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1+1 Nalionallibrary 01 Canada Bibliothèque nationale du Canada Acquisitions and Direclion des acquisilions el Bibliographie selVices Branch dèS selVices bibliographiques 395 Wellinglon Street 395. Ne Wellington Ottawa,Onlar)() Ottawa (Onlano) K1AON4 K1AON4 NOTICE AVIS The quality of this micrcfcrm is heavily dependent upon the quality of the original thesis submitted for microfilming. Every effort has been made to ensure the highest quality of reproduction possible. If pages are missing, contact the university which granted the degree. Some pages may have indistinct print especially if the original pages were typed with a poor typewriter ribbon or if the university sent us an inferior photocopy. Reproduction in full or in part of this microform is governed by the Canadian Copyright Act, R.S.C. 1970, c. C-30, and subsequent amendments. Canada La qualité de cette microforme dépend grandement de la qualité de la thèse soumise au microfilmage. Nous avons tout fait pour assurer une qualité supérieure de reproduction. S'il manque des pages, veuillez communiquer avec l'université qui a conféré le grade. La qualité d'impression de certaines pages peut laisser à. désirer, surtout si les pages originales ont été dactylographiées à l'aide d'un ruban usé ou si j'université nous a fait parvenir une photocopie de qualité inférieure. La reproduction, même partielle, de cette mlcroforme est soumise à la Loi canadienne sur le droit d'auteur, SRC 1970, c. C-30, et ses amendements subséquents.

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1+1 Nalionallibrary01 Canada

Bibliothèque nationaledu Canada

Acquisitions and Direclion des acquisilions elBibliographie selVices Branch dèS selVices bibliographiques

395 Wellinglon Street 395. Ne WellingtonOttawa,Onlar)() Ottawa (Onlano)K1AON4 K1AON4

NOTICE AVIS

The quality of this micrcfcrm isheavily dependent upon thequality of the original thesissubmitted for microfilming.Every effort has been made toensure the highest quality ofreproduction possible.

If pages are missing, contact theuniversity which granted thedegree.

Some pages may have indistinctprint especially if the originalpages were typed with a poortypewriter ribbon or if theuniversity sent us an inferiorphotocopy.

Reproduction in full or in part ofthis microform is governed bythe Canadian Copyright Act,R.S.C. 1970, c. C-30, andsubsequent amendments.

Canada

La qualité de cette microformedépend grandement de la qualitéde la thèse soumise aumicrofilmage. Nous avons toutfait pour assurer une qualitésupérieure de reproduction.

S'il manque des pages, veuillezcommuniquer avec l'universitéqui a conféré le grade.

La qualité d'impression decertaines pages peut laisser à .désirer, surtout si les pagesoriginales ont étédactylographiées à l'aide d'unruban usé ou si j'université nousa fait parvenir une photocopie dequalité inférieure.

La reproduction, même partielle,de cette mlcroforme est soumiseà la Loi canadienne sur le droitd'auteur, SRC 1970, c. C-30, etses amendements subséquents.

Thermal Analysis of Aluminum Foundry Alloys

by a Novel Beat Pipe Probe

by

Mahmood MERATIAN ISFAHANI

A Thesis Submitted to the Faculty of Graduate Studies and

Res~arch in Partial Fulfilment of the Requirements

fGr the Degree of Doctor of Philosophy

Department of Mining and Metallurgical Engineering

McGill University

Montreal, Canada

Jan., 1995

C M. Meratian, 1995

1+1 National Ubraryo'Canada

Bibliothèque nationaledu Canada

Acquisitions and Direction des acquisitions etBiblIOgraphie services Branch des servicas bibliographiques

39S Wellinglon St,eet 395. rue WelhngtonOttawa. Ontario Ottawa (Onlario)K1A 0N4 K1A ON4

THE AUTHOR HAS GRANTED ANIRREVOCABLE NON-EXCLUSIVELICENCE ALLOWING THE NATIONALLffiRARY OF CANADA TOREPRODUCE, LOAN, DISTRmUTE ORSELL COPIES OF mSIHER THESIS BYANY MEANS AND IN ANY FORM ORFORMAT, MAKING TffiS THESISAVAILABLE TO INTERESTEDPERSONS.

THE AUTHOR RETAINS OWNERSHIPOF THE COPYRIGHT IN mSIHERTHESIS. NEITHER THE THESIS NORSUBSTANTIAL EXTRACTS FROM ITMAY BE PRINTED OR OTHERWISEREPRODUCED WITHOUT mSIHERPERMISSION.

ISBN 0-612-05756-9

Canad~

L'AUTEUR A ACCORDE UNE LICENCEIRREVOCABLE ET NON EXCLUSIVEPERMETTANT A LA BffiLIOTHEQlT5NATIONALE DU CANADA DEREPRODUIRE, PRETER, DISTRIBUEROU VENDRE DES COPIES DE SATHESE DE QUELQUE MANIERE ETSOUS QUELQUE FORME QUE CE SOITPOUR METTRE DES EXEMPLAIRES DECETTE THESE A LA DISPOSITION DESPERSONNE INTERESSEES.

L'AUTEUR CONSERVE LA PROPRIETEDU DROIT D'AUTEUR QUI PROTEGESA THESE. NI LA THESE NI DESEXTRAITS SUBSTANTIELS DE CELLE­CI NE DOIVENT ETRE IMPRIMES OUAUTREMENT REPRODUITS SANS SONAUTORISATION.

-_......--------...,-_.~ ........~-... ..... '....~.~, ..• "'.~ ........._......__......_-_.._--

ABSTRACT

A new application of heat pipes is introduced. The pre3ent research deals

with the development of a heat pipe for the on-line quality control of liquid

aluminum silicon foundry alloys.

Thermal analysis is a technique whereby a small quantity of a melt is

allowed to solidify while its cooling curve is recorded. Analysis of the cooling

curve with standard mathematical algorithms allows one to determine a number of

useful parameters that characterize the liquid and solid states of the material. In

aluminum-silicon casting alloys thermal analysis is often used to assess the grain

size and degree of eutectic modification of the alloy before pouring.

A novel probe has been developed for conducting thermal analysis of

aluminum alloy melts. The probe, which resides in the melt, need not be

withdrawn as it solidifies a small sample (i.e. button) at a predetermined cooling

rate. Once the cooling curve results have been acquired, the probe can be

instructed to remelt the frozen button and await instrJctions for analyzing a fresh

sample.

The operating principle of Ibis novel device is based on heat pipe

technology. In simple terms, a heat pipe consists of a condenser and an evaporator

which contain a relatively small quantity of working substance fluid. As heat is

absorbed by the evaporator, the liquid phase of the working substance is vaporized

and subsequently condensed on the condenser walls from which heat is extracted.

Il has been shawn that the designed probe, which is classified as agas

loaded annular thermosyphon, is completely workable in the range of conditions

• ABSTRACT ii

typically encountered in the thermal analysis of aluminum alloys. Tht: thermal

analysis results obtained with this new technique are in a good agreement with

those of conventional thermal analysis. In addition, the new method is applicable

to a wider range of operating conàitions and i~ easier to use. Based on the semi­

continuous nature of the new method, it does not need pre-preparation (materials,

labour, pre-heating, thermocouple installation for each test, isolation of the

sampling cup, etc.) to start thermal analysis. Also, from a cooling rate point of

view, the system is weIl controllable. Moreover, it is shown that the probe is

simple in construction, easy to use, and intelligent enough to provide semi­

continu.Jus thermal analysis. There are no consumable mat.,rials and mcving parts.

Thermal analysis results are reported for pure aluminum, hypoeutectic

aluminum silicon (356) and eutectic aluminum silicon (413) casting alloys.

Agreement in the results between the new and conventional systems is shown to

be excellent. Finally, a heat transferlsolidification model of the heat pipe thermal

analysis probe is derived and validated.

RÉsUMÉ

Une nouvelle application des caloducs est introduite. Les travaux de

recherche présentés dans cet ouvrage concernent le développement d'un caloduc

pour le contrôle de qualité sur le site des alliages de fonderie Al-Si à l'état liquide.

L'analyse thermique est une technique qui permet d'enregistrer la courbe

de refroidissement d'un petit échantillon pris dans la coulée. Le traitement de cette

courbe avec des algorithmes standards permet de déterminer plusieurs paramètres

utiles qui caractérisent les états liquide et solide du matériau. Dans les alliages de

fonderie Al-Si, l'analyse thermique est souvent utilisée pour estimer la taille des

grains et le degré de modification de l'alliage avant la coulée.

Une nouvelle sonde a été développée pour faire des analyses thermiques des

coulées d'alliages d'aluminium. Placée dans la coulée, la sonde n'a pas à être

retirée lorsqu'elle solidifie un petit échantillon (par exemple un pion) à une vitesse

de refroidissement prédéterminée. Une fois que les résultats de la courbe de

refroidissement sont obtenus, on peut commander à la sonde de fondre à nouveau

le pion solidifié et d'attendre les instructions pour analyser un nouvel échantillon.

Le principe d'opération de cet équipement innovateur est basé sur la

technologie du caloduc. En termes simples, un caloduc se compose d'un

condenseur et d'un évaporateur qui contiennent une quantité relativement petite

d'un fluide comme substance de travail. Lorsque la chaleur est absorbée par

l'évaporateur, la phase liquide de la substance de trl1~lail est vaporisée et condensée

par la suite sur les parois du condenseur à partir desquelles la chaleur est extraite.

TI a été montré que la sonde conçue, qui est classée comme un

thermosyphon annulaire contenant un gaz, est entièrement utilisable dans le

domaine des conditions typiquement rencontrées dans les analyses thermiques des

alliages d'aluminium. Les résultats des analyses thermiques obtenus par cette

nouvelle technique sont en accord avec ceux obtenus par la technique

conventionnelle d'analyses thermiques. De plus, cette nouvelle méthode s'applique

dans un domaine plus large de conditions d'opérations et est plus facile à utiliser.

Etant donnée la nature semi-continue de cette nouvelle méthode, aucune

préparation est nécessaire (matériaux, main-d'oeuvre, pré-chauffage, installation

d'un thermocouple pour chaque essai, isolation du creuset d'échantillonnage, etc

...) pour commencer l'analyse thermique. Aussi, en ce qui concerne la vitesse de

refroidissement, le système se contrôle très bien. En outre, il a été montré que la

sonde est simple à construire, facile à utiliser, et assez intelligente pour produire

des analyses thermiques semi-continues. il n'y a aucun matériau qui se consumme,

ni aucune pièce en mouvement.

Les résultats des analyses thermiques pour l'aluminium pur, les alliages de

fonderie Al-Si hypoeutectique (356) et eutectique (413) sont présentés. La

concordance entre les résultats obtenus par les deux techniques, conventionnelle

et de type caloduc, se trouve être excellente. Finalement, un modèle de transfert

de chaleur/solidification de la sonde d'analyse thermique de type caloduc en a été

tiré et a été validé.

RÉSUMÉ iv

ACKNOWLEDGEMENTS

This reptJrt would not be complete without an acknowledgement of those

indivirluals who helped me a10ng dUr.dg the course of my work. ln particular, 1

would like to thank the following:

~1y wife, Dr. B. Hami, for her love, continuous emotional support,

understanding, and encouragement during those periods when my work

required much of my time and attention. Without her sacrifices, this work

could not have been accomplished.

My supervisors, Professors John E. Gruzleski and Frank Mucciardi

for their unending patience, constant encouragement and enthusiasm. Their

guidance and keen interest on the topic supplied both engaging and

iIIuminating diversions from the occasionally frustrating task of scientific

research.

One and ail of my compatriots to whom 1 owe this opportunity to

study abroad. In particular, the personal financial support of the Iranian

Ministry of Culture and Higher Education through a Post-Graduate

Scholarship is gratefully acknowledged.

1 would also like to acknowledge the technical personnel of the depnrtment

particularly Mr. Robert Paquette, Mr. Martin Knoepfel and O;Jr computer

Iaboratory manager Mr. François Dallaire.

During my stay here at McGiII 1 enjoyed a friendly multinational

environrnent. Special thanks to Peter Botos, Jon Kay, and Ms. Gail Stephen from

Canada, Wittaya LaOrchan from Thailand, Ning Jin from China, Musbah Mahfoud

and Hussein Aboulwefa from Libya, Anantha Lakhshmanan, Pranansu. S.

Mohanty alld, Ramany Sankaranarayanan from India, Ms. Guler Yamanoglu and

Hasim Mulazimoglu from Turkey, Masashi Ikezawa from Japan, Ms. Tatiyana

Luganova from Ghazaghistan and Ms. Florence Paray from France. 1 especially

wish to thank Florence for the Frencl: translation of the abstract. 1 also gratefully

acknowledge the support and encouragement from my lranian friends

1 gratefully acknowledge the Natural Sciences and Engineering Research

Council of Canada (NSERC) for materials and equipment support, and thr- Fonds

Concertés d' Action pour la Recherche (FCAR), and the McGiII Metals Processing

Centre (MMPC) for partial financial support of this project.

