cold [8] and fast neutrons [91. Therefore, the thermal

neutron cross-sections are valid for discussing the practical application fields for inspection of

objects. The balance between the contrast to distinguish between different material zones and

the penetrability of the samples are the two main aspects for the useful application of NR.

Compared to x-ray measurements, some important differences occur for hydrogen, other light

materials and strong neutron absorbers. Most of the metals can he penetrated well, especially

heavy elements such as lead, bismuth and uranium.

By~~~~~~~~~~i. 3: A gas target of a common airbag initiator was4 - t a - , ~~~~~~~investigated by neutrons (left) and X-rays (right).

. . - i -4 ~~~~~~~~Without intending to reveal the "producers secret- it> =- X a ~~~~~~~~can clearly be shown that the organic (hydrogen_;=, 5 ~~~~~~~~~~containing) material is not well visible by X-rays but

if: D ~~~~~~with neutron radiography.

[Sf] ~~~~~~~This example might be used as the starting point for0 . ~~~~~~~~~~~considerations where neutrons can be applied

_bL t: t 0 ~~~~~~~successfully or complementary to other methods.

Ir o C r Ne nyC r ' 757

FIg.er2:iNeutronfluxnc Nulevesfr thermal bnentamsfrdifrn Europe a raiorah staion

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Neutron Imaging Methods to Detect Defects in Materials

Beside the material choice (an example is given in Figure 3), some other boundary conditionsare given by the neutron properties. Because most of the NR stations are stationary, thesamples have to be investigated there, an in-situ inspection will not be possible with neutrons.Another aspect is the ability of neutrons to create long-living activation in material samples.Therefore, materials with high absorption cross-sections and half-lives longer than hours (e.g.Co, Hg, Ag, W) should be avoided to investigate. Due to the higher efficiency of new detectorsystems, a neutron fluence of about 108 cm-2 can be sufficient to obtain good images. Morethan ten times longer exposure was necessary in the past with the film method.In the industry, the number, the diversity and the complexity of new technical products isimproving and the reliability should remain constant or be improved. A good example are theairbag systems (see Figure 3), commonly used for motorcars for several years. The number,quality and performance is increasing now in order to protect drivers in accident conditions asgood as possible.A good direct dialog to industrial partners is required to understand the technical problem andto adapt the appropriate method for neutronic inspection.

4. Examples of NR Measurements at the NEUTRA Facility at PSI

A wide range of investigations was possible during the first period of operation (started in1998) of the new facility NEUTRA [10] at the spallation neutron source SINQ [11].

Fig. 4: The cooling equipment of a vacuum system consisting of copper block with penetrations for the coolingwater were inspected with neutrons. A nearly intact device is shown on the left side, but strongcorrosion was found in the part on the right side.

C-

Fig. 5: A honeycomb arrangement with aluminium as structural material was investigated at an angle of viewof about 450 to be able to see both adhesive connections of the outer layers. Only the organic glue isvisible in this image which has some non-horogeneity in the medium area.

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Neutron Imaging Methods to Detect Defects in Materials

As indicated by Figures 4 to 6, inspections of metallic sample made of copper, aluminium andsteel were done successfully and the accumulation of hydrogen, oxygen or carbon could bevisualised in its distribution. Reasons for possible failures in the past or future could be foundin this way.

Fig. 6: The jet of an oil burner wasassumed to be affected by theaccumulation of combustionproducts (coke). With neutroninspection, this material waslocalised on the inner surface ofthe equipment.

However, it was not only the. simple transmission image which could provide the answer tothe question of material damage. In some cases it was necessary to use the numericalinformation of the obtained images for a further improvement of the search for a deviatingsamples' behaviour. Because the data of our digital images have a dynamic range of 16 Bits(corresponding to more than 65000 grey levels), small differences can be distinguished muchbetter on the numerical level than by eye inspection using image post-processing tools. Suchan example is shown in Figure 7 for a high voltage isolator having a small defect on the innerpenetration which cannot be seen in the image but in the vertical profile.

_ ' indication for defects

|~~~~~~~~~ _ _ 1

e d o us l o o 2CC t O T CC C

Fig. 7: Inspection of an high voltage isolator utilising the help of the numeric information from the digitalimage

5. Detector Development for Neutron Imaging

The neutron sensitive detectors in use for NR have different properties in respect of spatialresolution and image acquirement time. Mostly efficient are camera systems which arecapturing the light emission of a neutron sensitive scintillator. Depending on the flux level ofthe beam several frames per second are possible with a reasonable quality. The limitation inspatial resolution of camera systems is given by the pixel size, the scintillator blurring and theinterference by "white spots" (saturised pixel by gamma events). An additional source ofunsharpness comes from the increased noise signal if an intensifier is installed for light

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Neutron imaging Methods to Detect Defects in Materials

amplification. Improved detector systems have to be developed by optimising all singlecomponents (scintillator, camera, intensifier, software and electronics).

1.OE-02

1 .OE-03 e tr-

0

01.OE-04

1.0E-05

1.OE-060.0001 0.001 0.01 0.1 1 10 100 1000 10000 100000

time resolution [a]

Fig. 8: The working area of different detectors applied at NEUTRA (PSI) shows what advantages anddrawbacks must be considered for an efficient choice of the most usable system for a given application.

Imaging plates become more and more a standard device as high resolution detector forneutron imaging due to its advantages compared to film. Their high sensitivity helps to reducethe exposure time significantly. However, they have also a relatively high sensitivity forgamma radiation. Therefore, the application of this method is limited at beam lines with highgamma background.Although there are some disadvantages in the use of etched track detectors (CN-85, CR-39)by the low achievable contrasts and the long exposure and etching time, this method is thebest option for the investigation of highly activated samples if the raw images on the foils canbe digitised in the right way t12y. Furthenmoye, some microscopic studies concerning thedistribution of boron in metallic surfaces can be done with these foils and grain sizes can belocalised [131.Two-dimensional arrays of amorphous silicon systems with pixel sizes of about 150 sum are inuse more and more for X-ray imaging. In principle, the step toward neutron imaging can bedone by changing and adapting the primary scintillation detector. Only the possible damage ofthe system at long term neutron exposure might be a limiting factor in the practicalapplication of such a device.

6. Status of Neutron Tomography (NT)

The 3D investigation of samples can be performed by the measurement of many transmissionimages (about 200 and more) where the object will be rotated around its vertical axis. Thethree dimensional material distribution (expressed by the local attenuation coefficient g(x,y,z)) can be obtained by different reconstruction algorithm.Detector systems based on CCD cameras are mainly in use for this type of measurements.Several countries in Europe are using this set up with satisfactory results (DE, CH, IT).The limiting factor for increasing the spatial resolution is the light emission characteristic ofthe neutron sensitive scintillator and the amount of data needed to be handled for thereconstruction and the visualisation. The last problem can be overcome by more powerfulcomputers. Adapted new scintillators emitting light spots smaller than 50 gim should beconsidered.

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Neutron Imaging Methods to Detect Defects in Materials

A nearly perfect detector for high resolution tomography might be the amorphous siliconarray because it unites the advantage of reproducibility and small pixel size in an idealmanner. However, no company is providing such a system on a commercial base up to now.

Fig. 9: The presented image is the view intothe innards of a hard disk driveobtained with neutrons after thereconstruction of 200 projections ofthis object. The voxel size is in theorder of about (0.5 mm)8. As theinherent resolution given by the beamproperties is much higher there is apotential for quality improvement forthis method.The work was done as a collaborationbetween PSI and TU Munich.

Some methodical problems in NT remain. Especially for thick samples, high absorbingmaterials or such with a high hydrogen content the simple assumption of exponentialattenuation of the neutrons in the beam fails more and more. This error will create visibleartefacts in the tomography images.A careful and iterative correction will be necessary to overcome this mistakes. This can bedone by Monte Carlo simulation of the neutron transmission process as done in [14]. Thisprocedure becomes more difficult if unknown materials or complicate material distributionsare within the samples.

7. Outlook to Future Activities

In the previous chapters it was intended to demonstrate by several examples that there aresome principle advantages for using neutrons in material studies and non-destructive testing.In addition to the more technical orientated investigations described here, medical orbiological studies can be performed under certain circumstances. Although such type ofsamples usually contain large amounts of hydrogen (which becomes a drawback for thickerlayers) some high quality images can obtained by dried animals, as shown in Figure 10.

Fig. 10: The neutron imagesof this Piranha(prepared bydrying) isdemonstrating thehigh resolution andthe good contrastobtainable at the

-. ~~NEUTRA stationof PSI.

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Neutron minaging Methods to Detect Defects in Materials

Higher contrasts and more dynamic range will be obtained by neutron radiography comparedto X-ray images for such biomedical objects. Several studies are in progress with dentalsamples where high spatial resolution is necessary, which can be provided with the traditionalfilm method in conjunction with a transmission light scanners.Competing and alternative investigations in comparison to other techniques can be provided ifa radiography facility with good beam performance and state of the art detectors will be used.

Acknowledgement

The authors want to express their thank to the operation team of SINQ for the submission ofgood neutronic conditions on a high performance level. We are pleased to thank G. Bauer andW. Fischer for the permanent interest and support in development and application of ourmethods.

References:

[11 1. C. Domanus (ed.), Practical neutron radiography, Kluwer Academic Publishers,Dordrecht, (1992)

[2] E. Lehmann et al., Application of new radiation detection techniques at the PaulScherrer Institut, especially at the spallation neutron source, Nucl. Instr. & Meth. A424 (1999) 158-164

[3] B. Schillinger et al., 3D neutron tomography: recent developments and first stepstowards reverse engineering, Nucl. Instr. & Meth. A 424 (1999) 58-65

[4] E. Lehmann, J. Meyer, Real-Time Neutron Radiography at NEUTRA - FirstAttempts, Outlook to practical Applications, Annual Report PSI, Annex, Volume VI,p.66

[51 General Secretariat of the European Union, Rules and Procedures for ImplementingCOST Actions, Brussels, July 1995

[6] K. Takahashi et al., Neutron sensitive Imaging Plates, Nucl. Instr. & Meth. A 377(1996) 119-122

[7] H. Pleinert, E. Lehmann, S. Kormer, Design of a new neutron radiaography detector,Nucl. Instr. & Meth. A 399 (1997) 382-390

[8] G. Bayon, Review on use of neutron radiography at Saclay Nuclear Research Centre,Proc. 5h World Conf. on Neutron Radiography, Berlin, 1996, p. 25

[9] K. Yoshi et al., Fast neutron radiography using a cooled CCD camera, Proc. 5th WorldConf. on Neutron Radiography, Berlin, 1996, p. 258

[10] E. Lehmann, P. Vontobel, The main performance parameters of the neutronradiography station NEUTRA at SINQ and its practical use for non-destructivematerial studies, Annual Report PSI, Annex, Volume VI, p.61, 1999

[11] G. S. Bauer, Operating Experience and Development Projects at SINQ, PSI-Report98-04, ISSN 1019-0643

[12] H.K. Jenssen, Neutron Radiography of Irradiated Fuel Rods - An Approach toImprove Spatial Resolution in Neutron Radiographs, Report IFE/F-98/159, Halden,Norway, 1998

[13] J.D.H Hughes, G.T. Rogers, High-Resolution Autoradiography of Trace Boron inMetals and Solids, Journal of the Institute of Metals, 1967, Vol. 95, p29 9

[14] H. Pleinert, E. Lehmann, S. Kbrner, Neutron signal transfer analysis, Nucl. Instr. &Meth.A 424 (1999) 177-182

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S102001 00Nuclear Energy in Central Europe '99Portorol, Slovenia, 6 to 9 September, 1999

X-ray Radiography Inspection of Core Model ofthe CODEX AIT-2 Facility

M. Balask6, Z. H6zer, L. Mar6ti P. Windberg

KFKI Atomic Energy Research Institute, H-1525 Budapest, P.O.B. 49. Hungary

ABSTRACT - X-ray radiography is an advanced non-destructive technique to visualize andanalyze the different damages of the investigated objects. An oxidation phenomena in severeaccident was simulated by the CODEX AIT-2 test facility. The placement, the extension andfeatures of the damages were discovered by radioscopy and film technique before cutting intoslices the AIT-2 boundle.

Keywords: X-ray radiography, radioscopy, film technique, oxidation phenomena, severeaccident simulation, damage discover

1. IntroductionX-ray radiography has proved to be highly useful in non-destructive testing inves-

tigations. It makes it possible to visualize the inner structure and the different damage of thecovered investigated object. Both radioscopy and film technique were able to show thedamages of the CODEX AIT-2 test facility after the air ingress experiments, before cuttingthe boundle into slices.

2. Experimental facilityThe X-ray radiography investigation was performed at Dynamic Radiography Station

(DRS)[1] of the BUDAPEST (10MW) research reactor. This working place is available tomake the neutron -, gamma - and X-ray radiography inspection, as it is seen in the Fig. 1. Thesource of the X-ray radiation is a portable industrial X-ray generator, its maximum power is300kV and 5mA. The dimension of the beam was optimized by an aperture of the source.Objects with a surface area of 700 x 1000 mm2 and weights of up 250kg can be investigatedand are manipulated into correct position of the beam by means of a remote controlmechanism The transmitted X-ray image of the object is converted into light by a ZnSscintillation converter screen and the "light image" is detected a low-light-level (LLL) TV-camera (104 lux for type TV1 122). The imaging cycle is 40 msec . The resolution of thedetected radioscopy picture is about 100Ogm. The radiography images are displayed on amonitor, stored by an S-VHS recorder and for further analysis, an image processing system isused (type Sapphire 5.05 by Quantel). A hard copy of the processed picture is provided by avideo printer. Higher resolution pictures are detected by X-ray films placed before thescintillator screen. The resolution of this method is 40pm. Naturally in this case the exposuretime is longer than the previous one, about several minutes.

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Neutron Iraging Methods to Detect Defects in Materials

\;s; . gl .-. ~~~~~~~~~Reactor -:

ClInside collimator ® Investigated object with

C~) Iron shutter system remote control mechanism'3 Beam diameter changer and filter unit maging st with

C4) Reactor shielding ~ ~~low light level TV camera4, Reatorshideoldingtor Working parameter indicators

56 Outidolgimato shedn Background TV camera6 Biologicalysh ieldn a e Beam stop

7 X-ray generator (ii)~~10 Control cabin

(f~j X-ray film position

Fig. 1.- Arrangement of the Dynamic Radiography Station at the Budapest research reactor

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Neutron Imaging Methods to Detect Defects in Materials

3. Investigated objectThe CODEX facility was built for the investigation of the behaviour of small fuel

bundles in severe accident conditions. The main component of the facility is the test sectionwhich can incorporate the fuel bundle to be investigated (Fig. 2). In the Air Ingress Test (AIT)tests 9-rod PWR type bundles were used[2,31. The rods are arranged on a square lattice, 8peripheral rod are electrically heated with tungsten bars. The central rod is not heated, it isused for instrumentation. Two spacer grids are applied to fix the bundle.The heated length ofthe bundle is 600mm. The cladding material is Zircaloy, the shroud part is made of a 2mmthick Zr2%Nb alloy. Inside of the fuel rods annular U0 2 pellets are placed between the heaterbars and the cladding. The depleted fuel has 0.2% enrichment. Around the shroud ZrO2thermal insulation is added. The test section is connected to the preheater and to the coolersections as coolant inlet and outlet respectively. Additional junction is connected to thebottom part of the bundle to inject cold air (room temperature). The preheater unit is able tosupply either hot gases or steam to the test section. The outlet temperature of the preheater canreach 800 'C. The off-gas streaming out of the test section is cooled down by thecooler/condenser unit and before releasing it into the atmosphere it is conducted through anaerosol trap and filtered by a special filter system. For the investigation of the aerosol releasea cascade impactor system is connected to the upper plenum of the cooler and two pipelinesallow the continuous measurement of aerosols by means of laser particle counters.

TES-T SECTION

e 1~c trocde

pyrometers-< I i =-L

0-P ~ ~ ~ ~ 0

ola

LI) 0~~~~~~~~~~~~~~~L

Fig. 2. CODEX AIT-2 facility

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Neutron Imaging Methods to Detect Defects in Materials

The test started with a preheating period using hot argon and electrical heating. The bundletemperature was stabilised at '-600TC.

The fuel rod cladding was oxidised in steam atmosphere in two steps: at 820TC and950TC to give an oxide layer thickness of 20-25 microns. Both steps lasted 30 minutes. Thetemperature stabilisation was reached with manual power control. Then the steam injectionwas stopped and the temperature decreased to -800TC. Due to a valve leak a small amount ofair flow joined the steam/Ar mixture during the preoxidation period.

The air ingress phase started with the injection of 2.5 g/s cold air and with a linearincrease of electrical power of 2 W/s to give an initial heating rate of 0.53K/s. Temperatureexcursion was observed on the fuel rods to a maximum indicated temperature of 1900 TC.Similar excursion took place on the shroud as well. The air injection was stopped when thetemperature in the central elevation reached 1700 'C, indicating the melting process.

isoo SH2 IU ___-~SHi

0 - 4 6OW 1000 120 14

Times

CODEX AIT-2 (Jan.22, 1999)

Fig. 3. Shroud temperatures at different elevations in the CODEX-AIT-2 test:SH4-450mm, SH3-300mm, SH2-150min, SH1-5Om_

The time variation the most important parameter during the test is shown in Fig.3. Theworking time is delineated by the horizontal coordinate in seconds, the temperature is writtenby the vertical coordinate in Celsius degree. Four curves were registred at four differentelevations of the CODEX AIT-2 test facility.

The SH4 was measured 45amm from the inlet of the heated lenght,SH3 was measured 30omm from the inlet of the heated lenght,SH2 was measured 150mm from the inlet of the heated lenght,SH1 was measured 50mm from the inlet of the heated lenght.

4. Experimental resultsAs the first step video imaging was used by the LLL TV -camera. In order to increase the

quality of the picture 800 images were integrated. For these measurements the parameters ofthe X-ray generator were 300kV and SniA. The damaged parts of the test facility weredistinguished by this method. In the second step - in order to obtain better resolution picturesfilm imaging technique was used with Structuri D7 Pb type X-ray films. In this case the X-raypower was 220kV and 2mA, the exposure time was 6 minutes.

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Neutron Imaging Methods to Detect Defects in Materials

The application of X-ray radiography provided a detailed vertical picture of the AIT-2 bundle.In Figs. 4-6 the structure and the distribution of materials can be seen. The upper spacer gridremained in its original position. Below the spacer grid severe fuel damage can be seen, thefuel rods were fragmented. Large part of the fuels fell down to the lower elevations. In thecentral part some pieces got stuck. The lower grid stopped most of the fragmented fuel andcladding pieces. Above the lower spacer grid a debris bed was formed, which included theintact lower fuel rods as well. The visual observation of the bundle showed strong oxidationand damage both of the shroud and fuel rods. Horizontal cross sections were prepared fromthe bundle for detailed analysis. The examination of cross sections confirmed that above 280mm elevation the degradation was strong. The fuel rods fragmented, the broken pellet andcladding pieces fell down. In the lower part of the bundle the debris accumulated and formedblockage on the spacer grid. Some small fragmented pieces could pass through the spacer gridand were collected in the lower chamber of the test section. At many places only the nakedW-rods indicate the original position of the rods. The photos of the whole cross sections areshown in Fig. 4 for elevations -20, in Fig. 5 for elevations 150, 280 and 375, moreover in Fig.6 for 450, 535 and 555 mm, together with the bundle X-ray radiography.

5. ConclusionThe X-ray radiography, both radioscopy and film technique, was useful method to study

the CODEX AIT-2 test facility after the air ingress experiments . It was able to discover theplacement, extension and the characteristic feature of the damage before cutting into slices ofthe bundle (test facility).