Many thanks go to David Sparkman of Foundry Information Systems, Inc.,

John T. Carter of General Motors Research Laboratories of Canada, and Ichizo

Tsukuda of Showa A1uminum Corporation of lapan for showing interest in this

work.

• ACKNOWLEDGEMENTS vi

Finally, but most importantly, 1 would Iike to express my deep gratitude to

my family in Iran for their love and moral support. My pursuit of higher education

is a product of their encouragement. Thousands of kilometres OOtween us never

existed in our hearts. As modest a work as this may 00, fust and foremost this

work is dedicated to them.

•TABLE OF CONTENTS

ABSTRACT

RÉSUMÉ

ACKNOWLEDGEMENTS

TABLE OF CONTENTS

LIST OF FIGURES

LIST OF TABLES

LIST OF SYMBOLS

Hi

v

vii

xii

xviii

xx

CHAPrERONE

INTRODUCTION 1

1.1 Scope of the Present Study . . . . . . . . . . . . . . . . . . . . . . ., 1

1.2 Overview of the Present Work 4

CHAPrERTWO

2.1 Introduction .•HEAT PIPE . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6

6

2.2 History 7

2.3 Operating Principles 8

2.4 Heat Pipe Types 9

2.4.1 Thermosyphon Il

2.4.2 Gas-Loaded Thermosyphon . . . . . . . . . . . . . .. 12

2.5 Heat Pipe Theory , 16

2.5.1 Thermodynamics 17

2.5.2 Fluid Flow , 18

2.5.3 Heat Transfer . . . . . . . . . . . . . . . . . . . . . .. 20

2.6 Design Considerations , 30

2.6.1 Working Substance . . . . . . . . . . . . . . . . . . .. 30

2.6.2 The Container . . . . . . . . . . . . . . . . . . . . . .. 33

2.7 Heat Pipe Applications. . . . . . . . . . . . . . . . . . . . . .. 35

• TABLE OF CONTENTS viii

CHAPfER TIlREE

METALLURGICAL ASPECTS 44

3.1 Introduction 44

3.2 Grain Refinement , 45

3.2.1 Grain Refinement Principles 46

3.2.2 Chemical Grain Refinement of Al Alloys 49

3.2.3 Thermal Behaviour During Heterogeneous

Nucleation 52

3.3 Modification . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 53

3.3.1 The Fundamentals of Modification 54

3.3.2 Chemical Modification of Aluminum Alloys 56

3.4 Thermal Analysis . . . . . . . . . . . . . . . . . . . . . . . . .. 59

3.4.1 Thermal Analysis Control of Grain Size . . . . . .. 62

3.4.2 Thermal Analysis Control of Eutectic

Modification . . . . . . . . . . . . . . . . . . . . . . .. 64

3.4.3 Thermal Analysis Equipment . . . . . . . . . . . . .. 67

• TABLE OF CONTENTS IX

CHAPTER FOUR

THE HEAT PIPE PROBE 70

4.1 Introduction 70

4.2 Characteristics of the Probe 70

4.3 Probe Design 72

4.3.2 Materials Selection , 73

4.3.2.1 Working substance selection ., . . . . . .. 73

4.3.2.2 Inert gas selection 77

4.3.2.3 Container material selection 78

CHAPfER FIVE

EXPERIMENTAL 80

5.1 Introduction 80

5.2 Experimental Set-up 80

5.2.1 Probe Elements " 80

5.2.2 Sensors . . . . . . . . . . . . . . . . . . . . . . . . . .. 83

5.2.3 Peripheral Equipment 84

5.3 Experimental Procedure . . . . . . . . . . . . . . . . . . ., " 87

5.3.1 Cooling (Solidification) 88

5.3.2 Heating (Remelting) 88

TABLE Of CONTENTS X

CIlAPTER SIX

MODELLING HEAT TRANSFER . . . .. 90

6.1 Introduction 90

6.2 Heat Transfer Model of the Heat Pipe Probe . . . . . . . .. 91

6.2.1 Model Construction 91

6.2.1.1 Nodes . . . . . . . . . . . . . . . . . . . . . .. 91

6.2.1.2 Heat pipe types ... . . . . . . . . . . . . .. 94

6.2.1.3 Variables and equations . . . . . . . . . . .. 94

6.2.2 Input 95

6.2.3 Output 97

6.2.4 Evaluation of Model Results 97

6.3 Heat Transfer Model of Soîidification 102

6.3.1 Model Construction 102

6.3.2 Initial and Boundary Conditions " 104

6.3.3 Numerical Solution Techniques 105

6.3.4 Solution Procedure . . . . . . . . . . . . . . . . . .. 107

6.3.5 Examples . . . . . . . . . . . . . . . . . . . . . . . .. 108

CIlAPTER SEVEN

RESULTS AND DISCUSSION 119

7.1 Introduction 119

7.2 Typical Results 121

7.2 Parametric Results 135

7.2.1 Grain Refinement . . . . . . . . . . . . . . . . . . .. 136

7.2.2 Modification . . . . . . . . • . . . . . . . . . . . . .. 143

• TABLE OF CONTENTS

CHAPTER EIGIIT

xi

8.1 Concluding Remarks .

8.2 Claims to Originality .

8.3 Future Studies .

CONCLlTSIONS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 150

150

152

153

BmLlOGRAPHY

LIST OF FIGURES

CHAPTER TwO

Figure 2.1 Components and principle of operation of a conventional heat

pipe 8

Figure 2.2 A two-phase closed thennosyphon . . . . . . . . . . . . . . . . . .. 10

Figure 2.3 Concentric annular thennosyphon . . . . . . . . . . . . . . . . . .. 12

Figure 2.4 Schematic diagram and temperature distribution of a gas loaded

heat pipe 13

Figure 2.5 Schematic of a gas-loaded thermosyphon in three different

cooling rate modes 15

Figure 2.6 Comparison of actual and idealized flow in a thennosyphon ., 19

Figure 2.7 Pool boiling regimes 21

Figure 2.8 Film condensation on a vertical surface . . . . . . . . . . . . . . . 23

Figure ~.9 Sodium charged heat pipe dryout . . . . . . . . . . . . . . . . . .. 27

Figure 2.10 Comparison of sonic limits in Na, K, and.Cs heat pipes 29

Figure 2.11 Operating temperature ranges of various heat pipe fluids 31

Figure 2.U Liquid transfer factor at boiling point versus boiling point . .. 32

Figure 2.13 A lypical heat pipe used for deicing 36

Figure 2.14 The use of heat pipe to reduce die wall temperature

gradients 37

Figure 2.15 Two configurations of heat pipe and chill . . . . . . . . . . . .. 39

Figure 2.16 Cooling of electrodes with water cooling and heat pipe

cooling ,.................. 40

Figure 2.17 Measurement of steel temperature with a heat pipe-sheathed

thermocouple . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41

Figure 2.18 Thermosyphon injection lance vs. normal injection lance . . . . 42

• LIST OF FIGURES xiii

CHAPTES THREE

Figure 3.1 Aluminum rich part of aluminum-silicon phase diagram ..... 45

Figure 3.2 Surface energy relations affecting the wetting of heterogeneous

nuc1ei by the liquid metal . . . . . . . . . . . . . . . . . 47

Figu.\'l! 3.3 The interfacial energy interaction between nuc1eant and

nucleus 48

Figure 3.4 Aluminum rich part of the aluminum- titanium phase

diagram' " 50

Figure 3.5 Nucleation by the peritectic reaction in the AI-Ti system 51

Figure 3.6 Schematic representation of the growth of silicon 55

Figure 3.7 Microstructural rating system for modification of Al-Si alloys . 58

Figure 3.8 A typica1 cooling curve of an off-eutectic Al-Si alloy ..... " 61

Figure 3.9 Typica1 cooling curve and ils first derivative of a 356 alloy at

approximately 0.8°C/s " 62

Figure 3.10 The cooling curve at the beginning of solidification 63

Figure 3.11 A comparison of the eutectic regions of the cooling curves of

modified and unmodified alloys 65

Figure 3.12 Relationship between eutectic structure and eutectic

temperature, apparent eutectic supercooling and period of

supercooling .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 66

Figure 3.13 Two typica1 sampling cups used for thermal analysis 68

CRAPTER FOUR

Figure 4.1 The basic appearance of the thermosyphon probe . . . . . . . .. 71

Figure 4.2 The cross section of the evaporator elements . . . . . . . . . . . . 79

• LIST OF FIGURES xiv

CHAPTES FM:Figure S.l Dimensions and materials of the laboratory scale thermosyphon

probe container 81

Figure S.2 The probe positioning inside the liquid metal bath . . . . . . . .. 84

Figure S.3 The experimental set-up . . . . . . . . . . . . . . . . . . . . . . . .. 85

Figure S.4 The data acquisition monitor during a routine test . . . . . . . .. 86

CHAPTES SIX

Figure 6.1 Vertical sections and allocation of nodes in the HEATPIPE model92

Figure 6.2 Cross section of a nodal ring in the HEATPIPE model . . . . .. 93

Figure 6.3 Main menu screen for HEATPIPE 1.0 98

Figure 6.4 Working substance screen for HEATPIPE 1.0 98

Figure 6.S Boundary condition screen for HEATPIPE 1.0 99

Figure 6.6 Configuration screen for HEATPIPE 1.0 99

Figure 6.7 Temperature profile screen for HEATPIPE 1.0 100

Figure 6.8 System parameter screen for HEATPIPE 1.0 " lOI

Figure 6.9 System limits screen for HEATPIPE 1.0 " lOI

Figure 6.10 Geometry and configuration of the sample " 102

Figure 6.11 Schematic of the computational domain " 104

Figure 6.12 A typical control volume for 2-D situation. . . . . . . . . . .. 105

Figure 6.13 The flow cbart of the solidification program . . . . . . . . . .. 108

Figure 6.14 Temperature distribution through the centre line for a slow

cooling case 110

Figure ~.15 The cooling curve of an AI-7% Si sample for a slow cooling

rate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. III

Figure 6.16 The cooling curve of an AI·7%Si sample for a fast cooling rate 112

Figure 6.17 Slow cooling solidification patterns at different times during

solidification . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 114

Figure 6.18 Fast cooling solidification patterns at different times during

solidification . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 114

Figure 6.19 A comparison of solidification rates for slow and fast cooling

rates . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 118

• LIST OF FIGURES xv

CHAPTES SEYEN

Figure 7.1 The cooling curve obtained by the conventional method for pure

Al 121

Figure 7.2 The general view of the results for a pure AI test by the probe 122

Figure 7.3 The cooling curve obtained by the thermosyphon probe for pure

Al 124

Figure 7.4 Quasi-equilibrium solidification with the thermosyphon probe. 125

Figure 7.5 The cooling curve obtained by the conventional method for a

413 alloy 126

Figure 7.6 The cooling curve obtained by thermosyphon probe for a 413

alloy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . " 127

Figure 7.7 The cooling and heating curves of 413 alloy 128

Figure 7.8 Effect of cooling rate on depression of eutectic temperature of

an Al-7% Si illoy " 129

Figure 7.9 The Meltlab screen for a 356 alloy obtained by the

thermosyphon probe in low cooling rates 132

Figure 7.10 The Meltlab screen for a 356 alloy obtained by the

LIST OF FIGURES xvi

thermosyphon probe in medium cooling rates . . . . . . . . . . . . .. 133

Figure 7.11 The Meltlab screen for a 356 aIloy obtained by the

thermosyphon probe in higher cooling rates . . . . . . . . . . . . . .. 134

Figure 7.12 Comparison of cooling curves of an unrefined and grain

refined 356 aIloy at the liquidus portion of solidification obtained by

the probe . . . . . . . . . . . . . . . . . . ., 136

Figure 7.13 Effect of Ti concentration on the liquidus portion of the

cooling curve for an Al 6%Si alloy . . . . . . . . . . . . . . . . . . .. 137

Figure 7.14 The microstructure of an unrefined Al-Si aIloy of Figure

7. 13(a) 140

Figure 7.15 The microstructure of a partially refined Al-Si alloy of Figure

7.13(b) 140

Figure 7.16 The microstructure of a partially refined Al-Si alloy of Figure

7.13(c) 141

Figure 7.17 The microstructure of the grain refined Al-Si alloy of Figure

7.13(d) 141

Figure 7.18 Effect of Ti concentration on the liquidus portion of the

cooling curve 142

Figure 7.19 The effect of modification on eutectic temperature of a 356

alloy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 143

Figure 7.20 Effect of Sr concentration on eutectic temperature of a 356

alloy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 144-

Figure 7.21 Effect of Sr content on eutectic temperature for 356 alloy .. 145

Figure 7.22 Effect of graduai increase of modifier agent (Sr) on eutectic

temperature of an Al-7%Si alloy . . . . . . . . . . . . . . . . . . . . .. 146

Figure 7.23 The microstructure of an unmodified Al-6%Si alloy . . . . .. 147

Figure 7.24 The microstructure of an Al-6%Si a110y modified by 40 ppm

LIST OF FIGURES xvii

Sr 147

Figure 7.25 The microstructure of an AI-7%Si alloy modified by 85 ppm

Sr 148

Figure 7.26 The microstructure of an Al-7%Si alloy modified by 130 ppm

Sr 148

LIST OF TABLES

CHAPTER nBEE

Table 3.1 Comparison of sorne mechanical properties of non-modified and

modified Al-Si casting a1loys o. 53

CHAPfER FouRTable 4.1 Constants in the pressure-temperature equation for saturated

vapor 75

Table 4.2 Selected properties of potassium and cesium as heat pipe

working fluids . . . . . . . . . . . . . . . " 76

CHAPrERSJX

Table 6.1 Variables employed in HEATPIPE model 94

Table 6.2 Equations employed in HEATPIPE model 96

Table 6.3 Results from experimental data and computed simulation 102

Table 6.4 Solidification and sample specifications used in the model . . .. 109

CHAJ'TER SEVEN

Table 7.1 Nominal chemical composition of the Al alloys tested . . . . .. 120

Table 7.2 Variations of cooling rate and eutectic temperature with inner

pressure for the curvc;s of Figure 7.8 . . . . . . . . . . . . . . . . . .. 130

LIST OF TABLES xix

Table 7.3 Summary of grain refinement results . . . . . . . . . . . . . . . .. 142

Tahie 7.4 Summary of eutectic modification results . . . . . . . . . . . . .. 149

a

A

~

Cc

Cp,l

cp,sas

CI,f .