6. References[1] M. Balask6, E. SvAb "Dynamic neutron radiography instrumentation and application

in Central Europe" Nucl. Instr. Methods A 377, 140, 1996[21 CODEX-AIT-2 Test Data Report, Budapest, April 1999[3] CODEX-AIT-2, Post Test Examination, Part 1 :Investigation of the Aerosol Samples,

Budapest, May 1999

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hwtt<'osJY.ag~mg 34C.e•-f.-S2ASq r (>t !e•t Det-Xvvas w, *Af~r , i~ds

Veetical Vi .of \'-r'av

Radfography

;>Outlet

......................

in'et>

Pig. 4 ny raldiography of' iM CQDFMX AU 2 hundkl~l

.......... .. ............. .... ........ ............. ... ........ .. . r.... ... ... .. . y. • i'.c....?

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V:erticl Viekw m

fRadikgrapt

:~~ ~ ~~~ .~t~ [. d'J

: ; ;4 .. 0tt t00::00 00t ................

t~~~~~~~~~~~I~rn Sh Ablteit~~ntet> - 0 000t- 1 - 0 tti000000\00 000\'f- s s 4$ >-l. -4,x~

'ig X . . ....... .. ... .. .t l : ....X 2 .20:0000 X~u;00; Xe0'oi. at S, 0Ornrnt 2a8w~0tenun Xn 37mm 21vtio n

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Neutron Imaging Methods to Detect Defects in Materials

Vertical View 555mmof X-rayRadiograph3

535mm

450mm

Inlet >

Fig. 6. X-ray radiography of the CODEX-AIT-2 bundleand cross sections at 450mm, 535mm and 555mm elevations

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liii111111 ililh11llS102001 01

Nuclear Energy in Central Europe '99Portoro2, Slovenia, 6 to 9 September, 1999

PERFORMANCES OF SOME MOBILE NEUTRON RADIOGRAPHY SYSTEMS

P. BachSODERN, 20 avenue Descartes 94451 Limeil-Brdvannes

Abstract: Present paper describes shortly three different mobile neutron radiography systemsin term of characteristics, performances, flexibility, and their main applications for nondestructive testing of materials, devices and structures. Examples of application in differentfields, with particular attention to aeronautics (early corrosion detection, turbine blades qualitycontrol inspection) and pyrotechnic devices / specific parts inspection, are presented.

1. INTRODUCTION

Neutron radiography, invented in Germany in 1930 and further developed in UnitedKingdom, France and the United States in the sixties, is recognised as a powerful method, buta demanding method due to the practical problems associated with neutrons (safety andradioprotection). Beginning of seventies, mobile systems were proposed [1,2] where reactorneutron source is replaced either by small accelerators or by isotopic sources. The applicationof new technologies in aircraft airframes and devices, as well as the increase in aircraft servicelife, are examples of specific needs for "smart" mobile systems [3].

Mobile systems including Californiurn sources [4-7] have proven their suitability for nondestructive inspection in aeronautics and more generally in industry, including aerospace,automobile, plastic and explosives. Nevertheless, such systems are now less interesting, whileenvironmental laws as well as handling and storage rules related to isotopic sources becomemore severe. Modem mobile neutron radiography systems include now switchable, and evenpulsable, neutron sources such as small accelerators [8] and sealed tube neutron generators [9-15].

Main applications of such systems are related to an easy detection of hydrogen, oxygen andcarbon based materials when using thermal neutrons. Neutron radiography is useful for anumber of inspections, for instance:

- non destructive testing of thin films of glue in honeycomb or fiber glass epoxy structures,- inspection of composite materials, carbon fibers, and ceramics,- inspection of metallic or concrete block assemblies,- early detection of moisture or corrosion,- study of films and lubricants,- pyrotechnic devices inspection,

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Neutron Imaging Methods to Detect Defects in Materials

- turbine blades quality control inspection.

In this paper three mobile thermal neutron radiography systems, one using Cf-252 isotopicneutron source, one using a small size accelerator, and one using a sealed tube neutrongenerator, are shortly described.

2. SYSTEM BASED ON CF-252

Recent work on the use of neutron radiography has led to the design and operation of apractical inspection facility for aircraft maintenance [4] at Mc Clellan Air Force Base inCalifornia, U.S.A.

Beside a reactor based system, a robotic system was built for inspection of components ofaircrafts by neutron radiography. This manoeuvrable neutron radiography system includes aneutron head with Cf-252 assembly on the robotic arm.

Neutron source is a combination of 3 to 6 sources of 252 Cf, 10 mg to 15 mg each. Effectiveoutput is in the 10" n/s range, emitted at neutron energy of 2.2 MeV. Neutrons are thenthermalized by successive energy transfer in a hydrogen based material, up to a low levelabove thermal energy, say 0.1 eV. Common materials to thermalize neutrons are heavy water(the best), graphite, beryllium, oil, polyethylene, or water. In the present case, graphite andpolyethylene are a good compromise, taking into account physical and economical aspects.The neutron source is surrounded by the moderator. A filter is placed between the fast neutronsource and the beam exit port to help to remove gamma rays. An exit channel permit neutronsthat have scattered in that direction to emerge in a divergent beam. In order to have nearlyparallel neutron beam, a collimator is installed to remove neutrons in the wrong directions.Divergent collimator is used here, the thermal neutron beam divergence is characterised by theL / D ratio. In low flux mobile systems, L / D is low, between 10 and 50, corresponding to aquite large divergence and then to a limitation of the geometrical resolution of the system. Asa consequence, expected spatial resolution with such systems (as well as any other mobilesystem) is 100 - 200 jim;

The advantages of the Cf-252 based system are nearly no power consumption, a goodmobility in spite of the neutron head weight (- 500 kg), and an acceptable compromisebetween exposure time and resolution.

The disadvantages are: no switch off capability, safety problems, and change of highlyradioactive material each year (half life of 252 Cf = 2.6 years). Different kind of detectorswere used during years at this installation, showing very interesting results.

3. SYSTEM BASED ON ACCELERATOR

The second system is based on a RFQ small accelerator neutron source [16]. The entiresystem was designed for a high detection efficiency.

The accelerator, an Accsys Technology DL-1, is a compact radiofrequency quadrupole ionaccelerator which produces 0.9 MeV deuterons striking a beryllium target. Neutrons with an

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Neutron Imaging Methods to Detect Defects in Materials

energy spectrum up to 5 MeV and with an average energy of 1 MeV are produced through thereactions Be (d, n) B. These neutrons are then thermalized in a moderator-collimatorassembly. When the accelerator delivers 2.109 n/s into 4 xt, tlhell flux at the detector screen isestimated to be 2.104 n / cm2 s at low L/D ratio.

The image detection system is a CCD camera based unit, consisting of a LiF -ZnS scintillator,20 x 20 cm2. NE - 426 type, viewed through a front surfaced mirror at 45°. Camera includes acooled CCD matrix (-50 0C), 22.5 jlm pixel size (-160 pm in object space), with 1242 x 1152pixels. Neutron detection efficiency of this device is approx. 15 %.

Dominant limitation is the neutron statistical noise, and not the performance of the CCDsystem. Despite the low fluence, useful images may be obtained, showing for instance an

amount of corrosion at about 100 gm thick.

This system is more flexible than the first one (switch on/off capability), in spite of a higherweight and in spite of the requirement to deal with target refurbishment.

4. SYSTEM BASED ON NEUTRON GENERATOR

The third system is based on a sealed tube neutron generator. The DIANE l system is anexample of this technology [9-12], developed in the frame of a European Program (EUREKA,EU-22); The whole system was designed and manufactured by SODERN , in association withIABG in Germany, and L T V in the U.S.A.

The sealed tube neutron generator in a GENIE 46, delivering up to 4 x 1011 n/s at the energyof 14 MeV. The tube itself is a small sealed accelerator, without any external pump. A beamof deuterons and tritons (D +T),is accelerated at 225 kV toward a target loaded withdeuterium and tritium (D +T), and neutrons are emitted mainly from the fusion reactionT (d, n) He4. Neutrons are then thermalized in a moderator / collimator assembly. When thetube delivers 2 x 1l 1 n/s into 4 a, thermal flux is approx 105 n/cm2 .s for an effective L / Dratio of 25, or 2.8 x 104 n/cm 2 .s for an L / D ratio of 60.

The DIANE system is available with different imaging devices. Using a conventionalTRIMAX-2 converter (Gd 202s) in conjunction with a 3M -FM film, exposure time is approx.15 min at L / D = 25 [10]. Other film + converter devices are available; i.e. NE 426scintillator and D8 Agfa film for a shorter exposure time (3 min), or Gd metal and D7 film forbetter resolution at higher L / D but longer exposure time (I h). A conventional 30 x 40 cm2

Li/ZnS scintillating screen associated with a cooled CCD matrix camera is available. Inaddition, the camera for tomography designed and manufactured by Lebedev Institute [14]was successfully tested in the case of turbine blades.

Using a very similar design, W.E. Dance [3, 17] has made a neutron radiograph of aircrafthoneycomb panel indicating corrosion and moisture (see Fig 1), and another corroded partassociated with standard image quality indicators (see Fig.2). Radiographs from the existingDIANE systems were previously published [10, 12, 13].

' EUREKA project, supported by ANVAR - MRT - SERICS

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More generally speaking, the standard method for determining image quality was the ASTM-E545, using two main indicators (see Fig 3): a beam purity indicator (BPI) and a sensitivityindicator (SI). We have add a third specific indicator for pyrotechnic devices, in which gapsare to detect for resolution evaluation. Performances as obtained with the DIANE system are

- from BPI : thermal neutron content 70 %O,

scattered neutron content 1.2 %,gamma content < 0.2 %,pair production content < 0.2 %.

- from SI : gaps detected up to 13 gm,3 low contrast holes 0.5 mm diameter detected.

These performances are very close to performances as obtained on TRIGA reactor basedneutron radiography systems.

This system is very flexible, while running in a steady state or in a pulsed mode, and able tobe switched off. Tube replacement is made by the manufacturer.

5. CONCLUSION

On the basis of the results of this study, it is possible to consider mobile neutron radiographyas an available and effective non destructive testing method. Three kind of neutron sources areproposed, and a wide range of detection devices is available, for a good technical andeconomical optimization of the system.

REFERENCES

[1] J.P. Barton, ((Neutron radiography using non reactor sources))Isotopes and Radiation Technology 6, 2, (1969) 149-153

[2] C.B. Shaw, J.L. Cason, USAEC report BNWL -SA - 3090, Battelle MemorialInstitute - Pacific Northwest Laboratories, 1970

[3] W.E. Dance, S.F. Carrollo, Proc. 2id World Conf. On Neutron Radiography(WCNR-2), Paris, France (June 16-20, 1986) Reidel, Holland, 1987, p. 475-422

[4] K. Shields, W.J. Richards, ((Aircraft inspection using neutron radioscopictechniques»), SPIE vol 2455, 1995, p. 133-144.

[5] H.U. Mast, ((Neutron radiography in an aircraft maintenance environment)» Proc.5th. WCNR, June 17-20, 1996, Berlin, Gernany, p. 563 - 570.

[6] J.P. Barton et al., «(Feasability of neutron radiography for space shuttle inspection,<<WCNR-4, Gordon and Breach, 1993, p. 123-132.

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[7] K. Mochiki et al., (<252 Cf based neutron radiography using Musashi dynamic rangeprocessing system)), WCNR-5, Berlin 1996, p. 374-381.

[8] R.W. Hamm, «(Status of LANSAR neutron generators)», WCNR-5, Berlin 1996, p.540-547.

[9] W.E. Dance, S. Cluzeau, H.U. Mast <( Integration of an advanced sealed tubeneutron generator into a mobile neutron radiology system o NIM-B56, 1991, p 907-910.

[10] S.Cluzeau, P. Le Tourneur, W.E. Dance, <(DIANE neutron radiography deviceperformances: comparison with reactor beam)), NIM-B, 1995

[11] S.Cluzeau, P. Le Tourneur, «<Upgrade of the DIANE performance»>, WCNR-5,Berlin 1996, p. 512-518.

[12] P. Klein et al., ))Utilization of a cooled CCD camera»), WCNR-5, Berlin 1996. p.336-342.

[13] J.P. Dupuis et al., Industrial inspection of aeronautic samples: first step with theDIANE>>, WCNR-5, Berlin 1996, p. 657-664.

[14] V.1. Mikerov and al., ((Development of a mobile neutron defectoscope: currentstatus >>, WCNR-5, Berlin 1996, p. 456-462.

[15] V.T. Bobylev and al., «<Pulsed neutron generators (ING) of the VN1AA and systemson their base»), WCNR-5, Berlin 1996, p. 519-523.

[16] R.C. Lanza and al., (( An RFQ accelerator based neutron radiography andtomography system >>, WCNR-5, Berlin 1996, p.9 9-1 04 .

[17] W.E. Dance and al., <( Corrosion detection in aerospace structures using smallaccelerator neutron radiology, <( WCNR-4, May 1992, San Francisco (USA).

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Fig. [:Early detection of corrosion using thermal neutrons and Gadoliniumconverter/film cassette, on an F 15 structure part

Fig.3: Image quality indicatorsfrom left to right

* beam purity indicator,* sensitivity indicator

(achieved resolution fora given L/D),

* pyrotechnic deviceresolution indicator

Fi~ 2: Corroded parts, shown with image qualityindicators (LTV photo, ref. 6)

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Nuclear Energy in Central Europe '99 S10201 0Portoro2, Slovenia, 6 to 9 September, 1999

DETECTION OF 10B DISTRIBUTIONS IN HISTOLOGICAL SAMPLESBY NCAR USING THERMAL AND COLD NEUTRONS AND

PHOTOLUMINESCENT IMAGING PLATES: NEW RESULTSJ. Rant'* D. Gabel2, G. Bayon3 , H.Yanagie 4, H. Kobayashi 5 , E. Lehmann6 , G.Kuehne 6,

J.Skvar61 and R. Ilidl

J.Stefan Institute, 1000 Ljubljana, Slovenia2 Chemistry Dept., University of Bremen, POB 330 440, D-28334 Bremen, Germany

3CEA Saclay, F91191 Gif sur Yvette Cedex, France4 Institute of Medical Science, Univ. of Tokyo, 4-6-1 Shiroganedai, Tokyo 108, Japan

5Institute of Atomic Energy, Rikkyo University, 2-5-1 Nagasaka, Kanagawa, 240-01, Japan6 Paul Scherrer Institute, Villigen, Switzerland

The Neutron Capture Autoradiography (NCAR) using various Solid State Nuclear Track Detectors (SSNTDs)is a well established and accurate method to detect and measure the distributions of '0B in the ppm range onmacroscopic and microscopic level in biological samples, such as histological sections of tumours loaded with1°B compounds used for BNCT (e.g. 1,2). Recently a new technique of NCAR using sensitivephotoluminescent Imaging Plates (IP) has been proposed to detect 1°B distributions in histological sections(3), exploiting excellent detection properties of IP systems such as very high detection sensitivity andquantum detection efficiency, broad linear response and dynamic range, very small image distortion,reusability of IP and possibilities of digital autoradiography. The advantage of IP-NCAR vs. NCAR withSSNTDs should be the much lower neutron fluence ( 107-109 vs. 1010_1013 n/cm

2 with SSNTDs) , nointermediate chemical treatment (track etching ) and direct and fast computational handling and evaluation ofthe digitized autoradiographic image. However, the spatial resolution of the present available IP detectionsystems is somewhat lower (-0.04 mm) than with SSNTDs (-0.01 mm ). Another problem with IP NCAR israther high sensitivity of IP to all types of ionizing radiations. Therefore the background of direct and inducedgamma-rays as well as of epithermal and fast neutrons has to be filtered out of thermal neutron beam to beused for IP-NCAR. To improve the signal/background ratio and to increase the detectibility of '0B we proposeto use clean cold neutron or clean thermal neutron beams for the IP-NCAR of 10B distributions in histologicalsamples in BNCT experiments (4,5). In the present work the recent results of experiments in IP-NCAR withcold neutrons from the neutron radiographic channel of the ORPHEE reactor in Saclay and with the ratherclean thermal neutron beam of the NEUTRA neutron radiography facility of the PSI (Villigen) will bepresented. For the calibration of the NCAR histological samples of chicken liver with well knownconcentration of '0B were used and the limit of 10B detection in tissue samples down to at least 5 ppm hasbeen demonstrated.

1. Introduction

Neutron Capture Autoradiography (NCAR) using various Solid State Nuclear TrackDetectors (SSNTDs) is a well established and accurate method to detect and measure thedistributions of 10B in the ppm range on macroscopic and microscopic level in histologicalsections of tissues loaded with l B compounds used for BNCT [1,2]. The SSNTDtechniques require relatively high neutron fluences, chemical etching and somewhat timeconsuming quantitative evaluation. Two exposures are normally needed- one for Bdistribution visualization (102_10 3n/cm2) and second, 2-3 orders of magnitude lower, forquantitative boron determination by various track counting techniques. Recently a new

Retired from JSI

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technique of NCAR using sensitive photoluminescent storage phosphors (Imaging Plates orIP) has been proposed to detect heavy charged particles from the ' 0B(n, a )7Li reactions forthe topography of '°1 distributions in histological sections [3]. The new method exploitsexcellent detection properties of IP systems such as very high detection sensitivity andquantum detection efficiency, broad linear response and dynamic range, very small imagedistortion, reusability of IP and possibilities of digital autoradiography and immediatequantitative evaluation [4,5]. A severe problem for using IP in NCAR is their highsensitivity to all types of ionizing radiation and hence the background of direct and inducedgamma-rays as well as of epithermal and fast neutrons has to be suppressed or filtered outof the neutron beam. To improve the signal/background ratio and to increase thedetectability of ")B we proposed the use of rather gamma ray free cold neutron beams forthe IP-NCAR of '0B distributions in histological samples [6]. In the present work the firstresults of preliminary experiments in IP-NCAR with cold neutrons (IP-CNCAR) from theneutron radiographic channel of the ORPHEE reactor at Saclay are presented. In the firstbatch of experiments the cold neutron source was rather remote from the IP laser scanner(at 1JS, Ljubljana). The time lag between the IP neutron irradiation and the read outamounted several days greatly increasing the background due to cosmic and environmentalradiation and preventing the correct assessment of the detectability of the method. Thenumber of NCAR images produced in total was only 12, produced in 3 separate sets ofirradiations. However, the preliminary results were encouraging enough and enabled acomparison with the existing NCAR techniques. In the second batch of only 2 dayexperiments the IP scanning was performed in Saclay immediately after the irradiation,greatly reducing the gamma-ray background. New standards of freeze dried histologicalsamples of chicken liver with known B concentrations were prepared instead of previousstandards made of the filter paper. In the paper experiments are described and somecharacteristics of the IP-NCAR using cold neutrons for B detection are presented.

2. Methods and Materials

Neutron Capture AutoradiographyThe procedure for NCAR with IP is practically the same as used in NCAR with SSNTDs.The freeze-dried whole body histological sections of mice were put directly on theunprotected surface of the imaging plate, wrapped by light tight thin plastic cover and sealedafter evacuating air by vacuum pump. By this way an intense tight contact between the IPand the sample was achieved. The use of thin light tight plastic foil as irradiation cassette isessential for IP NCAR as the IP has to be protected from the light (in particular UV) and alltypes of ionizing radiation. The use of thin low Z -cassette" materials with a low neutronabsorption cross section is important to minimize the production of neutron and y-rayinduced secondary ionizing radiation. The wrapped IP/sample assemblies were air mailed toSaclay and after neutron irradiation immediately returned back for reading. The time lagbetween the preparation of the sample/IP assembly and read out was typically 6-8 days andthe time elapsed after the neutron irradiation was 4-6 days. Due to transport time the signalfaded for a factor 2-2.5 and the background due to cosmic and environmental radiationincreased for about factor 25! This drawback was removed by performing experiments andread-out of IP directly in Saclay during 2 days of experiments.