D

l)(X)

e

f.

F

g

go

G

• li

LIST OF SYMBOLS

Fluid parameter for a given material. Governs relationship between

gas phase pressure and temperature at equilibrium.

Cross sectional area of the vapor space, m2.

Area exposed for heat transfer at probe tip=7t (r?-r/).

Cross-sectional area of fluid flow in pipe, m2.

Cross-sectional area available to reagent gas flOW=7trb2.

Fluid parameter for a given material. Governs relationship between

gas phase pressure and temperature at equilibrium.

Stefan-Boltzmann constant=5.669x 10-8 W/(m2_K4).

Molar density of gas/vapor mixture, kgmol/m3•

Specific heat of saturated liquid at constant pressure, Jlkg-K.

Heat capacity of reagent gas, J/kg-K.

Coefficient ofEq. 2.4, depends on surface liquid combination.37

Diameter, m.

Condensate thickness over a distance (direction) x, m.

Surface emissivity.

Solid fraction.

View factor for radiative heat transfer.

Gravitational acceleration=9.Slm/s2.

Proportionality constant= 1 kgmN-l.s-2.

Mass of working substance in pipe, kg.

Average condensation heat transfer coefficient over a distance

LIST OF SYMBOLS•hbollom

hrg

hgas

h,cxtl,

hi,ws

htip,ws

H

ka

k"kl

le.la

1.

1.~

~g,rr

Il

mm

M

M'

Il,

n

xxi

(direction) x, W/(m20C).

Heat transfer coefficient, environment with probe tip, W/(m20C).

Latent heat of vaporization of working substance, J/kg.

Heat transfer coefficient, reagent gas with inner pipe, W/(m20C).

Heat transfer coefficient, ith node, outer periphery of pipe with

ambient enviromnent, W/(m20C).

Heat transfer coefficient, ith node, heat pipe shen with working

substance, W/(m20C).

Heat transfer coefficient at probe tip, heat pipe shen with working

substance, W/(m20C).

Total enthalpy, J.

Boltzmann's constant= 1.38 X 10-23, JIK.

Thermal conductivity of the protective coating, W1(mK).

Thermal conductivity of saturated liquid, W/(mK).

Thermal conductivity of the heat pipe shen, W/(mK).

Length of adiabatic section, m.

Length of active condenser, m.

Length of evaporator section, m.

Vertica1length of ith axial segment, m.

Length of blocked off region predicted by fiat front model =It-I.,m.

Total condenser length including blocked off region, m.

Mass flow rate, kg/s.

Mass of molecule.

Merit number for a heat pipe.

Ment number for a thermosyphon.

Viscosity of saturated liquid, kg/sm

Coefficient of Eq. 2.4, depends on surface liquid combination.37

LIST OF SYMBOLS• II;g

P

Pgas

Py

Prl

"q crit,b

q",

<Ii"

<Ii,b

lhipR

rb

rc

ri

fi,e

r· f1,

ri,g

PI

Pr

Py

(J

t

tet.T

T.mb,i

Tb,••

xxii

Moles of inert gas contained in the pipe.

System pressure, Pa.

Pressure in reagent gas line, Pa.

Vapor pressure, Pa.

Prandtl number of saturated liquid, tJ.Cp/k.

Critical heat flux of boiling("boiling limita), W1m2•

Heat flux in nucleate pool boiling regime, W1m2•

Energy transfer from environment to working substance,ith node, W.

Energy expelled from working substance to reagent gas,ith node, W.

Energy transfer from environment to working fluid, probe tip, W.

Gas constant=8.314 Nm/(molK).

Inner radius of inner pipe; m.

Outer radius of inner pipe, m.

Internal radius of heat pipe outer shell, m.

Inner radius of outer pipe, ith nodal ring, m.

Outer radius of outer pipe, ith nodal ring, m.

Outer radius of protective refractory, ith nodal ring, m.

Liquid density, kg/m3•

Density of ~gent gas, kg/m3•

Vapor density, kg/m3•

Surface tension, N/m.

Time, s.

Thickness of coating at probe tip,m.

Thickness of pipe shell at probe tip,m.

Temperature, K.

Temperature of external environment, ith node, K.

Temperature of pipe bottom, exposed coating surface, K.

LIsT OF SYMBOLS•

Tcnv,tip

Ti ,&

Ti-l,.

T' b"Ti.:

T· f"

T.ol

T.Tw

Tws

u(y)

Vg

Vig

xxiii

Temperature of pipe bottom, inner edge of protective coating, K.

Temperature of pipe bottom, inner edge in contact with working

substance, K.

Temperature of ambient environment, probe tip,K.

Bulk temperature of reagent gas, ith node, K.

Bulk temperature of reagent gas, node i-l (node above ith node), K.

Temperature of inner wall of inner pipe, ith node, K.

Temperature of outer wall of inner pipe, ith node, K.

Temperature of inner wall of outer pipe, ith node, K.

Temperature of inner wall of protective coating 1outer wall of outer

pipe, ith node, K.

Temperature of outer wall of protective coating, ith nodfi, K.

Temperature of reagent gas, K.

Liquidus temperature, K.

Solidus temperature (Eq. 6.21), K.

Saturated vapor temperature, K.

Wall temperature, K.

Temperature of working substance, K.

Velocity profile in the condensate film, mIs.

Velocity of reagent gas, mIs.

Volume consumed by inert gas plug, m3•

CHAPTER1

INTRODUCTION

1.1 Scope of the Present Study

The heat pipe is an innovative engineering structure characterized by its

high capacity to transfer thennal energy through relatively small cross-sectional

areas over minimal temperature gradients. A heat pipe contains no moving parts

and requires no external power or mass input during operation. More importantly,

the heat transfer rate is also controllable. A heat pipe is basica11y a closed chamber

with a material inside called the working substance (or fluid). Its ability to transfer

energy is based on the large latent heat of vaporization and condensation of the

working fluid. Heat is absorbed over the evaporator, vaporizing sorne of the

working fluid. The vapour travels to the condenser portion and condenses by

giving off the latent heat of condensation. This fluid is then returned to the

evaporator and the cycle continues. In agas loaded heat pipe the presence of an

inert gas leads to the control of the rate of heat absorption from the evaporator.

The principle of the heat pipe was conceived in 1942,1 and since then, heat

pipes in various fonns and designs have found a wide variety of applications. For

metallurgical applications, one can only find a few papers dealing with heat pipes,

mostly on the use of heat pipes in the cooling of casting molds(see 2.7).

• CHAPTER ONE 2

At present, one of the newest methods for quality control of Iiquid

aluminum alloys is "the thermal analysis technique". Conventional thermal analysis

techniques graphically monitor the temperature changes in a sample as it cools

through a phase transformation interval giving the so called "cooling curve". The

proper chemical analysis of a melt is a necessary but not a sufficient parameter to

produce quality castings since it does not indicate the size, shape, proportion, or

distribution of the phase features that affect the mechanical and physical properties

of a multiphase alloy. Analysis of the temperature-time cooling curve allows the

metailurgist to monitor the progress ofcertain metailurgical phase transformations.

More specifically, thermal analysis can provide an evaluation of the potential

nucleation and modification state of the melt prior to casting. Thermal analysis can

thus estimate the potential of the melt to solidify with a specifie microstructure.

The microstructure developed during solidification depends not only on the

nucleation potential and modification potential of the melt, but also on the thermal

gradient imposed during solidification. The characteristic cooling curve parameters

are correlated with the proper state of nucleation and modification in the melt

required to produce the desired microstructure in a specifie casting section size.2

Thermal analysis is carried out by pouring a relatively smallliquid sample

of the melt into a sampling cup. The liquid metal is then allowed to solidify with

a thermocouple fixed in the centre of the cup and connected to a data acquisition

system. The physical and thermal characteristics of the sampling cup in any one

given test determine the effective cooling rate.

Upon completion of successful design and manufacture of a self cooled heat

pipe injection lance3 and significant contributions to the understanding of the

conventional thermal analysis of aluminum silicon casting alloys4.s.6.7 at McGiII

University, the novel idea of thermal analysis of aluminum alloys using a heat pipe

• INTRODUCTION 3

probe was initiated. It was realized that since solidification by nature is a heat

removal process from a liquid sample, a heat pipe might be used to force

solidification. The idea was to develop a heat pipe probe to permanently reside in

the liquid metal bath and to solidify a small volume of liquid (button shaped

sample) in a large ladle of molten metal. The gas loaded feature of the heat pipe

probe enables the system to:

i) Reverse the freezing process and remelt the solidified sample after

completion of a thermal analysis test. This allows the thermal

analysis technique to be semi-continuous.

ii) Impose a desired cooling rate on the freezing sample.

Consequently, a wide range of cooling rates from extremely low to

those typical of cooling rates in die casting can be obtained with the

same set-up and for the same batch of liquid metal.

iii) Computerize and automate the entire quality control process.

Since no sample is manually taken and the desired cooling rate is

adjusted by the inner pressure, no sampling cup is needed and the

cooling rate may be set automatically.

This research work contains two distinct aspects: 1) heat transfer (solidification

and melting) with a heat pipe, and 2) thermal analysis of aluminum-silicon alloys.

The objective of the present research work was to develop a probe usable in liquid

aluminum alloys to perform improved thermal analysis and to compare the results

of the new method with those of the conventional thermal analysis technique,

emphasizing grain refinement and eutectic modification treatments. The new

technique to be elaborated upon in this thesis is, semi-continuous, applicable to a

wide range of solidification rates, computerized and automated. These features are

not found in the conventional thermal analysis technique.

After developing and proving the viability of the heat pipe probe for the

• CHAPTERONE 4

thennal analysis of aluminum foundry alloys, a research effort is now underway

on development of the next generation of the probe (intelligent heat pipe probe) at

McGill University through a strategie grant. The next generation will be focused

on further quantification of the metallurgical aspects of cooling rates, grain

refinement, and eutectic modification that were investigated semi-quantitatively in

the present work.

1.2 Overview of the Present Work

As mentioned earlier, heat transfer by a heat pipe and thennal analysis of

aluminum silicon alloys are two distinct aspects that are combined in the present

work. This thesis elaborates on the connection between these two distinct

principles. This work details the author's experimental and computational efforts

to develop the new thennal analysis method for aluminum silicon alloys by a heat

pipe based probe.

Chapter Two reviews briefly the literature on heat pipes. The history,

operating principles, various types, brief theory, and applications of the heat pipe

are discussed. Emphasis is placed on the type of heat pipe used in this work Le.

the gas loaded annular two phase thermosyphon.

In Chapter Three, the metallurgical background of the work, including

liquid metal treatrnents such as grain refinement and eutectic modification is

discussed. The chapter ends with a review of the conventional thennal analysis

technique and equipment that is currently used.

Chapter Four describes the steps that were undertaken in the developrnent

of the heat pipe probe. It elaborates on the probe design including the critical step

of materials selection and also specifies the characteristics of the probe.

Chapter Five details the experimental part of the work. The set-up of the

• INTRODUCTION 5

components and the expt:rimental procedure for the new method of thermal

analysis by the heat pipe probe is explained.

Chapter Six deals with modelling of the heat transfer. It contains two

computational models; one is a software package called HEATPIPE 1.0 used to

perform rapid, easy simulation of the heat pipe probe. This model was initially

developed to simulate the heat pipe injection lance, but it is adapted to the heat

pipe probe by applying the proper boundary conditions. The other mathematical

model simulates general solidification behaviour of the freezing sample during a

thermal analysis test by the probe. Good agreement is found between the computed

and experimental results. Aiso, sorne parameters which are difficult to obtain in

practice such as solidification rate (temperature/distance) are evaluated. For the

sake of brevity, a limited number of results from the mathematical model are

presented in Chapter Six.

Chapter Seven details the results obtained by the new method and discusses

them. This chapter is divided into two parts. The first part illustrates typical results

regarding a general view of the cooling curves obtained by the probe. Comparisons

are made between the cooling curves of the conventional and the new mt;thods.