Cold Neutron SourceThe neutron irradiations were performed on the neutron radiographic facility at the coldneutron guide G4 of the research reactor ORPHEE (Saclay, France). The cold neutron flux is

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approximately 9.108 n/cm2 s and the average energy of the neutrons is 0.003 eV. The neutronbeam has a square profile 25 mm by 150 mm. The profile of the neutron beam is skewed forabout 7 % in both X- and Y- axis. The samples are irradiated by moving the irradiation rigalong the X-axis and the neutron fluence has to be corrected relevant to the irradiationposition along the vertical axis. Neutron fluences for IP based cold neutron captureautoradiography (IP-CNCAR) varied between 1.0 - 5.0 109 n/ cm2 . The y-ray background isconsidered to be negligible [7]

Imaging Plate Detection SystemThe imaging system used consists of FUJI Photo Film imaging plate type BAS IP-TR, FUJIBAS 1500 laser scanner at US ( FUJI BAS 1800 scanner at Saclay) and Raytest UV IPeraser. The digital images are handled, processed and analyzed by a personal computer andprinted by Epson Stylus Photo printer. The image handling, processing and analyzingsoftware is TINA 2.0 supplied by Raytest (Germany) and Photoshop ADOBE 3.0.The IP-TR type consists ofa plastic support plate (12.7 cm X 12.7 cm) covered with 0.05mm thick layer of crystals of photostimulable storage phosphor BaFBr:Eu2+ combined in aplastic binder. The phosphor layer is intended for the registration of 3H soft beta radiationand is hence unprotected and susceptible for surface damage and wetting. The thickness ofthe active layer of the phosphor is much thicker than the range of a and 7Li particles in thephosphor (few Sim).The BAS 1500 He-Ne laser (632.8 nm) scanner has a pixel size 0.1 mm X 0.1 mm, (0.05 X0.05 mm with BAS 1800) scanning speed 14 pts/pixel and 12 bit digitalization (4096 graylevels). Scanners with pixel size 25 Etm X 25 plm and digitalization of 16 or 32 bits arecommercially available. The inherent resolution of the system is lower than the pixel size,only about 0.2 mm (with advanced scanners 0.05 mm).

Standards and histological samplesThe standard samples with known concentration of 10B were prepared by pouring10 ptl drops of sodium borocaptate (BSH) solution in water on the filter paper ( B impuritybelow detection limit 3 ppm) forming stains of -I cm 2. The B content of the BSH solutionswas measured by plasma emission spectroscopy. The measured 10B concentrations (in ppm)were: 841±28, 248±8.7. 84.6±1.5, 25.2 ±0.32, 8±0.3. Boron concentration on the filterpaper wvere determined by digesting the paper samples in 65% HNO3 , diluting by purewater for factor 1 0 and measuring again by plasma emission spectroscopy. The measured' 0B concentrations were 483±15., 176±3.0, 73.5+6, 19.1+2.0 and 7.3±4. ppm. The Bdetection limit was at -4 ppm. It would be useful to measure B content in this indicator by aPGAA method nondestructively.New standards made of thin (0.025 mm) histological freeze dried chicken liver with known'0B concentration were supplied by one of us (D. Gabel). The concentration values were (inppm): 150. 100, 50, 25. 10, 5.0, 2.5, 1.75, 1.0, 0.5 and 0.1.Three different samples of whole body histological sections of a mouse were supplied bytwo of the co-authors:-Whole body section of the tumor bearing mouse sacrificed 31 after the intravenousinjection of 10BSH solution (1.5246%, PGAA result) and another section of a mousesacri'iced 6` after injection of 013 conjugated liposome/PEG liposome. In the formersample high B concentration was found in the liver and to smaller extent also in the tumourand kidney. In the later case the B was localized only in the tumour at low concentration, asconfirmed by subsequent NCAR with SSNTDs. The thickness of the samples was about

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0.04 mm and were freeze-dried mounted on 3M scotch tape. Details of the preparation ofthe samples can be found in the literature of the relevant group [3,8].- Whole body section of the mouse with B16 melanoma, sacrificed 1h after theintraperitoneal injection of 2 mg 10BSH. The thickness of the sample was 0.05 mm.

3. Results and Discussion

The IP-CNCAR images of new chicken liver 10 B standards are presented in Fig. la. Thesurface distribution of B in each liver standard is not uniform and an average signal fromthe whole surface area of the liver section has to be determined using tools of the TINAsoftware and correlated with the B content. The average signal of photostimulatedluminescence (PSL) above the average of the local background is proportional to the Bconcentration of the relevant standard. The calibration curve relating PSL signal abovebackground to B content is presented in Fig. lb.From Fig. I a it is evident that B content of at least about 5 ppm can be easily detected. The

detection limit is in this case possibly still below 5 ppm, since the relevant standards with Bconcentrations below 5 ppm can be observed and the signal can be discerned frombackground noise. This can be concluded also from Fig. lb, where the points with the Bconcentration of 0.1 to 5 ppm are showing significant scatter in the signal. However, thecalibration curve ( PSL signal vs. 10B conc.) does not cross axes at 0 indicating the presenceof some unresolved background. Increased nitrogen concentration in liver in comparisonwith the support layer would offer possible explanation. An experimental verification of theB concentration values by a reliable analytical and non-destructive method (e.g. PGAA orSSNTD NCAR) would be most helpful, while nitrogen content in the liver vs. support layercan be evaluated by the selective autoradiography with SSNTDs [10].In IP-(C)NCAR the background due to protons from neutron captures in nitrogen and heavyparticles and gamma rays from neutron absorption in hydrogen, oxygen and Li and Bimpurities in tissue is rather high and signal/background ratio is much worse than withNCAR using SSNTDs. The SSNTDs are sensitive only for heavy charged particles abovecertain threshold energies and offering the possibility of particle track discrimination byproperly selecting the etching conditions[l], etchant [8,9] and in addition by automaticimage analysis by measuring track dimensions, their shape and optical properties [2,10].However, for complete visual and quantitative image evaluation in SSNTD NCAR twoexposures are needed. Computerized track discrimination and counting requires fluencesmore than 2 orders of magnitude lower (-2. 109 nth/cm2 ) than required for visual imageobservation (_ 1(02 n12n/cm

2 ) in order to prevent track overlapping. With IP-(C)NCAR asdigital autoradiographic method quantitative evaluation and visual observation can beperformed simultaneously.In Fig. 2 the IP-CNCAR image of whole body section of a mouse prepared to put high Bconcentration in the body organs is presented. The distribution of B in the organs andtissues is clearly observed as well as differences in B content of different organs. In Fig. 2the high B concentration is in liver and at much smaller concentration in tumor, bladder andintestines. Using an appropriate calibration curve for B concentration monitoring preparedin the same way as actual samples and using similar tissue it could possible immediately todetermine the B content in selected regions. The spatial resolution is fair (0.2 mm with BAS1500) but with modern scanners (e.g. FUJI BAS 5000) it can be improved down to - 40pm, close to that of the whole body NCAR using SSNTD ( 10-20 pm ) [1,2].

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Neutron Imaging Methods to Detect Defects in Materials

4. Conclusions

The digital NCAR using clean cold neutron beams and IP as detectors has a potential todetect °B in histological sections of tissue at the level lower than 10 ppm and with thespatial resolution of - 40 1tm. Using calibration curves prepared by tissue standards withknown B content and in the same way as actual histological samples for BNCT studies themethod enables immediate and simple quantitative analysis. The advantage of IP-NCAR vs.NCAR with SSNTDs should be the much lower neutron fluence ( 10 -109 vs. 1010_1013n/cm2 with SSNTDs) , no intermediate chemical treatment (track etching ) and direct andfast computational handling and evaluation of the digitized autoradiographic image. Furtherexperiments in optimal experimental conditions are required to estimate accurately thedetection limit of this technique of B in tissues and to estimate the signal/background ratio.

5. References

1. Larsson,B., Gabel,D., BOrner,H.G., Phys.Med.Biol.,29(1984) 361-702. Woolard, J.E., Blue, T.E.. Curran, J.F., Dobelbower, M.C., Busby, H.R., Nucl. Sci.

Eng., 110 (1992) 96-1033. Yanagie, H. et al., Proc. 5.World Conf. on Neutron Radiography, June 17-20, 1996,

Berlin, DGZfP (1997) 750-574. Miyahara, J., Takahashi, K., Amemiya, Y., Kamiya, N., Satow, Y., Nucl. Instr. Meth. in

Phys.Res., A246(1986)572-5785. Sonoda, M., Tahano, M., Miyahara, J., Kato, H., Radiology, 148 (Sept. 1983)1486. Yanagie, H., lli, R., Skvard, J., Rant, J., US internal report, Dec. 19977. Bayon, G., CEA/CEN, Saclay, personal communication8. Yanagie, H., Ogura, K., Matsumoto, T., Eriguchi, M., Kobayashi, H., Proc. 3. Int.

Topical Mtg. on Neutron Radiography, March 16-19, 1998, Lucerne, Nucl. Inst. Meth.Phys. Res. A. 424 (1999) 122-125

9. Sornogyi, G., Hunyadi, 1.. Proc. 10th Int. Conf. "Solid State Nuclear Track Detectors",Lyon, France, 2-6 July 1979, (Eds., H. Frangois et al.), Pergamon Press (1979) 443-52

10. Skvarc, J., lli, R., Yanagie, H., Rant, J., Ogura, K., Kobayashi, H., Selectiveradiography with etched track detectors, Nucl. Instr. Meth. Phy. Res. B "Beam Inter.Mater. Atoms", 152 (1999) 115-121

1 1. JEFPC 2.0 Cross-Section Data Base, NEA Data Bank, OECD, 1997

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S10200103Nuclear Energy in Central Europe '99Portoro2, Slovenia, 6 to 9 September, 1999

Neutron radiography at the"Institut de Maintenance Aeronautique"

Serge Cluzeau, Institut de Maintenance Aeironautique, Merignac, France

AbstractRecently the French Instilut de Maintenance Aeronautique (IMA) decided to open a new field of researchspecially devoted to the inspection methods that should be used by the aircraft overhauling industry. Taking intoaccount its proved ability for an early corrosion detection, neutron radiography (NR) was selected as aninspection method to be appraised. This paper presents the approach that IMA intends to follow for achievingthis objective and involving selection of equipment, design of the facility and research program.

1 Introduction of the "Institut de Maintenance Aeronautique".The French "Institut de Maintenance Aironautique" (IMA), is a Physics Branch

Department of the Bordeaux-1 University. It is located in Meirignac, a city in the district ofBordeaux, quite near to the International Mirignac Airport. Its activities are developed inaeronautic field through four different ways.a-First, IMA is a training center for turning out executives of the aircraft overhaulingindustry. It leads its students to the title of engineer at the master degree level. The trainingcourse meets the level C of the new JAR' 66 regulationb-Secondly, IMA is a center for designing and producing new educative tools. For instanceRMA supplied the Airbus Training Center with interactive computer based teaching aids.c-Thirdly, IMA fulfills research and development studies for the benefit of small and middlecompanies, thanks to its laboratories specialized in engines, mechanics, hydraulics, and so on.d-Last but not least, JMA is also a center for technology transfers from University to industry.An international society called Specialized Training in Aeronautics and Research (STAR),was created so as to make easy the cooperation between University and private companies.STAR is an Enterprise-University Training Partnership (EUTP) in the field of space andaeronautics. It is the only EUTP supported by the European Union (Comett Program) in thisfield of activity. It includes more than 200 industrial and university members located in 18countries. STAR, as well as the French STAR society have their headquarters at IMA. Bythe way of STAR and with the help of its partners, IMA has implemented several projectsleading every time to an additional expertise.At the present time, three new projects are to be started subject to get the necessary budget:1- The use of modern teaching tools for pilot training (multimedia, simulator,..)2- Practice of LASER in aeronautics and space industry.3- Practice of neutron radiography in aeronautic and space industry.

' The "Joint Aviation Requirements" ( JARs) are the new European standards for airlines taking effect from2.000/2.001. The JAR 66 is related to the training of engineers.

International Conference Xucl,, le a Incrgi il Central Europe '99 785

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Neutron Imaging Methods to Detect Defects in Materials

2- Neutron radiography at IMA.As said before, IMA is an institute mainly devoted to the training of aircraft

overhauling agents. These people are educated in many technological fields but usually theyhave a poor knowledge in Nuclear Physics. Then, when IMA decided to fit out a NonDestructive Testing Laboratory (NDT Lab.) with a neutron radiography (NR) ability, theproject manager in charge of this action looked for an equipment easy to use andcharacterized by the less possible safety nuclear constraints. With such a requirement, a smallmachine based on the use of a sealed-tube neutron generator (STNG) was a good choice. Thisneutron source is indeed very similar to an industrial X-ray generator quite usual in NDTimplementation. Both these equipment are on-off sources emitting ionizing radiation and needa specific shielding moreover they are built with the same architecture and operate with thesame ergonomy as well. Then, IMA got in touch with the SODERN French company whichcould supply it with a STNG or even with a small NR system (DIANE system). Recently acooperation agreement has been reached, by which this company will place its own STNGprototype, type GENIE 46, [ 1], (see Figure 2a), and its imaging systems [2] at the disposal ofthe future NDT Laboratory. For its part, IMA will build a facility, (see Figure 1 and 2c), andmanufacture a DIANE equipment with an upgraded design [3], (see Figure 2b). At the presenttime, this project is supported by the University of Bordeaux-1 and submitted to the FrenchDepartment of Education and Science for an official recognition. At the same time the firststeps was taken to get the necessary budget with a good hope to succeed.

3- Applied research program at IMA.Subject to get its NDT facility, IMA intends to undertake applied research that meets

unsatisfied requirements of aircraft overhauling activity in cooperation with maintenanceindustry. Whatever study is begun, the corresponding research program will be lead incooperation with a company acknowledged as a major in the approached field. Thispartnership will make sure that the problem to be solved is actual and the expected solution isacceptable by industry. At the same time the cooperation will be extended to any appropriatelaboratory if a specific expertise is needed, what is expected in many cases. A first list ofsubjects supposed to be of interest for industrial companies has been drawn in two classesinvolving either the "NDT implementation" or the "Improvement of the inspection tools".

3-1 NDT implementation.Three subjects are expected to be initiated in this class.a-Detection of hidden corrosion in aeronautic structures: In some already known cases,corrosion attacks cannot be effectively detected with the usual NDT methods (X-ray,ultrasonic, eddy current). It is the case for instance for the intergranular corrosion or forcorrosion which lies between two thick overlapping metallic plates. Many times such acorrosion hits aging aircraft due to material fatigue under mechanical strains. This worryingphenomenon caused several aeronautic disasters in the last fifteen years and remains difficultto detect at the present time even thought it was very soon proved that NR could help to solvethis problem [4]. After the above mentioned crashes, the FAA lead a tremendous program inUSA called the "National Aging Aircraft Research Program Plan" (NAARPP) and, in aformer step, the study of NR capabilities was considered, but later, this field of research waswithdrawn, probably due to the lack of industrial equipment but to the lobbying of "greenparty" as well.In this field IMA will aim to identify which parts are better inspected with NR than with usualalternative methods, the wanted result being a reduced inspection cost due to an earlierdetection or a faster testing. This subject includes several intermediate issues such as: choiceof the best implements, setting up of the testing process, design of standards, methodacceptance test by the authority, and so on....

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Neutron Imaging Methods to Detect Defects in Materials

b-Inspection of aluminum honeycomb structures: In this case it is very well known that NRand X-ray inspections complement each other strikingly. Then, the same kind of research asabove should be fruitful, peculiarly for moisture and corrosion detection which are hardlyseen with usual NDT methods.c- Inspection of parts made of composite materials: More and more aircraft parts are madeof composite materials even though they are difficult to be inspected and that rather fewinformation is available about the aging effects. Taking into account this fact, it should seemreasonable to explore the potentiality of the NR inspection in this field.

3-2 Improvement of the inspection tools.Taking into account the design of its NR equipment, IMA will favor the research concerningthe systems using a sealed-tube neutron generator but the resulting issues should be of interestfor all of the low output systems. It is worth pointing out that from a social point of view, tomaintain a very low output is the best way for making it possible and safe the in-plant use of aneutron source. So, from a technical point of view, researches aiming an image improvementare vital for putting up an acceptable performance in the widest possible application field. Inthis field the study is expected to bear on the thermal neutron source, the imaging systems,and the image processing taking into account the "optical transfer function " of each part ofthe equipment. Another very interesting study would be to set up some "diagnosis aids" suchas computed virtual inspections of sample, or fusion of inspection results from all of theperformed methods. In every cases the goal should be a better detection defect, a moreaccurate measurement or an inspection with a reduced exposure time, but in any way, theactual industrial goal remains a reduced expenses as explained above.

4- Conclusion.To conclude this paper, it is worth pointing out that the implementation of a so wide

research program needs a good knowledge in many specific scientific and technologic fields.That is why IMA intends to be open to any offer of cooperation concerning such a program.From now on for instance, IMA intends to be a partner of the 524-COST Action if agreed bythe Management Committee and the French Authority.

References.[11 Thermal neutron source using a sealed neutron tube/ S.Cluzeau, J.Huet, P.Le Tourneur,J.L Ma,,! Proceedings of the 4 World Conference on Neutron Radiography, San Francisco,Ca, USA, May 10-16, 1992.[21 Utilization of cooled CCD cameras for static neutron radiography and computedtomography/ P.Klein, P. Le Tourneur. B.Poumarede, P. Turon-Lacarrieu, G.Bayon/Proceedings of the 5th World Conference on Neutron Radiography, Berlin, Germany, June17-20, 1996.[3] Upgrade of the DIANE performance/ S.Cluzeau, P. Le Tourneur!! Proceedings of the 5thWorld Conference on Neutron Radiography, Berlin, Germany, June 17-20, 1996.[4] Proceedings of the 2nd World Conference on Neutron Radiography, Paris, France, June16-20, 1986/ Cold neutron radiography of mechanical connectors: P.A. Attwood, P. Swift/Experience with an on-off mobile neutron radiography system: J.J Antal, W.E. Dance, J.D.Moravec, S.F. Carollo/ The sensitivity of neutron radiography for detection of aluminumcorrosion products: J. Rant, R. Ilic, CG. Pregl, P. Leskovar, B. Znidar/Neutron Radiography ofaluminum alloy corrosion damage: A. Ridal, N.E.Ryan/ Corrosion detection by real-timeneutron imaging: H. Berger, R. Polichar, W.J. Rowe/ Economics of neutron radiography forcomercial aviation: D. A. Froom, J.P. Barton.

International Conference Nuclear Energy in Central l'urupc '9 'I7

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Neutron Imaging Methods to Detect Defects in Materials

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inspection room depending on the need

788 International Conference Nuclear Energy in Central Europe '99

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Neutron Imaging Methods to Detect Defects in Materials

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Figure 2: Sketch map of the plant room and its fitting out

International Conference ,N'uclear Energ, in Central Europe '99

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001 `SI0200002008AS99/01/I/AMIK009AA100AUpson, P. (European Nuclear Society)2001Assuring nuclear energy's future through international co-operation2101nternational Conference Nuclear Energy in Central Europe 99, V. 1. Proceedings211 APortoroz (SI))213^6-9 Sep 1999500^p. 3-7600A(EN)009AM100AGortnar, 0.; Stritar, A. (eds)(Nuclear Society of Slovenia)109AEuropean Nuclear Society; Ministry of Science and Technology of Slovenia, Ljubljana (SI); Ministry of

Economic Affairs of Slovenia, Ljubljana (SI), Inst. Jozef Stefan, Ljubljana (SI); Slovenian NuclearSafety Administration, Ljubljana (S1); Agency for Radwaste Management, Ljubljana (SI); ENCONETConsulting GmbH, Vienna (AT); SlAP d.o.o, Pesnica pri Mariboru (SI); S-NET Internet Provider,Ljubljana (SI)

1 0Nuclear Society of Slovenia, Ljubljana (SI)200`1nternational Conference Nuclear Energy in Central Europe 99, V. 1. Proceedings300AINIS-SI--02-002320AISBN 961-6207-13-X401ALjubljana (SI)4021Nuclear Society of Slovenia (SI)403^ 1999500A683 p.611 AAvailable from Nuclear Society of Slovenia, Jozef Stefan Institute, Jamova 39, Ljubljana (SI)009A9

800APUBLIC INFORMATION; PUBLIC OPINION; EDUCATION; INTERNATIONAL COOPERATION;ENERGY POLICY; EUROPE

009AX/EN860Alt is invited lecture as the introduction to the sixt international meeting entitled Nuclear Energy in

Central Europe. Good commercial operation, public information and education are needed to win theconfidence of the public, and to attract young people to take over the industry's founding generation.Stimulating international co-operation and transfer of best practices can assure this happens across thewhole of the Europian nuclear industry.