Features of the new method in terms of cooling rate adjustments, are shown in this

section. The next part includes results from sorne parametric studies and features

a discussion on the grain refinement and modification of one of the most

commOlùY used aluminum silicon alloys (356). The results presented in this

chapter are basically semi-quantitative.

The thesis cornes to an end with a set of conclusions summarizing the

results of the work. Finally, concluding remarks, claims to originality, and

suggestions for future work are the basic elements of Chapter Eight.

·c.•·..•••• RAP'fE..•..•....• >( ···R. ' .. _. ' "

..~.

~

HEATPIPE

2.1 Introduction

The worldwide emphasis on energy conservation with regard to exhaustible

energy sources such as gas and oïl has 100 scientists to focus on the development

of new methods and devices with higher efficiencies, less waste of consumable

materials and lower maintenance costs.

The heat pipe is such a device that meets these criteria. The heat pipe is an

innovative engineering device with a capacity to transfer large quantities of heat

from one point to another. In a heat pipe, thermal energy is absorbed at one end

and is dissipated at the other. Its ability to transfer heat is basOO on the large latent

heat of vaporization and condensation of the material sealOO inside: the so called

"working substance". In a heat pipe, the working substance lasts indefinitely and

no extemal inputs are needOO for the operation of the device.

A heat pipe can transfer heat at high rates over considerable distances with

ooly a relatively small temperature gradient. More importantly, especially with

regard to this research work, the rate of heat transfer can he well-controlled.

Additionally, the heat pipe is simple in structure, relatively inexpensive, contains

no moving parts and is reliable in its operation.

• HEATPlPE 7

2.2 History

In 1944 R. Gaug1er, an automotive engineerB, patented a heat transfer

device to he used in refrigeration systems.9 It was not until 1963 that Graver et

al. 10 ofLas Alamos Scientific Laboratory independently invented the idea and built

prototypes. He also named the device a "Heat Pipe". Grover used water as the

working substance in bis first heat pipe prototype for ambient temperature regimes

and shortly thereafter, he expanded the application to bigh temperatures by using

sodium at 11OOK,92.

The idea of a gas-Ioaded heat pipe was first explored by Hall of ReA in a

patent application :ln 1964. Nevertheless, although the effect ofa non-condensable

gas was shown in Grover' s original publication, its significance for acbieving

variable conductance was not immediately recognized. In the subsequent years, the

theory and techno10gy of gas-Ioaded variable conductance heat pipes was greatly

advanced, MOSt notably by Bienert and Brennan at Dynathermll and Marcus at

TRWI2•

Aside from the advances realized from the various heat pipe applications,

basic research and development have also continued. Analytical techniques and

computer programs have been developed to predict performance and design

parameters for Many applications13 •

In terms of the literature, the first Heat Pipe Design Handbook was

published in 1972. Since then several international heat pipe conferences have been

conducted, and numerous papers and books on heat pipes have been published.93

Our latest patent search in January 1994 shows about five thousands patents

worldwide on different heat pipe applications. Research and deve10pment on heat

pipes for different applications is increasing rapidly. As a result, revo1utionary

advances on new heat pipe applications are anticipated.

• CHAPTER. Two 8

2.3 Operating Principles

The heat pipe is a thennal device for transporting heat from one location to

another over a relatively small temperature gradient. 10.14 It is typically an evacuated

closed tube or chamber, varying in shape and size9 (Fig. 2.1). In its simplest fonn,

a heat pipe consists of a container, a material inside commonly called the working

substance and, possibly a capillary wick structure.

Hest output

t t t t

Uquid f10w \lapor f10w'Mck

Heat input

++++

Container

~~ tL ,...~ __ ~:"":,+section section section

Fig. 2.1 Components and principle of operation of a conventional heat pipe.

Heat is supplied at one section, called the evaporator or hot section, thereby

vaporizing the internal working substance. Due to a pressure gradient established

within the chamber, the vapor travels to another part of the pipe called the

condenser or cold section, where it is condensed on the walls thus releasing the

absorbed latent heat of vaporization. This energy transport is accomplished by

means ofliquid vaporization in the evaporator, vapor flow in the core region and

vapor condensation in the condenser. The condensate, then, returns to the

evaporatorl4• The condensate return mechanism depends on the type of heat pipe.

In a wicked heat pipe, capillary action is employed to pump the condensate back

to the evaporator. In a wick1ess heat pipe, usually called a thennosyphon,

• HEAT PIPE 9

gravitational force is used and a wick structure is not necessarily needed. The

cycle of evaporation and condensation will continue if the flow passage for the

fluid is not blocked.10 Sometimes an intermediate adiabatic (no heat transfer)

section lies between the heat source (evaporator) and sink (condenser). This

adiabatic region is created by externally insulating the appropriate section of the

heat pipe.

Since there is ooly a very small pressure drop over the length of the pipe

(order of 1% or less1S), the evaporation-condensation cycle is essentially an

isothermal process where the temperature may be considered equal to the saturated

vapor temperature corresponding to the vapor pressure of the working substance.

However, according to the second law of thermodynamics, no heat pipe can ever

be considered to be perfectly isothermal18•

The tremendous heat transfer ability of a heat pipe is due to the large

quantity of energy absorbed and released by the phase change. The amount of

thermal energy that can be transported as latent heat of vaporization is usually

several orders of magnitude greater than that which may be transported as sensible

heat in either convective cooling or conductive cooling. For a given cross-sectional

area, a heat pipe cao transport fifty to a thousand times more heat than a copper

conducting bar. For this reason a heat pipe is sometimes called a "super­

conductor" 8,14,17,18,19 of heat.

Heat pipes cao be used at many different temperatures. When heat transfer

is a dominant problem heat pipes are often amenable to the task. The proper

selection of the working substance material for a given application is an important

consideration.

2.4 Beat Pipe Types

To date, many different types of heat pipes have emerged. Heat pipes may

• CHAPTER Two 10

he classified by various means. The more common aspects are:

.Working temperature range: High, moderate, low (sub-zero and

cryogenic) temperatures.

• Method used to transport the working substance from the condenser to the

evaporator: Capillary force is used in the standard wicked heat pipe and

~

~r ~

"r ~

~

~r .."r ~

~

~~ ..~r

..

~k)-~- - -- - -

1- - -

..­..-

..­---. ..-Fig. 2.2 A two-phase closed thermosyphon.

..

..

gravitational force in the wickless heat pipe. The latter is called a

thermosyphon.

• Presence of non-condensable gas in the system.This leads to an important

group of heat pipes known as gas-Ioaded or variable conductance heat pipes

(VCHP).

• Physical shape of the envelope. The container may have any shape that

can reasonably be fabricated. Cylindrical heat pipes are more common and

may consist of simply a hollow tube or annulus.

For different applications severa! combinations of the above classifications

• BEAT PIPE 11

may he employed.

For the sake of brevity, the topic of concentration for the balance of this

volume will be that particular kind of heat pipe utilized in this research work,

unless otherwise stated.

2.4.1 Thermosyphon: "... A thermosyphon is a prescribed

circulating fluid system driven by thermal buoyancy forces. This

definition inclut/es ail basic studies to which the name thermosypJwn

has been applied in the literatur~9 . . . ".

The two-phase thermosyphon is essentially a gravity- assisted heat pipe. The

wick structure is not compulsory. Since it uses gravity to return condensate to the

evaporator, it requires the heat source to be located below the heat sink, Le., the

evaporator must be below the condenser. Fig. 2.2 shows a typical thermosyphon

schematically. In fact, a thermosyphon uses gravitational forces, thermal buoyancy

(either locally or in a general sense) forces and vapor pressure forces to transport

the liquid phase of the working fluid. 19•2O The generated vapor in the evaporator

moves up the pipe to regions of lower pressure. In the condenser, the vapor is

condensed to a liquid, lowering the density and pressure. The condensate, then,

returns to the evaporator via gravity. Since the condensate return is in the body

force direction, the system is restricted to the upward heat transfer direction and

therefore, acts as a thermal rectifier1•( ... thermal diode22).

Comparing the maximum heat flux in a standard (wicked) heat pipe versus

thermosyphon, it has been shown that in a thermosyphon, the critica! heat fluxes

are about 1.2-1.5 times larger than for the equivalent wicked heat pipe12.

Additionally, the thermosyphon is simpler in construction, has wider operating

limits and the fabrication cost is lower23 than in the case of a wicked heat pipe.

One type of heat pipe is the " concentric annular thermosyphon" which is,

• CHAPTER Two 12

schematically depicted in Fig. 2.3. This kind is constructed from Iwo pipes of

different diameters. One pipe is placed inside the other and then sealed at the ends

by end caps to create an annular vapor space. The advantage of this type over the

conventional thermosyphon is the increased area for heat transfer into and out of

the pipe without any increase in the outside pipe diameter, Le., the heat transport

per unit length in an annular thermosyphon will be more than is the case for a

conventional design. AIso, the cor:centric design will be as easy to manufacture as

Fig. 2.3 Concentric annular thermosyphon.

a standard one, requiring no expensive tooling or other special treatment2".

2.4.2 Gas-Loaded Thermosyphon In many applications, adequate thermal control

of the thermosyphon is essential. The operating state of a conventional

thermosyphon is, in fact, governed by heat source and sink conditions14, e.g., with

an increase in heat load the operating temperature of the thermosyphon rises.

Likewise, a drop in heat load will result in decreased operating temperature. In

practice, it is often desirable to maintain the thermosyphon within a set temp­

erature range. AIternatively, as in this research work, it is desirable to control the

rate of heat absorption and dissipation into and from the thennosyphon with a

constant heat source temperature. There are severa! methods to produce such beha­

vior. One of the most important consists of loading a portion of the condenser with

a non-condensable (inert) gas.

A gas-Ioaded thennosyphon also known as a two-component heat pipe14

• BEAT PIPE

1 Evaporator 1 Adive condenser

......

13

1Gas-blocked condenser

..

AxIal positionFig. 2.4 Schematic diagram and temperature distribution of agas loaded heatpipe. 99

(thennosyphon) involves a non-condensable gas and a gas reservoir attached to the

conventional thennosyphon shen. When a non-condensable gas is present in such

a system, it moves with the vapor* toward the condenser. Since the gas does not

condense, it concentrates at the condenser end fonning a agas plug"2S. The

presence of this gas plug in a portion of the condenser prevents the vapor from

*) 'The tenn vapor is used ta denole the gaseous phase of working substance for the balance of Ibisvolume.

condensing in that section and acts as a diffusion barrier to the flowing vapor. In

fact, the gas plug tends to ·shut-off" the portion of the condenser which it fills,

leading to an axial temperature gradient along the thermosyphon as shown

schematically in Fig. 2.4. By varying the length of the gas plug, one varies the

active condenser area and, therefore, the heat rejection of the system. The non­

condensable gas section allows the operator to have control over the operating

pressure and temperature of the pipe.

Regarding the controllability of a gas-loaded thermosyphon, two types may

be considered;

i) Fixed quantity of inert gas inside the pipe with variable source

temperatures.

li) Variable quantity (pressure) of inert gas with a fixed heat source

temperature.

The former is more popular and has been widely studied whereas no

publications were found concerning the latter type. The latter type is investigated

in this research work and will be discussed in some detail.

The fixed mass of gas introduced into the system occupies a certain portion

of the condenser. The size of this portion depends on the operating temperature of

the pipe's active region and the environmental conditions. If the heat source

temperature increases, the working substance vapor pressure increases, resulting

in the compression of the· non-condensable gas into a smaller volume, thus

providing a greater active condenser area. On the other hand, once the heat source

temperature decreases, the vapor pressure of the working substance decreases and

the gas inventory expands to a greater volume, thus blocking a longer portion of

the condenser area. This reduces the temperature response of the active zone to

extemal conditions.94,9S

In the case of a fixed temperature hot medium with a variable mass of non-

CHAPTER Two 14

condensable gas, a given quantity of gas will produce sorne defined set of

equilibrium conditions, i.e., a certain length of inactive condenser. Adding more

gas into lite system enhrges the shut-off length of the condenser and reduces the

area available to heat transfer in the thermosyphon thus raising the working

substance temperature. Removing gas from the system, reduces the blocked part

of the condenser, increases the area available to heat tI'l'..nsfer and, as a result,

• HEATPlPE 15

T Il: Inerl gas 1(Q

Z -:>~ .l:

" Gravily en~(..

c

"'QC y8 Vaporflow

'1(''Ir'" Uquld film

l("'y"

J l fi..