001 AS10200003008AS21/01/1/AM/K009AA100^Holubec, J. (Mochovee NPP (SK))2001Mochovce NPP unit 1&2 completion project210"1nternational Conference Nuclear Energy in Central Europe 99, V. 1. Proceedings211 ^Portoroz (S1)213^6-9 Sep 1999500^p. 9-16600^(EN)610^5 tabs., 4 figs.009AM100^Gortnar, 0.; Stritar, A. (eds)(Nuclear Society of Slovenia)109^European Nuclear Society; Ministry of Science and Technology of Slovenia, Ljubljana (Sl); Ministry of

Economic Affairs of Slovenia, Ljubljana (SI); Inst. Jozef Stefan, Ljubljana (SI); Slovenian NuclearSafety Administration, Ljubljana (SI); Agency for Radwaste Management, Ljubljana (SI); ENCONETConsulting GmbH, Vienna (AT); SIAP d.o.o, Pesnica pri Mariboru (SI); S-NET Internet Provider,Ljubljana (SI)

110^Nuclear Society of Slovenia, Ljubljana (SI)

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2 0 0A1nternational Conference Nuclear Energy in Central Europe 99, V. 1. Proceedings300^ INIS-SI--02-002320^ISBN 961-6207-13-X401 'Ljubljana (SI)4021Nuclear Society of Slovenia (SI)403^ 1999500^683 p.611 'Available from Nuclear Society of Slovenia, Jozef Stefan Institute, Jamova 39, Ljubljana (SI)009A9800AMOCHOVCE-1 REACTOR; SLOVAKIA; MOCHOVCE-2 REACTOR; REACTOR SAFETY; WWER

TYPE REACTORS; WWER-4 REACTOR; REACTOR LICENSING; REACTOR COMMISSIONING009AX/EN860AHistory of Mochovce NPP is quite long and reflects political changes that happened in Europe in the end

of 80'ties. The plant site was chosen in south-west of Slovakia in the frame of Nuclear IndustryDevelopment Plan adopted by former Czechoslovak government in 70'ties. In that time was decided tobuild in Mochovce four VVER 440/213 units together with other NPP's (Dukovany, Temelin, Kecerovee).

001 S10200004008'S62/01/I/AM/K009`A100ABrenizer, J.S. (Dept. of Mechanical and Nuclear Engineering, The Pennsylvania State Univ. (US))2001Current and future neutron radiography standards210A1nternational Conference Nuclear Energy in Central Europe 99, V. 1. Proceedings211 1Portoroz (SI)213^6-9 Sep 1999500^p. 17-24600"(EN)610^21 refs.009^M100'Gortnar, 0.; Stritar, A. (eds)(Nuclear Society of Slovenia)109"European Nuclear Society; Ministry of Science and Technology of Slovenia, Ljubljana (SI); Ministry of

Economic Affairs of Slovenia, Ljubljana (SI); Inst. Jozef Stefan, Ljubljana (SI); Slovenian NuclearSafety Administration, Ljubljana (S1); Agency for Radwaste Management, Ljubljana (SI); ENCONETConsulting GmbH, Vienna (AT); SIAP d.o.o, Pesnica pri Mariboru (SI); S-NET Internet Provider,Ljubljana (SI)

1 10^Nuclear Society of Slovenia, Ljubljana (SI)200^1nternational Conference Nuclear Energy in Central Europe 99, V. 1. Proceedings300^ INIS-SI--02-002320^ISBN 961-6207-13-X401 ^Ljubljana (SI)402^Nuclear Society of Slovenia (SI)403" 1999500^683 p.611 'Available from Nuclear Society of Slovenia, Jozef Stefan Institute, Jamova 39, Ljubljana (SI)009^9800^STANDARDS; SAFETY STANDARDS; NEUTRON RADIOGRAPHY; ISO009^X/EN860^Only two organizations are actively producing standards which are used in neutron radiology (NR): the

American Society of Testing and Materials (ASTM) and the International Organization forStandardization (ISO). Six ASTM standards exist that address the neutron radiography method. Two ofthe ASTM standards have been extensively used world-wide. ISO has a working group which isdeveloping three standards that also address the neutron radiography method. Two of these arecurrently making their way through the ISO approval system. No ASTM or ISO standards exist for theneutron radioscopic method. Future ASTM standards will address the neutron radioscopic method andneutron radiologic system characterization. It is expected that similar efforts will be undertaken in lSO.

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Given the relatively small community providing neutron radiologic services, international cooperationand the need for ISO standards will most likely continue to grow.(author)

001 AS10200005008AS99/01 l/AM/K009AA100AGregoric, M. (Slovenian Nuclear Safety Administration, Ljubijana (SI))200AHarmonisation of Slovenian nuclear legislation with EU210^lnternational Conference Nuclear Energy in Central Europe 99, V. 1. Proceedings211 ̂ Portoroz (SI)213^6-9 Sep 19995001p. 25-32600A(EN)009AM1001Gortnar, 0.; Stritar, A. (eds)(Nuclear Society of Slovenia)109AEuropean Nuclear Society; Ministry of Science and Technology of Slovenia, Ljubljana (SI); Ministry of

Economic Affairs of Slovenia, Ljubljana (SI); Inst. Jozef Stefan, Ljubljana (SI); Slovenian NuclearSafety Administration, Ljubljana (SI); Agency for Radwaste Management, Ljubljana (SI); ENCONETConsulting GmbH, Vienna (AT); SIAP d.o.o, Pesnica pri Mariboru (SI); S-NET Internet Provider,Ljubljana (SI)

1 101Nuclear Society of Slovenia, Ljubljana (S1)2 0 0 1International Conference Nuclear Energy in Central Europe 99, V. 1. Proceedings300 ̂ INIS-SI--02-002320AISBN 961-6207-13-X401Ljubljana (SI)4021Nuclear Society of Slovenia (SI)403 A 1999500^683 p.611 'Available from Nuclear Society of Slovenia, Jozef Stefan Institute, Jamova 39, Ljubljana (SI)009A9

8001SLOVENIA; LEGISLATION; EUROPEAN UNION; ATOMIC ENERGY LAWS; CONTAMINATIONREGULATIONS

009A X/EN860Slovenia as a member of the first group of candidates countries which started the accession negotiations

with the European Union. The extensive work started in 1998 to align the domestic legislation with thelegislation of the European Union. The activities related to the accession of Slovenia to EU in the area ofnuclear legislation are carried out in different national working groups. The main part of activities is inworking groups: energy and environment, but there are some topics, which are covered in other groups,like control of dual-use materials in the group of External Relations, research in reactor physics, nuclearengineering and fusion in the group Science and Technology.

001 AS10200006008AS21 /01/1/AM/K009^A100IRozman, S. (NPP Krsko (SI))200'Krsko modernization project210A1nternational Conference Nuclear Energy in Central Europe 99, V. 1. Proceedings211 APortoroz (SI)213^6-9 Sep 19995001p. 33-46600A(EN)610A1 ill., I tab., I fig.009AM

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100AGortnar, 0.; Stritar, A. (eds)(Nuclear Society of Slovenia)109AEuropean Nuclear Society; Ministry of Science and Technology of Slovenia, Ljubljana (SI); Ministry of

Economic Affairs of Slovenia, Ljubljana (SI); Inst. Jozef Stefan, Ljubljana (SI); Slovenian NuclearSafety Administration, Ljubljana (SI); Agency for Radwaste Management, Ljubljana (S1); ENCONETConsulting GmbH, Vienna (AT); SIAP d.o.o, Pesnica pri Mariboru (SI); S-NET Internet Provider,Ljubljana (SI)

110Nuclear Society of Slovenia, Ljubljana (SI)200A1nternational Conference Nuclear Energy in Central Europe 99, V. 1. Proceedings300AINIS-SIl-02-002320^ISBN 961-6207-13-X401 ALjubljana (SI)4021Nuclear Society of Slovenia (SI)403A 1999500^683 p.611 'Available from Nuclear Society of Slovenia, Jozef Stefan Institute, Jamova 39, Ljubljana (SI)009A9

800AKRSKO REACTOR; SLOVENIA; POWER GENERATION; STEAM GENERATORS; REACTORSIMULATORS; REACTOR LICENSING; LICENSING; FINANCIAL DATA

009AX/EN860APresented are the activities for NPP Krsko modernization project which covers Steam Generators

replacement ant power increase for 6 %.

001 AS10200007008AS22/01/1/AM/K009`A1001Neufert, A.; Van de Velde, A. (Siemens AG Unternehmensbereich KWU, Erlangen (DE))200AThe integrated code system CASCADE-3D for advanced core design and safety analysis210Alnternational Conference Nuclear Energy in Central Europe 99, V. 1. Proceedings211 1Portoroz (SI)213^6-9 Sep 1999500^p. 49-56600^(EN)610^6 refs., 3 tabs., I fig.009AM100^Gortnar, 0.; Stritar, A. (eds)(Nuclear Society of Slovenia)109^European Nuclear Society; Ministry of Science and Technology of Slovenia, Ljubljana (SI); Ministry of

Economic Affairs of Slovenia, Ljubljana (SI); Inst. Jozef Stefan, Ljubljana (SI); Slovenian NuclearSafety Administration, Ljubljana (SI); Agency for Radwaste Management, Ljubljana (SI); ENCONETConsulting GmbH, Vienna (AT); SIAP d.o.o, Pesnica pri Mariboru (SI); S-NET Internet Provider,Ljubljana (SI)

110^ Nuclear Society of Slovenia, Ljubljana (SI)

2 0 0 ^1nternational Conference Nuclear Energy in Central Europe 99, V. 1. Proceedings300AINIS-SI--02-002320^ISBN 961-6207-13-X401^Ljubljana (SI)402^Nuclear Society of Slovenia (SI)403 ̂ 1999500^683 p.611 AAvailable from Nuclear Society of Slovenia, Jozef Stefan Institute, Jamova 39, Ljubljana (SI)009A9800^C CODES; COMPUTER CODES; FUEL MANAGEMENT; REACTOR ACCIDENTS; REACTOR

CORES; COMPUTER-AIDED DESIGN; SAFETY ANALYSIS009^X/EN860AThe new program system CASCADE-3D (Core Analysis & Safety Codes for Advanced Design

Evaluation) links some of Siemens advanced code packages for in-core fuel management and accident

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analysis: SAV95, PANBOX/COBRA and RELAP5. Consequently by using CASCADE-3D the potentialof modern fuel assemblies and in-core fuel management strategies can be much better utilized becausesafety margins which had been reduced due to conservative methods are now predicted more accurately.By this innovative code system the customers can now take full advantage of the recent progress in fuelassembly design and in-core fuel management.(author)

001 SI0200008008`"S22/01/1/AM/K009A A100"Trkov, A.; Aldama, D.L. (Inst. Jozef Stefan, Ljubljana (SI))2001Definition of pseudo fission product data for reactor calculations210"International Conference Nuclear Energy in Central Europe 99, V. I. Proceedings211 1Portoroz (S1)213"6-9 Sep 1999500"p. 57-62600"(EN)61015 refs., 2 tabs., 2 figs.009"M100AGortnar, 0.; Stritar, A. (eds)(Nuclear Society of Slovenia)1091European Nuclear Society; Ministry of Science and Technology of Slovenia, Ljubljana (SI); Ministry of

Economic Affairs of Slovenia, Ljubljana (S1); Inst. Jozef Stefan, Ljubljana (SI); Slovenian NuclearSafety Administration, Ljubljana (SI); Agency for Radwaste Management, Ljubljana (SI); ENCONETConsulting GmbH, Vienna (AT); SIAP d.o.o, Pesnica pri Mariboru (SI); S-NET Internet Provider,Ljubljana (SI)

110"Nuclear Society of Slovenia, Ljubljana (SE)200" nternational Conference Nuclear Energy in Central Europe 99, V. 1. Proceedings300AINIS-SI--02-002320AISBN 961-6207-13-X401"Ljubljana (SI)402"Nuclear Society of Slovenia (Sl)403A 1999500"683 p.611 'Available from Nuclear Society of Slovenia, Jozef Stefan Institute, Jamova 39, Ljubljana (SI)009^9800AFISSION PRODUCTS; PLUTONIUM RECYCLE; BENCHMARKS; FISSION; PLUTONIUM 242;

REACTOR CORES; N CODES; A CODES009AX/EN860"ln the WIMS-D library the important fission products are treated explicitly. The remaining ones are

lumped into a single pseudo fission product. The methods and the criteria for defining the pseudo fissionproduct data are described. The data based on ENDF/B-V1 and JEF-2.2 evaluated nuclear data files areprocessed and the WIMS-D library is updated accordingly. Some preliminary results of the NEA/OECDPlutonium Recycling Benchmark are presented.(author)

001 AS 10200009008AS21/01/1/AM/K009AA100"Bace, M.; Pevec, D.; Trontl, K. (Dept. of Applied Physics, Faculty of Electrical Engineering and

Computing, Univ. of Zagreb (HR))200"Radiation dose rates in the vicinity of the NPP Krsko spent fuel pool2101International Conference Nuclear Energy in Central Europe 99, V. I. Proceedings211 "Portoroz (SI)213"6-9 Sep 1999500"p. 63-68600"(EN)

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610^6 refs., 4 tabs., 3 figs.009AM100"Gortnar, 0.; Stritar, A. (eds)(Nuclear Society of Slovenia)109"European Nuclear Society; Ministry of Science and Technology of Slovenia, Ljubljana (SI); Ministry of

Economic Affairs of Slovenia, Ljubljana (SI); Inst. Jozef Stefan, Ljubljana (SI); Slovenian NuclearSafety Administration, Ljubljana (SI); Agency for Radwaste Management, Ljubljana (SI); ENCONETConsulting GmbH, Vienna (AT); SIAP d.o.o, Pesnica pri Mariboru (SI); S-NET Internet Provider,Ljubljana (SI)

1 10"Nuclear Society of Slovenia, Ljubljana (SI)2001 International Conference Nuclear Energy in Central Europe 99, V. 1. Proceedings300^INIS-SI--02-002320AISBN 961-6207-13-X401 ^ Ljubljana (SI)4021Nuclear Society of Slovenia (SI)403^1999500^683 p.611 `Available from Nuclear Society of Slovenia, Jozef Stefan Institute, Jamova 39, Ljubljana (SI)009^9800ASPENT FUEL ELEMENTS; SPENT FUEL STORAGE; SPENT FUELS; KRSKO REACTOR; FUEL

STORAGE POOLS; S CODES; DOSE RATES; NEUTRONS009AX/EN860A0ur recent analysis showed that from the criticality standpoint of view it is possible to increase capacity

of the NPP Krsko spent fuel pool by reracking to accommodate spent fuel assemblies for plant lifetime.The reracking will also effect the radiation dose rates in the vicinity of the NPP Krsko spent fuel pool. Inthis paper we have investigated the radiological impact of reracking using SAS sequences of the SCALEcode system. Gamma and neutron dose rates are calculated at different positions close to the spent fuelpool surface for current and reracked spent fuel pool configuration. A comparison of the calculated doserates and the dose limit in 10 CFR 20 for the restricted work area has been performed.(author)

001 "S10200010008AS21/01/I/AM/K009"A100AKromar, M. (Inst. Jozef Stefan, Ljubljana (SI))200"Power feedback effects in the LEM code210"1nternational Conference Nuclear Energy in Central Europe 99, V. 1. Proceedings211 "Portoroz (SI)213^6-9 Sep 1999500Ap. 69-73600^(EN)610^7 refs., 2 tabs., 2 figs.009^M100^Gortnar, 0.; Stritar, A. (eds)(Nuclear Society of Slovenia)109^European Nuclear Society; Ministry of Science and Technology of Slovenia, Ljubljana (SI); Ministry of

Economic Affairs of Slovenia, Ljubljana (Sl); Inst. Jozef Stefan, Ljubljana (SI); Slovenian NuclearSafety Administration, Ljubljana (SI); Agency for Radwaste Management, Ljubljana (SI); ENCONETConsulting GnmbH, Vienna (AT); SIAP d.o.o, Pesnica pri Mariboru (SI); S-NET Internet Provider,Ljubljana (Sl)

11 0^Nuclear Society of Slovenia, Ljubljana (SI)200^1nternational Conference Nuclear Energy in Central Europe 99, V. 1. Proceedings300^INIS-SI--02-002320^ISBN 961-6207-13-X401 ^Ljubljana (SI)402^Nuclear Society of Slovenia (SI)403^1999500^683 p.

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611 'Available from Nuclear Society of Slovenia, Jozef Stefan Institute, Jamova 39, Ljubljana (SI)009A9

800AKRSKO REACTOR; L CODES; REACTOR CORES; REACTOR CORE DISRUPTION; PWR TYPEREACTORS; COMPUTER CALCULATIONS

009A X/EN8601The nodal diffusion code LEM has been extended with the power feedback option. Thermohydraulic and

neutronic coupling is covered with the Reactivity Coefficient Method. Presented are results of the codetesting. Verification is done on the typical non-uprated NPP Krsko reload cycles. Results show that thecode fulfill objectives arising in the process of reactor core analysis.(author)

001 AS10200011008AS22/01/1/AMNK009AA

100lBace, M.; Jecmenica, R. (Dept. of Applied Physics, Faculty of Electrical Engineering and Computing,Univ. of Zagreb (HR)); Smuc, T. (Inst. Rudjer Boskovic, Zagreb (HR))

200'Validation of SCALE code package on high performance neutron shields21OAInternational Conference Nuclear Energy in Central Europe 99, V. 1. Proceedings211 APortoroz (SI)213A6-9 Sep 1999500'p. 75-81600A(EN)610^4 refs., 2 tabs., 5 figs.009AM100AGortnar, 0.; Stritar, A. (eds)(Nuclear Society of Slovenia)109AEuropean Nuclear Society; Ministry of Science and Technology of Slovenia, Ljubljana (SI); Ministry of

Economic Affairs of Slovenia, Ljubljana (SI); Inst. Jozef Stefan, Ljubljana (SI); Slovenian NuclearSafety Administration, Ljubljana (SI); Agency for Radwaste Management, Ljubljana (SI); ENCONETConsulting GmbH, Vienna (AT); SIAP d.o.o, Pesnica pri Mariboru (SI); S-NET Internet Provider,Ljubljana (SI)

1 10^Nuclear Society of Slovenia, Ljubljana (SI)2 0 0 1International Conference Nuclear Energy in Central Europe 99, V. 1. Proceedings300AINIS-SI--02-002320AISBN 961-6207-13-X401 ALjubljana (SI)402`Nuclear Society of Slovenia (SI)403A 1999500^683 p.611 AAvailable from Nuclear Society of Slovenia, Jozef Stefan Institute, Jamova 39, Ljubljana (SI)009A9800AS CODES; NEUTRON SOURCE FACILITIES; SHIELDING MATERIALS; SHIELDING;

COMPUTER CALCULATIONS; ONE-DIMENSIONAL CALCULATIONS; NEUTRON EMISSION009AX/EN860The shielding ability and other properties of new high performance neutron shielding materials from the

KRAFTON series have been recently published. A comparison of the published experimental and MCNPresults for the two materials of the KRAFTON series, with our own calculations has been done. Twocontrol modules of the SCALE-4.4 code system have been used, one of them based on one dimensionalradiation transport analysis (SASI) and other based on the three dimensional Monte Carlo method(SAS3). The comparison of the calculated neutron dose equivalent rates shows a good agreementbetween experimental and calculated results for the KRAFTON-N2 material.. Our results indicate thatthe N2-M-N2 sandwich type is approximately 10% inferior as neutron shield to the KRAFTON-N2material. All values of neutron dose equivalent obtained by SASI are approximately 25% lower incomparison with the SAS3 results, which indicates proportions of discrepancies introduced by one-dimensional geometry approximation.(author)