Jt •.J_"- • etlnetln qln

~(a) (b) (c)

Fig. 2.5 Schemalic of agas loaded thennosyphon in three different cooling rate modes;

a) AJmost no heal transfer correspondlng to remelllng perlod,

b) Law heat transfar rate corresponding to Iow rate of cooOng,

c) H1gh heat transfer nale corresponding 10 h1gh nale of cooOng,16,80

•reduces the working substance temperature. Fig. 2.5 illustrates a gas-Ioaded

thermosyphon in three different heat transfer modes. Note that the bounding

conditions for the three modes are identical. In mode (a), the pressure of the gas

• CHAPTER Two 16

is gre&ter than the equilibrium vapor pressure of the working substance 'lt the

evaporator temperature. Thus, the gas plug fills the whole available condenser

length (volume) and there is no room for condensation. This statement is valid if

diffusion of the working substance vapor phase in the inert gas phase is relatively

smal1. Generally, this is a valid assumption and it implies a very limited rate of

vaporization and condensation of the working substance with the inherent result of

minimal heat transfer between the evaporator and the condenser. Consequently,

this mode can be seen as a "turned-off" mode. In case (b), the pressure of the gas

is smal1er than the equilibrium vapor pressure of the working substance at the

same temperature. Here, the condenser is divided into a hot (active) zone and a

cold (inactive) zone and sorne heat transfer by vaporization and condensation

occurs (two-component thermosyphon). In mode (c), a larger amount of absorption

and dissipation into and from the system exists (conventional thermosyphon).

2.5 Beat Pipe Theory

Heat pipe theory encompasses the fundamental laws of thermodynamics,

heat transfer, fluid dynamics and materials science. Despite its simple appearance,

a theoretical analysis of the heat pipe cycle involves the complex, multidimensional

conjugate effects of transport phenomena, interfacial phenomena and

thermodynamics. Generally, the circulation process in a heat pipe is weIl described

by hydrodynamic theory. The most important function of the working fluid

circulation is to establish heat transfer within the heat pipe. Therefore, the

maximum heat transfer capability of a heat pipe arises from the maximum possible

circulation!8. On the other hand, the circulation process is affected by sorne

interfacial phenomena inside the pipe such as surface tension, wettability,

capillarity and the liquid/vapor shear force. Furthermore, the internaI heat

transport process within a heat pipe is a cycle subject to the first and second laws

of thennodynamics.

Several Ph.D. level research studies have been conducted on the

investigation of tubular thennosyphons. 26,27,28,29,30 A detailed theory of heat pipe

operation is beyond the scope of this experimental effort. However, to successfully

design and use a heat pipe in a given application, a general knowledge of heat pipe

theory is essential. Hereafter, in this volume, a macroscopic approach to the

thennosyphon cycle and the dominant factors affecting it will be utilized.

2.5.1 Thermodynamics: From the thennodynamics point of view, a

thennosyphon involving liquid/vapor phase transition can only operate between the

triple point" and critical point""" of the working substance. These two bounding

points are rarely approached in practice, but represent the theoretical limits of

operating temperature.

Il ...The fact that thermodynamic equilibriwn exists at

the liquid/vapor interface is central to the

understanding of the thermodynamic state of the

worldng fluid in the heat pipe . . . wU

Therefore, the phase equilibrium conditions must be satisfied at the liquid

Ivapor interface. Using the Clausius-Clapeyron equation, it can be shown that:

• HEAT PIPE

hp=c exp(-~

17

2.1

In the above equation, a constant latent heat of vaporization and ideal gas

behavior have been assumed.

At temperature Tl' a certain amount of heat is applied to the system and

at temperature T2 <Tl the same amount is rejected. In titis system "work" is

**) Triplo point-Tho cœdition wbo!e saUd, liquid and gasoous phases cooxist in oquilibrium•

***) CritiCli point- Tho cœditiODS (T,P) al wbich tbe vapor ancIliquid arc indistingWshablo61.

• CHAPTER Two 18

internally generated and then totally consumed. The energy conversion arising

from the phase change occurs across the liquid/vapor interface where sorne thermal

energy is converted to mechaJùcal energy with the appearance of the pressure

head18.

In the general case, regarding the first law of thermodynamics, the

difference between the aJOount of heat input (in the evaporator zone, QJ and the

heat output (from the condenser zone, QJ is the work that is produced:

2.2

The thermal efficiency of the thermodynamic cycle ofany heat pipe can be defined

as:

2.3

Regarding the thermal efficiency, heat pipes can be classified into three

groups as follows:

i) llT > 0, heat pipes employed basically for converting thermal energy into

other kinds of energy.

ü) llT = 0, classical heat pipe as a heat transfer device.

ili) llT < 0, active control heat pipe31.

2.5.2 F1uid Flow: Flow in a thermosyphon is a rather complex process.

During normal operation, there is a continuous flow of working substance from

the evaporator to the condenser in vapor state and from the condenser to the

evaporator in liquid state. The vapor rises along the central core of the pipe

whereas downward liquid movement occurs along the pipe surface to the liquid

pool. Fig. 2.6 illustrates the actual and ideal flow in a thennosyphon

schematically. Also, there is continuous interchange of mass between the liquid

and vapor phases in the evaporator (liquid to vapor) and condenser (vapor to

liquid) sections. In the evaporator, the heat input causes a net flux of working

substance molecules to move from the liquid pool surface and possibly from the

wetted surface of the evaporator.

• HEAT PIPE

....""

- 1\( c-on

1 1

,jl

j L

fttn-

) \ r-b

1pool .E-

Z

f-I

!

19

(a) (b)

Fig. 2.6 Comparison of actual and idealized flow in a thermosyphon;(a) actual, (b) ideal.

The velocity of the bulk vapor flow is detennined by the rate of heat flow into the

evaporator plus the total pressure of the chamber. On the other hand, in the

condenser, a lower temperature causes subcooling of vapor and a net flux of

molecules enters the liquid surface. Similarly, the velocity of the bulk liquid flow

is detennined by the localized rates of condensation. Consequently, the liquid film

thickness is not unifonn, not smooth, and may be covered by a complex system

of waves32•

The addition of mass to the downward liquid stream increases the

momentum flow rate (mass flow rate times velocity) thus causing a pressure drop.

• CHAPTER Two 20

Finally, a liquid pressure gradient occurs along the flow of condensed liquid

flowing back from the condenser to the evaporator. Removal of the mass from a

flow stream reduces the momentum flow rate, causing a pressure rise that leads

to a bulk pressure gradient through the vapor flow passage. In a thermosyphon,

an additional pressure drop by gravity also exists. Also, d pressure drop in both

liquid and vapor phases is produced due to frictional resistance at the liquid/vapor

interface. Since vapor flow velocity is normally much higher than liquid stream

velocity, pressure changes resulting from variations in the momentum flow rate are

generally significant for the vapor stream. Additionally, in terms of body force

action on the flow streams, pressure change is ooly significant in the liquid flow

stream because of the liquid's much greater density. The liquid friction pressure

drop is added to the pressure change due to gravity in order to obtain the total

liquid pressure rise.96,97

2.5.3 Beat Transfer: Transmission of heat is the dominant principle in any

thermosyphon application. Reat can enter and leave the pipe by several different

heat transfer mechanisms such as conduction into and out of the pipe,

environmental convection, boiling (vaporization) and condensation and/or

radiation. An electrical analogy of the equivalent thermal resistance, R, can be

stated with the associated heat flows and temperature drops, ÔTI4.

Reat transfer mechanisms inside a thermosyphon are govemed by the

following processes:

.Evaporation in the heat source zone.

• Condensation in the sink zone.

• Vaporlliquid interfacial heat and mass transfer in the transport zone.

• Some thermosyphon parameters such as heat flow rate, nature and state of

working substance, and system geometry affect these parameters and, thus, the

performance of the thermosyphon.

• HEAT PiPE 21

In the most general case, investigation of thermosyphon operation may be

classified into two groups22.42:

i) Investigation of heat transfer mechanisms inside the pipe such as

evaporation, condensation and convection heat transfer coefficients.

ü) Investigation of heat transfer limits characterized by a decrease in

total heat transfer due to a blockage of the fluid flow.

If the maximum heat transfer capacity has not been exceeded, the heat transfer

mechanisms are nucleate boiling in the evaporator and film condensation in the

condenser.

Heat transfer in the evaporator originates from standard "boiling heat

transfer" described in heat transfer texts. Consider a heating surface (with surface

E

A log âT=T...T.Fig. 2.7 Pool boiling regimes;

q=heat input, Tw=surface temperature. Ts=pool temperature.

...j

•temperature Tw) immersed in a liquid pool whose temperature (T~ is kept at the

boiling point corresponding to the pressure of the system. The different regimes

ofboiling for such a system are shown in Fig. 2.7. In the region A-B, convection

is responsible for the movement of fluid to the evaporating surface. By increasing

the input flux, bubbles hegin to form at the surface. As the temperature difference

increases, bubbles form more rapidly and rise to the surface of the liquid. The heat

transfer rate is intensified (region B-C). This region shows nucleate or pool

boiling. In the pool boiling regime, high heat transfer rates are associated with

small values of the excess temperature. The heat flux in pool boiling cannot be

increased indefinitely. At point C, bubbles are formed so quickly that they blanket

the heating surface and it hecomes difficult for the liquid to reach the hot surface.

A vapor film forms. Heat transfer from the surface to the liquid occurs by

conduction through the vapor. The temperature difference increases rapidly and

this condition is known as the bumout boiling crisis, or critical heat flux. The

region C-D is called partial film boiling in which boiling is unstable, Le.. the

surface is altemately covered by vapor and liquid. In region D-E the vapor film

is stable34.

Boiling heat transfer is characterized by several distinct parameters

associated with bubble initiation, formation and growth. The process is not as

thorough1y understood as other heat transfer mechanisms3S. Boiling heal transfer

is described in more detail in other heat transfer texts,3S,36,37

For pool boiling, the dependence of heat flux, q". on the wall superheat is

the basis for the correlation proposed by Rohsenow:

• CHAPTER Two 22

2.4

•In the evaporator, either the "evaporation" or "boiling" mode of heat

transfer can occur. Nevertheless, unless the heat flux is fairly low, the boiling

mechanism will he dominant. It has been observed that the boiling heat transfer

• HEAT PIPE 23

regime in thermosyphons is generally pool boiling. Therefore, Rohsenow's pool

boiling correlation appears to be satisfactocy38.

Heat transfer in the l;~ndenser98 of a thermosyphon is approximated by

Nusselt's laminar, nonrippling film condensation model. The condensation process

on a vertical wall is depicted in Fig 2.8.

Bird et al39 provide a fitting explanation for condensation of pure vapors on

..

•m{x)

. ~.dm _ imnlnlnl q •

dq=hfg+dm . _liii!iiWii!i-..........t!J

J. .m+dm

Vapor movement

Fig. 2.8 Film condensation on a vertical surface.

•a vertical solid surface: (p. 415)

w...Vapor flows over the condensing surface and is moved

toward it by the small pressure gradient near the liquid

• CHAPTER Two 24

surface. Note that there occur small abrupt changes in

pressure and temperature at the interface. These dis­

continuities are essential to the condensation process but are

generally ofnegligible importance in engineering calculations

for pure fluids, Some of the mo/ecules from the vapor phase

strike the liquid surface and bounce off; others penetrate the

surface and give off their latent heat of condensation. The

heat thus released must then flow through the condensate to

the wall, At the same time the condensate must drain from

the surface by gravity flow, . . ",

Despite the complexities associated with film condensation, sorne useful

correlations can be derived by making assumptions that originate from the Nusselt

analysis:

i) Constant Iiquid properties.

ii) Laminar downward flow of condensate.

iii)The '/apor temperature at the edge of the film is equal to the saturation

temperature of the vapor with no temperature gradient in the vapor,

iv) Negligible shear stress between the vapor and the film.

v) Linear temperature distribution between the wall and the vapor

conditions,

Regarding the Nusselt theory, the average value of the heat transfer

coefficient, h, over a distance x is given by:

and the condensate thickness:

• HEAT PIPE 25

An improved analysis of film condensation is presented by Rohsenow6• He

recommended using a modified latent heat of vaporization as:

in equation 2.6. In this case, allliquid properties should be evaluated at the film

temperature Tr=(Ts+Tw)/2 and hrg should be evaluated at Ts.

The total condensation rate may be derived from the equation:

2.8

and the velocity profile in the film is calculated as:

2.9

Although Nusselt's film condensation model was initially developed for a

vertical plate, the above expressions may be used for condensation on the inner or

outer surface of a vertical tube ofradius R, if R»li.3S•36,37,39

In terms of heat (and mass) transfer in a thermosyphon, consider a liquid

surface in a liquid/vapor system. If the liquid is in equilibrium with the vapor at

the interface, the flux of molecules leaving the surface will be equal to the flux of

molecules returning to the liquid and there will be no 1055 or gain of mass. If the

surface gains mass by condensation, the vapor pressure and temperature must be

higher than the equilibrium values. In the vaporization mode, similarly, the vapor

• CHAPTER Two 26

pressure and substance temperature are less than the equilibrium values.

The average velocity of vapour, Va., is given by kinetic theory as:34

8k T 112V =(_8_)

av nm2.10

In the regular cycle of a thermosyphon, there is net mass transfer from the

liquid phase to the vapour phase in the evaporator and from the vapour phase to

the liquid phase in the condenser. Therefore, a true state of equilibrium does not

exist. However, the departure from equilibrium is generally small. If the

interchange of molecules between the phases exists, the phase from which the

molecules are lost must be hotter. Therefore, a temperature gradient develops.

An interface heat transfer coefficient, hi' characterlzes the heat transfer

process along the interface between phases:

2.11

Where ~Ti is the temperature difference across the interface and 'li is the interface

heat flux.

In a thermosyphon assuming the "critical heat transport capacity" is not

exceeded, the condensation heat transfer coefficient is generally much smaller than

those associated with the other mechanisms. Therefore, the heat transport

resistance is dominated by the condensation process.40,41,42

Thermosyphon limitations: For a given working substance (fluid) and

thermosyphon design, a temperature range exists over which the thermosyphon

will be functional. This operating temperature range is dictated by several heat

transport limits. AlI of the limits for successful operation of a thermosyphon are

associated in one way or another with the interruption of mass circulation43• Based

on experimentaI studies, it is well established that performance limits of a

thermosyphon depend on the heat addition to the evaporator (radial evaporator

• BEAT PIPE 27

Vaportemperature

Wall -/temperature

e 0 ­e

heat flux, axial heat flux), geometry of the thermosyphon, liquid filling and fluid

characteristics. Heat pipe (and thermosyphon) limits have been studied

extensively.15,18,32,43,44,45,46,47,48,49

In a thermosyphon, operating limits are described in the literature as the

dry-out limit, burnout or critical heat flux limit, flooding or entrainment limir2 and

the sonic limit. A continuous circulation of working fluid is required for the proper

functioning ofa thermosyphon. When the liquid charge (pool height) is insufficient

and/or when a given heat flux to the evaporator causes the liquid to evaporate

faster than it can he supplied by gravity, the evaporator becomes dry43 (dry-out

limit). Once the evaporator reservoir dries-out, its surface is no longer subjected

to the high cooling rate provided by a wetted surface. As a result, the wall

temperature jumps in the evaporator.32,33 Fig. 2.9 illustrates this phenomenon for

a sodium/stainless steel heat pipe43.

SOO750

~ 700e. 6501- 600

550500

450 6L...00:----:7"="00:---..,S:':0-:'0---::90:-::0..,.-.(,~7.1000Power transferred fY'l)

Fig. 2.9 Sodium charged heat pipe dryout.

However, when the heat input is only to the liquid pool (high liquid

fillings), the performance of the thermosyphon can he limited by the boiling or

critical heat flux limit. This limit is similar to the critical heat flux condition in

pool boiling33 and obeys the saroe principle (see Fig. 2.7). The maximum critical

heat flux q"cril,b is generally on the order of 1()6 W/m2 and has been estimated by

Zubero as the following:• CHAPTER Two 28

2.12

Operation of the thermosyphon below the boiling limit is advisedls .

The vapor and liquid flow in a thermosyphon comprise a countercurrent­

flow condition. If the vapor reaches a high enough velocity due to high input heat

fluxes, a high ~ii.~erfacial shear stress will be established and may cause

entrainment of liquid from the film into the vapor. The heat flux at which

entrainment occurs is termed the entrainment or flooding limit. Onset of this limit

may cause:

i) The accumulation of liquid in the condenser,

ii) Sudden release of the accumulated liquid to the evaporator,

iii) Re-establishment of a film flow regime and finally,

iv) The occurrence of flooding atd film flow reversal whereby the cycle

repeats itselpl.

The entrainment limit is expressed as an axial heat flux: the heat transport

rate per unit of vapor space cross-sectional area.

Several different correlations have been presented to predict the critical heat

flux at which entrainment occurs. For example 16 correlations were examined by

Peterson and Bage. According to them, the studied correlations yielded variations

spanning a geometric factor of fiveS2•

Faghri et al40 presented an improved correlation in order to predict the

entrainment limit for different types of working substanœs as follows:

•2.13

• HEAT PIPE

where

and

P 0.14K=(-I) tanh2Bo1/4

Pv

29

2.14

2.15

In a thermosyphon with a constant diameter for vapor flow, the process of

vapor addition in the evaporator and vapor removal in the condenser causes the

vapor stream to first accelerate and then decelerate as it moves upward. Therefore,

the velocity variation results from a variable mass flow through a constant area.

At an extremely high heat input rate, the vapor velocity leaving the evaporator

may be extremely high. When the vapor velocity becomes sonic at the evaporator

exit, the "sonic limit" is encountered. Any further heat load added to the system

Fig. 2.10 Comparlson of sonie Iimits in Na, K, and Cs heat pipes.•

,.. 3.0E~~"" 2.5x:>~ 2.0

~~ 1.5~

S~ 1.0

~~ 0.5ï=:5 ft ,

400 500 600MAXIMUM EVAPORATOR TEMP. (Ocl

Experimental

- - - - - Calculated

• CHAPTER Two 30

does not increase the mass flow of vapor but causes an increases in the working

substance temperature in the evaporator and, finaUy, a high axial temperature

gradient is established in the thermosyphon. Fig 2.10 displays the sonic limit effect

for different (liquid metal) fluids. 43

The simplest correlation for the sonic limit is given as34•49

q" =0 474h (p .p\ll2s· :tg.'" 2.16

It has been observed that the heat transfer limits in closed two-phase

thermosyphons depend on many factors such as the rate of heat input to the

evaporator, working fluid material, liquid inventory, and operating pressure

(temperature) of the fluid. 32 Among aU the limits, the effective heat transport limit

in a heat pipe is the one with the smaUest magnitude. In a tw<:>-phase closed

thermosyphon, it is generally believed that the entrainment limit is dominant over

the other limits.32,33,40

2.6 Design Considerations

The first step in thermosyphon design is to identify the temperature range of the

heat source to which the evaporator is exposed. From titis, a proper working

substance and shell may he selected. By judicious selection of materials, it is

possible to build heat pipes for use at temperatures ranging from 4K to about

23ooK.34 In titis sense, the vapor pressure corresponding to the operating

temperature is a factor that has to be accounted for. A desirable vapor pressure

generally lies in the range between 6900 and 690000 N/m2 CO.07 to 7 atm.).ls

2.6.1Working Substance: Working substance selection is the first and the most

important step in designing a thermosyphon (heat pipe). It determines the

thermosyphon' s operating temperature range. Fig. 2.11 shows different heat pipe

• HEAT PIPE 31

fluids with their respective operating temperature ranges. These ranges correspond

to a pressure range of 6900 to 690000 N/m2 C 0.07 to 7 atm.). Once the operating

temperature range is identified, the working substance may he selected.

1200

T 1000am ·800pa

600rat 400ur 200a

(C) 0

-200

Soclum Potaulumi--

,.--

Callum

Mercury

Naphtlllane

.Water.i:

Fig. 2.11 Operating temperature ranges of various heat pipe fluids.

Usually, within the approximate temperature range band, several possible working

substance materials may exist. In order to pick the most acceptable material, sorne

other criteria have to he considered such as:

i) Compatibility with the container material,

il) Thermal stability.

iii) Wettability,

iv) Vapor pressure in the operating temperature range,

v) Law melting point in the case that the working fluid is in the sond state

at ambient temperature,

vi) High thermal conductivity,

vii) High latent heat of vaporization,

• CHAPTER Two 32

viii) High liquid and vapor densitiess3,

ix) High surface tension,

x) Low liquid and vapor viscosities.

The effects of the last four factors are gathel'ed together as a 'liquid

Li

Cs

H20

10la

12la

11la

13 r--------{f------...---,la

...o

.oJUco.....oJ...oI:l.alC

~.oJ

'0....6-....o-'l

-N

e......~

a 100 200 300 400 1000 1200 1400 1600

Boiling point (K)Fig. 2.12 Liquid transfer factor at boiling point versus boiling point.

transport factor,ls or 'Merit number'34. In a heat pipe, the ioerit number for a

given working substance is defined as:

2.17

•Fig. 2.12 illustrates the value of a material' s liquid transport factor versus

its boiling point for a variety of working substance materials. IS In a thermosyphon,

the thermal conductivity of the liquid working substance has a more pronounced

• HEATPlPE

effect than surface tension. Thus, the merit number may be defined as34:

3 2..1/4M' = (hlg k/ Po

J.L/

33

2.18

Additionally, the ideal fluid should be not easily contaminated in storage,

readily available and inexpensiveS3 • The quantity of working substance inventory

greatly affects the normal behavior of a thermosyphon. The amount must be

enough to wet all internai surfaces during normal cycling. However, an excessive

quantity is also not desirable. The fluid inventory in a thermosyphon has been

extensively studied.21,23,32,33,34,4O,48 Il has been observed that a quantity which is

too small may result in the dry-out limit6 and leads to a reduction in the maximum

heat flux of the system21 • For liquid fillings which are too large, it has been found

that the liquid is carried up to the cooled section and subcooled there.

Consequently, periodic burst boiling occurs, which causes vibration of the

thermosyphon accompanied by a bursting noise12 and in the Most severe case,

steady-state operation may not be possible because of the entrainment of the liquid

film by the vapor core33 • Bezrodnyi and Alekseenko recommended that the liquid

fill should be at least 50 per cent of the volume of the evaporator4• Also,

according to Streltsov analysis, the following equation yields the optimum fluid

inventory for a thermosyphon.S2

2.19

•2.6.2 The Container: The thermosyphon container isolates the working

substance from the outside environment. Therefore, to maintain the pressure seal

and working substance purity, no leaks should exist. Selection of the container

• CHAPTER Two 34

material is based on severa! factors. A major factor is the compatibility of th~

envelope with both the working fluid and the external environment. Caution must

be observed, particularly in high temperature thermosyphons since corrosion at

high temperature can be especially problematic. Other factors affecting the

container material selection are as follows:

• Temperature characteristics,

.Thermal conductivity,

• Ease of fabrication (weldability, machinability, ductility ... ),

• Strength to weight ratio,

• Porosity,

.Wettability,

.Cost.

The material should be non-porous to prevent the diffusion of gas inlo the

pipe34. Good wettability insures avoiding hot spots on the thermosyphon's wall, a

phenomenon that can cause failure in normal cycling.

It is highly recommended that the container be extremely clean and free of

any contamination such as oil or oxide layer. This is due to the fact that when the

evaporated working fluid condenses, the condensate is highly purified and hence

has maximum capacity to dissolve low-solubility solids and gases. As the

condensate flows down to the ev~porator, it may dissolve a small quantity of

impurities from the wall before reaching the evaporator. In the evaporator, the

solute (impurities) will remain and concentrate there. This can detract from the

normal performance of the thermosyphon.15

Severa! cleaning procedures have been proposed. Generally, cleaning

procedures include the following stages;

• Degreasing

• Solid particle removal

• HEAT PIPE 35

• Deoxidizing

• Degassing

A sarnple cleaning for stainless steel parts is as follows:

1. Clean in 1,1,1, -trichloroethane

2. Rinse with cold trichloroethane and force dry with filtered air

3. Immerse in passivating solution-sodium dichromate (7.5- 30 Kg/m3) ant

nitric acid (15-30% by volume) at room temperature for 30 minutes to 2

hours

4. Two minutes tap wRter rinse

5. Thoroughly dry with forced filtered air

6. Rinse with isopropyl alcohol

7. Force dry with clean, filtered, dry nitrogen heated to 70°C

2.7 Beat Pipe Applications

The heat pipe has been used in a large variety ofapplications. Theoretica11y,

the heat pipe may he applied to an almost limitless number of thermal transport

problems, i.e., the heat pipe application range covers almost the complete

spectrum of temperatures encountered in heat transfer processes. With regard to

the working fluid, liquid helium (with au eful temperature range between -271 to

-269°C) and lithium (with a useful range between 1000 to 1800°C)17 represent the

two bounding limits of the operating temperature range for heat pipe applications

(Fig. 2.11).

As for typical applications, cryogenic heat pipes have been used for cooling

infrared sensors, arnplifiers and laser systems and in medicine for cryogenie eye

and tumour surgery. Moderate temperature heat pipes have been applied to cool

electronie elements. They have been used to cool shafts, turbine blades,

• CHAPTER Two 36

generators, motors and transformers. In heat recovery systems, they are employed

to collect heat from exhaust gases, solar energy and geothermal energy. In

spacecraft, moderate temperature heat pipes have served to control the vehicle's

temperature instruments and space suits. Finally, liquid metal heat pipes have been

widely applied for cooling nuclear and isotope reactors and for heat recovery in

gasification plants. 10 An interesting example of heat pipe application is road

deicing, extensively used in Japan18•

Concrete Surface

1%" Caver

Fig. 2.13 A typical heat pipe used for deicing.

In such a sy,tem, heat is transferred from underground regions, where

temperatures are still above the freezing point, to the grcund level. This deices

critical sections of highways, bridges, and airport runways. Fig 2.13 depicts a

cross section of a heat pipe used for road deicing1o•

Applications of heat pipes in metaBurgy-Among the thousands of different

applications of heat pipes in various engineering fields, only a limited number have

been found in the metaliurgical engineering field. In die casting and injection

moulding processes, heat pipes have been used in two manners. First, heat pipes

• HEAT PIPE 37

may he inserted into the main body of a die to equalize the temperature field in the

die. For example, a die used to produce a cylindrical shaped component may have

a significant temperature gradient along its length. Using a heat pipe in the mold

could minimize the temperature gradient as shown in Fig 2.14.

Hea~es

r x

\'\. Wattr;, ·····,:c ln

d2\......

I~ J,,....·::c Wattr.......

aut", ,

\ \1

ca\ting LxDie

Water

Die

~&:;~/""-Heat pipes

/Casting

View on XX

Fig. 2.14 Thil use of heat pipe to reduce die wall temperature gradients.

In the other case, a heat pipe is used in conjunction with a water cooling system.34

Kunes et alS4 employed sodium heat pipes in combination with a c1assical

passive chill in different steel casting sand mold systems to form an active dynamic

chill. Their main goal was to check the applicability of the heat pipe in foundry

technology, especiaIly during solidification and cooling of large steel castings.

Forced air flow and water were applied to the condenser in order to control the

heat flux removed by the heat pipe. They observed that the active chill provided

a substantiaIly higher and more controllable cooling effect on the various steel sand

mold castings.

BahadoriSS proposed a simple one dimensional analytic approach to

solidillcation in a cylindrical mold peripherally inserted with severnl stabilizing

gas-Ioaded heat pipes. In such a system, liquid metal heat pipes (sodium or

potassium) and argon or helium could be used as working fluids and inert gases.

The latent heat of fusion of the liquid metal casting provides heat input to the heat

pipe. By changing the inert gas temperature stored in the reservoir, the occupied

volume of inert gas may he modified. This, in tum, affects the effective condenser

area and the heat transported by the heat pipe may he controlled. Bahadori used

bis model for 81uminum, cast iron and tin. He concluded that different solid­

ification rates may be maintained for various sections of a casting by proper design

and operation of a heat pipe.

ZuzanaJcS6 developed a smple numerical model to examine the effect of heat

pipes on casting solidification and defined fundamental parameters to control the

solidification process during the extraction of the latent heat of fusion. He

simulated steel casting solidification at constant temperature (freezing point) in a

sand mold by using a sodium heat pipe attached to the chill. Zuzanak ran the

simulator in a sand mold with chill both with and without the heat pipe. He

concluded that during solidification, a heat pipe in contact with the chill in the

mold yields the same effect as cooling the chill by forced convection. Fig. 2.15

shows the physical model of Zuzanak's work.

Wells et 8144 81so developed a computer program to study the effect of a

heat pipe on the temperature distribution throughout a solidifying alloy. Their two­

dimensional numerical model was run for a 6040 lead-tin alloy by using a heat

pipe to influence the solidification process by controlling the rates of heat transfer

from the casting. They found that a heat pipe can effectively influence the

temperature gradients, solidification rates, and the shape of the solid-liquid

interface during solidification. These effects agreed favourably with experimental

CHAPTER. Two 38

• BEAT PIPE

Casting

Ica

Casting

Ica

Adiabatic wall

Chili

Ich

Chili(ch

Heatpipe

39

hco

h ; taFig. 2.15 Two configurations of heat pipe and chili.

results.

Bullerschen and WilhelmiS7 suggested a gravity-assisted heat pipe replace

the water circulating system used in cooling of arc furnace electrodes. Generally

in VHP furnaces cooling of graphite electrodes are essential in order to reduce the

electrode consumption. Traditionally water cooling shanks are employed for

cooling purposes. These present the danger ofvapor explosions in case of rupture.

Heat pipes are highly efficient two phase conductors which could provide a safer

alternative to water cooling shanks, since they contain only a small amount of

• CHAPTER Two 40

cooting waterinsidedouble walled top

t·····~,t~:ZW1%'j

furnace covercondensatef10wing downwardvapourflowing upward

container

- . ... "supporting arm, " ... '" '.

~111

e

er

ter

m

water inld

et~~~ W'ater out!-t

( , , , , '- ~ , " , ,i supportmg ar

b i '" ~" "... .... "'.1

i WW4?~~*?';1....... furnace cov

t'l, ~ cooling wa~ 1

I~ - inner tube•11 j-- outer tub

protection rings

graphitewearing part

protection rings

graphitewearing part

Fig. 2.16 Cooling of electrodes with water cooling and heat pipe cooling.

liquid. Besides, the operating temperature can be controlled by design parameters

such as the thermal resistance of the cooling zone.

Calculation of the maximum heat load on the pool was based on electrodes

0.508 m in diameter with a current of 50 KA (effective value) per phase.

They showed that a copper/water heat pipe can produce efficient cooling and safe

performance in a low temperature range while a steel/sodium heat pipe is suitable

for higher tempemture operation. Fig 2.16 shows arc furnace electrode cooling

• HEAT PIPE 41

with forced convection water cooling and with a heat pipe.

ChoisB innovated a technique for continuous temperature measurement of

Thermocouple wite

g11111111 131

Oeta acquisition

TundlshFig. 2.17 Measurement of steel temperature with a heat pipe-sheathedthermocouple.

liquid steel by means of a stainless steel sodium thermosyphon. The molten steel

temperatlJr.~, especially during the continuous casting operation, greatly affects the

quality of the final product. However, conventional thermocouples employed to

measure the temperature generally do not tolerate the severe corrosion around the

slag line. In bis proposed technique, a thermosyphon protects the thermocouple

wire from the harsh, corrosive region. The thermosyphon provides a colder

surface and solidifies and maintains a thin layer of slag on the thermosyphon, thus

producing a protective solid barrier against chemical attack from the slag. Fig.

2.17 illustrates the fundamentals of the technique.

Botos9 investigated a new thermosyphon lance for use with the Mitsubisbi

Process for copper production. In this process the liquid copper matte (CUzS) is

converted to blister copper by top air blowing. The conventionallance used for

blowing incurs the following problems:

• The harsh combination of bigh temperatures and chemical attack

causes continuous dissolution (consumption) of the lance tip during

• CHAPTER TWo 42

the blow.

• Since the lance material is a high chromium stainless steel, a

substantial material cost is required for replacement.

• Due to uncertainty of the positioning of the lance tip, it is almost

impossible to optimize the process.

Botos tested a stcinless steel thermosyphon injection lance of annular cross­

section. The reagent gas (air) is blown through the inner pipe to the melt while the

Reagen!gas flow

Thermosyphon lance Convenlionallance

Fig. 2.18 Thermosyphon injection lance vs. normal injection lance.

whole system is self cooled. The new system overcomes the above-mentioned

problems. It also a110ws higher efficiency due to the preheating of reagent gas.

Fig. 2.18 illustrates the cross-section of the thermosyphon injection lance in

comparison with the normal lance.

Based on the thermosyphon injection lance principles applied for smelting,

• BEAT PIPE 43

Mucciardi et alS9 designed and tested a thermosyphon exygen top blowing injection

lance for BOF steelmaking. The lance was used in laboratory-scale steelmaking

and it was observed that it could be operated without any cooling circuit. Heat

fluxes of about 1 MW/m2 at the lance tip were readily dissipated at typical

industrial rates of decarburization and oxygen utilization.

KayS2 developed a user-friendly PC-based computer model to facilitate the

design and analysis of gas-Ioaded thermosyphon injection lances. His model

employed a simple flat-front model for computation of the relevant quantities.

These quantities include temperatures, heat flows, system pressures, condenser

length and inert gas inventory.

In order to confirm the assumptions, Kay conducted a low-temperature

bench-top experiment. He concluded that the assumptions of a flat-front interface

may be used in the case when the density of the working substance vapor exceeds

that of the inert gas. AIso, experimental and computational results compared

favourably with data collected in high temperature injection lances as well as this

work (see 6.2).

CHAPTER3

METALLURGICAL ASPECTS

3.1 Introduction

Hypoeutectic aluminum-silicon casting alloys are used in many applications

because of their excellent c'lStability, good corrosion resistance, machinability,

weldability and low density. Generally, they can be produced by all major casting

processes such as:

• Sand mold ca:ting ( lower cooling rates; aùoul I°C/s),

• Permanent mold casting (medium cooling rates; about 3°C/s),

• Die casting (high cooling rates; about lOOC/s).

Certain melt treatments are often necessary in order to improve the quality

of the final product. Common treatments inc1ude 6rain refinement, modification,

and degliSsing.60

According to the Al-Si equilibrium phase diagram (Fig. 3.1), solidification

of a hypoeutectic alloy (Si < 12%) occurs by the formatiol' of a mushy zone at the

beginning of cooling, then proceeding to eutectic solidification at a constant

temperature. In this chapter the grain refinement and the modification treatments

of aluminum-silicon hypoeutectic alloys as weIl as the thermal analysis method of

controlling these treatments will be briefly reviewed.

• METALLURGICAL ASPECTS 45

1210

W.:.i.;:ht Percent Silicon, ~

• • •Alomic Percent Silicon

~II."'"

,~0 L

•~

-'10-• • •~77I1DC • ~ ........

1 (Al) " lU

(Al) + (Si)

D :<>cr•g eelkro.41Slm+ OlFra)( 14Rob93ZBro• 76tobl.

o

""

300oAI

...

Fig. 3.1 Aluminum rich part of aluminum-silicon phase diagram 1OO•

3.2 Grain Rermement

The average grain size of the casting is inversely related to the number of

nuclei (nucleation sites) that exist in the liquid. The greater the number of nuclei,

the greater the number of grains and hence the smaller the average grain size.

Once grains are large, the overall area of grain boundaries is small, thus leading

to a high concentration of impurities at the boundaries. Since smaller grains are

usually desired, it is a common practice to add some heterogeneous nuclei (grain

refiners) to the melt prior to casting. This leads to heterogenous nucleation, and,

as a result, finer grains are produced. In hypoeutectic aluminum-silicon alloys

grain refinement occurs by the formation of many primary aluminum crystals. The

main reasons for grain refining are:63

• CHAPTER THREE 46

i) to improve the mechanical properties of the cast metal and tG make

these properties uniform throughout the material.

li) to achieve a finer distribution of secondary phases thereby

improving machinllbility.

iii) te improve resistance to grain boundary corrosion.64

iv) to improve the resistance to hot cracking.

v) to improve feeding of the casting in order to minimi:Lc

shrinkage.65

Grain refinement can be done either by chemical addition or through rapid

cooling of the melt. In aluminum and its al1oys, chemical grain refinement is the

most widely used technique. It has been practiced for over fifty years, mostly by

primary aluminum producers in ingot casting. Titanium or titanium-boron mixtures

are added to liquid alufiÙnum as grain refinement reagents. They can be added via

master al10ys available as ingot, or as salt fiÙxtures.

3.2.1 Grain Reïmement Principles: It is well known that by chemical

grain refinement treatment, one promotes heterogeneous nucleation by adding a

number of solid-foreign particles into the melt. Thus, at the beginning of

solidification, a lower driving force (undercooling) for initiating solidification will

be required. Aho, since each grain is nucleated by one foreign particle, a greater

number of particles (nuclei) will yield more grains and a smaller grain size will be

obtained. On the other hand, in any metallic melt, a given solid particle may not

act as an effective nucleus. The question of what constitutes an effective nucleus

is not clearly known. However, it is believed that the interfacial energy between

the nucleant and the solidifying material bas a key role in successful grain

refinement. As shown in Fig. 3.2, a foreign particle may or may not be wetted by

the nucleating crystal, depending on the nature of the interfacial forces between

them. The relationship between the surface forces at the beginning of solidification

• METALLURGICAL ASPECTS

at the surface of a heterogeneous nucleus can be expressed as:

47

3.1

aHL

a5L

~UqUid

- ---Gfowing crystal

----;;r:

"----Heterogeneousnucleus

Fig. 3.2 Surface energy relations affecting the wetting of heterogeneous

nuclei by the Iiquid metal.

The smaller the value of e, the greater will be the tendency of the substrate

to initiate crystallization. A detailed theory of heterogeneous nucleation can be

found elsewhere.66 Fig. 3.3 illustrates nucleus-nucleant interaction in terms of

interfacialenergies. For heterogeneous nucleation, condition (c) is usually regarded

as the best scenario. Here, the nurleus enve10ps the nucleant such that it forms

a film of large radius of curvature with little distribution of energy. It has been

shown that a certain crystalline similarity between the nucleus and nucleant is

necessary to produce heterogeneous nucleation (epitaxial relation). Thus, a very

close atomic matching may occur across the interface separating the two67• It is

• CHAPTER THREE 48

usually deemed that a difference in the basic lattice unit size of the two crystal

systems should not be more than 15 to 20% for effective heterogeneous nucleation,

yet sorne particles satisfying this criterion still have no nucleating effect.67

Liquid metals with commercial qualities always contain a multitude of

foreign particles. At a given temperature below the melting (or liquidus)

Nucleant

aHigh interfacial

energy

Nucleant

bModerate interfaclal

energy

illllllmmiimmmmiiiiHiiHiiiHiHiHiHmHmmi ",,;;i

mm Nucleant mhU

1!llltmmmimii!ii!imiimiimiii!!ii!!miimm;!iiimjll~11c

Very low interfacialenergy

Fig. 3.3 The interfacial energy interaction between nucleant and nucleus.

temperature, any foreign particle may or may not be effective as a nucleant.

Particles which satisfy the heterogeneous nucleation conditions described above

will act as an effective nucleant at temperatures very close to the melting (liquidus)

point, while particles with a higher crystal mismatch will require a higher

undercooling to aet as effective nuelei. In faet, from the energy point ofview, the

magnitude of undercooling is the driving force to aetivate an existing particle to

aet as a heterogeneous nucleant. The smaller the required undereooling (driving

force) the better the potential nueleant is for the grain refinement. This deseribes

how rapid cooling causes grain refinement in addition to the ehemical grain

refinement effeet. In a very fast cooling sample, the magnitude of supereooling is

high enough to aetivate almost any existing foreign partiele to aet as a nueleation

site. Consequently, in casting methods with high eooling rates sueh as die casting,

ehemical grain refinement is usually not necessary.

Grain refinement can be affeeted by certain other minor factors sueh as

vibration, stirring, and surface roughness of the nucleant. Melt vibration yields

finer grains eompared to a no vibration situation. Also, the rougher the surface of

the nueleant (or even the mold wall) the finer the size of the grains.

• METALLURGICAL AsPECTS 49

3.2.2 Chemical Grain Refmement of AI Alloys: Several elements will

grain refine aluminum, but the MOSt effective have been found to be titanium in

about 0.15%, or titanium-boron in the range of 0.01-0.03% Ti and 0.001 % B.4

Grain refiners are added to the melt through a hardener (master) alloy. The

aluminum matrix dissolves and releases intermetallie partieles into the mf-it whieh

subsequently aet as nucleants.

Several hypotheses exist ta explain how titanium grain refines aluminum

alloYS.l01,102 According to the carbide theory TiC is the nueleant since both AI and

TiC are FCC materials whose lattice parameters differ by 6% or 7%. TiC forms

by the reaetion of titanium and residual carbon in the melt. It is also possible to

add TiC to the melt through a master alloy. There are studies showing the

existence ofepitaxy between AI and TiC, but due to the thermodynamie instability

of TiC in an aluminum melt, this theory is not supported in its original form.68

• 50

According to the phase diagram theor'y, and from the aluminum-titanium phase

diagram, titanium in solution in the liquid metal at Il concentration above 0.15%

precipitates as Al3Ti in a peritectic reaction (Fig. 3.4) according to the following:

Liquid + Al3Ti ~ a(Solid) + Q 3.2

670 Liquicl

u•!.: 665~

!

655

liquid + A13Ti

,,0;;,;'�5:.- ~~I,2~---1 665'C

"

0.5 1.0 1.5

T1tMùum,~'_'

Fig. 3.4 Aluminum rich part of the aluminum- titanium phase diagram.62

There is no doubt that Al3Ti is an active nucleus for aluminum, because

Al3Ti is found at the core of aluminum grains and a well-established orientation

relationship between the lattices of the two phases has been observed.64 A

schematic presentation of the peritectic reaction is depicted in Fig. 3.5. As seen

the aluminum grows along the surface of the Al3Ti particle that is in contact with

the solidifying melt and saon after, the solid Al3Ti will be totally cl,vered by solid

aluminum. A further thickening of the aluminum layer then occurs by diffusion

through the solid aluminum cover, which is a rather slow process (peritectic

transformation). The peritectic reaction is exothermic (Bq. 3.2) and once started

will continue spontaneously. At this stage the growth process practically stops and

the particle becomes an inactive nucleus until the bulk temperature reaches the

actual growth temperature69•

In cast shops, Ti is added through a master allo~' which contains Al3Ti

partic1es in suspension. As the master alloy disperses in the bulk melt, the Al3Ti

• METAlJ..URGICAL AsPECTS

UquidGrowth direction•

Peritectic reactionPeriteetic transformation(thickening of the ct layer

51

Fig. 3.5 Nucleatlon by the peritectlc reaction in the AI-Ti system.69

partic1es tend to dissolve and grain refining efficiency will decrease with time

(fading). Nevertheless, this pror-ess talœs in the order of one hour. This allows

ample time for the treatment and casting of the melt. A master alloy containing

many small Al3Ti particles will be a better grain refiner than one which contains

fewer, larger Al3Ti particles. This is the reason that the effectiveness of grain

refinement depends on the microstructure of the master alloy and may vary from

batch to batch and from supplier to supplier.4

The addition ofboron to the master alloy greatly increases the effectiveness

of grain refinement. It still remains unc1ear what is the process by which Al-Ti-B

grain refiners operate.68 The ternary master alloy contains relatively coarse

52CHAPTER THREE-------------------=p:lrti(;les of Al3Ti in the order of3.0 l'm and many fine T~ crystals in the order

of O.3I'm.70 It is believed that the finer T~ or (Ti,Al)Bz particles in suspension

collect around the Al3Ti particles and reduce the rate at which they dissolve.4

According to another hypothesis, nucleation may be greatIy enhanced by the action

of solutes adsorbed on the surface of the Al3Ti.4,64

Most recentIy, Mohanty et al68,71 proposed a duplex nucleation mechanism

for aluminum grain refinement. According to them, on addition of Al-Ti-B master

alloy to the melt, dispersion ofT~ and dissolution of Al3Ti occur coincidentally.

Since the level ofTi addition is below the peritcctic composition, T~ introduces

an activity gradient in the melt, and Ti segregates onto the TiB2/melt interface,

causing Al3Ti formation onT~ particles. SubsequentIy, a aluminum nucleates

at the interface by the peritectic reaction as cooling proceeds.

3.2.3 Thermal Bebaviour During Heterogeneous Nucleation: As a melt

cools to the freezing point (liquidus temperature), two processes happen

concurrentIy. Solid nucleates on the available nucleant surfaces, and when the

temperature has fallen low enough, the nucleated particles begin to grOVl and

evolve latent heat. At first, the temperature will continue to fall almost uniformly,

but as nucleation and growth aceelerate, the cooling rate decreases until the

temperature reaches a minimum and recalescence occun. Although foreign

particles are being consumed during this stage, the nucleation rate per unit area of

available substrate rises to a maximum at the minimum temperature and then falls

offvery quickly. This sequence talœs place in a short time interval, typically about

five seconds, and nucleation is almost complete just beyond the minimum

temperature. After that, the process is entirely a growth process, though there still

may he many solid foreign particles present which were not involved in the

promotion of nucleation.7o

• METALLURGICAL ASPECTS

3.3 Modification

53

According to the aluminum-silicon phase diagram (Fig. 3.1), hypoeutectic

alloys solidify over a range of temperatures. During solidification there always

exists a mushy zone in which a primary solid phase coexists wiili sorne liquid. Al

the end of the freezing process, the liquid phase surrounding the primary phase

dendrites undergoes a transformation resulting in the formation of an eutectic

silicon phase. The size and ti.e geometry of the eutectic structure is important in

determining the final mechanical properties of the casting. Coarse, long flakes of

silicon impose poor properties. Fine, fibrous shapes improve mechanical

Table 3.1 Comparison of some mechanical properties of non-modified

and modified AI-Si casting alloys8s.

YIELD • •IILLOY • STRENGTH UTS ELONGIITIONTEMPER PRODUCT TREIITMENT 10.2\1 k.si ksi 1\1

13l Si Sand Cast None -- 18.0 2Test Bars Na-modif ied 28.0 13

13\ Si IJermanent Mold None 28.0 3.6Test Bars Na-modified 32.0 8

359.0 Permanent Hold None 26.1 5.5Test Dars 0.07\ Sr 30.5 12.0

356.0-T6 Sand (".&:ft. None 30.1 41.9 2.0Test Ba.ts O. 007\ Sr 34.5 42.5 3.0

356.0-T6 Bars eut from None 30.9 41.2 4.4Chil1ed Sand Casting 0.007\ Sr 31.6 42.2 7.2

11356. a-TG Sand Cast None 26.0 40.0 4.8Test Bars 0.01\ Sr 30.0 43.0 8.0

1\444 .0-T4 Permanent Mold None 21.9 24.0Test Bars 0.007\ Sr 21.6 30.0

11413.2 Sand Cast None 16.3 19.8 1.8Test Bars 0.005 to 0.05\ Sr 15.6 23.0 8.4

11413.2 Permanent None 18.1 24.4 6.0Mold Test Bars 0.005 to 0.08\ Sr 18.1 27.7 12.0

1\413.2 Test Bar eut 0.05\ Sr 17.5 28.0 10.6from Au,te Wheel 0.06\ Sr 18.2 28.0 12.8• • Note that one kai equala 6.89xlO· Nlm'

• CHAPTER THREE 54

properties. An unmodified alloy casting contains large brittle flakes of

(eutectic)silicon and exhibits poor ductility. The unmodified alloy will typically

have a tensile elongation no more than a few percent and the fracture surface has

been observed to be largely brittle.65

The transformation of silicon morphology from acicular to fibrous is called

"modification". This transformation is responsible for the enhanced mechanical

properties associated with modified Al-Si castings. Table 3.1 compares sorne

mechanical properties of modified and unmodified Al-Si alloys.

Modification can be achieved either chemically (Le. addition of modifier

elements to the melt) or by rapid solidification (quench modification). In practice,

chemical modification is more common. Several elements are known modifiers for

aluminum-silicon alloys. These include sorne group lA, IIA, and rare earth

elements. Of these, sodium and strontium are most often used in practice. They

are effective at very low concentration levels, typically in the order of 0.007% to

0.02%.

3.3.1 The FundamentaIs of Modification: In the freezing of an Al-Si

eutectic, the silicon phase plays a critical role in modification. The aluminum solid

solution exerts only a minor influence on the process. Therefore, the solidification

of silicon will be explained in sorne detail.

Silicon crystals can grow only in a specific crystallographic direction

(faceted growth). Twins are easily formed in the crystal. Crystallization of the

silicon occurs by the addition of atoms to form steps which accumulate across the

solid-liquid interface. These steps initiate at twins, and since twin planes always

intersect the solidifying interface, a constant supply of growth sites exists at which

freezing of silicon may occur (Fig. 3.6). Studies by transmission electron

microscopy show that modified silicon fibers contain orders of magnitude more

• MEl'ALLURGICAL ASPECTS 55

twins than do unmodified silicon plates. This means that during solidification, a

large number of twins provides more sites for addition of solid silicon in different

crystallographic directions. This promotes branching. Silicon fibers contain many

crystallographic imperfections each of which is a potential site for branching to

occur. As a result, fibers in the chemically modified eutectic are able to bend,

curve and split to create a fine microstructure. 4

Growth direction

t Ste~ motion

<112>-111

(111 )

Twin lane

Freezing direction

a b

Fig. 3.6 Schematic representation of the growth of silicon;

al Directional growth of an élcicular silicon crystal from the melt,

bl Solid-Iiquid interface of a solidifying silicon crystal4 ,

In quench modification, a rapidly solidified structure appears optically

identical to a chemiC?Jly modified one. However, electron microscopy has revealed

that the silicon is similar to the unmodified forro with very low levels of twinning.

In fact, the quench modified structure is nothing oilier than a fine forro of an

unmodified eutectic. This may be the reason that chemical modifiers are more

effective at higher cooling rates.

• CHAPTER THREE 56

3.3.2. Chemical Modification of Aluminum Alloys: Several elements have

been observed to produce a modified aluminum-silicon eutectic; however, it is

believed that sodium and strontium offer the most promise for the successful

modification of aluminum silicon eutectic and hypoeutectic alloys.4.72

To study how these elements modify aluminum-silicon eutectic alloys, one

must take into account the role of phosphorus in the melt. Phosphorous is nearly

always present in non-modified commercial alloys as the compound AlP. AlP has

been observed to be an effective nucleant for silicon. Sodium and/or strontium

react with and either neutralize or remove AlP from the melt. In addition to the

successful neutralization or removal of AlP, it appears that an effective modifier

retards the growth rate of silicon crystallization in the melt. Thus, there will be

higher undercooling required for the nucleation of silicon (theoretically about

lO°C). As a result, it is seen that eutectic solidification occurs at a nearly constant

temperature about lOoC below the equilibrium eutectic temperature.72

Sodium and strontium produce equivalent modified structures when they are

used correctly. The chemical and physical properties of these modifier agents are

different and, because of this, they are added to the melt in different situations.

Sodium has low solubility in liquid aluminum, high vapour pressure and oxidizes

quickly. Because of the low solubility of sodium (about 0.01 %) the manufacture

of aluminum based master alloys is not practical. The high vapour pressure of

sodium (0.2 atm. at 730°C) causes large losses from thr. melt, and despite the

excellent dissolution characteristics of sodium, recovery of this element is poor

(20% to 30% of the addition).

Strontium on the other hand, can be added easily via master alloys and the

vaporization problem is much less severe. Higher (about 90%) and molC

reproducible recoveries are achieved. How.;ver, its dissolution characteristics are

more complex than those of sodium and its successful application requires more

• METALLURGICAL ASPECTS 57

precaution. High strontium (containing about 90% Sr) master alloys dissolve best

at low rather than high temperatures and should be added at the lowest practical

temperature. Low strontium (containing about 5% Sr) master alloys behave quite

differently. They exhibit classical dissolution behaviour such that their dissolution

improves as the temperature increases.4•73 A detailed discussion on strontium

dissolution can be found in Ref. 4.

The required amount of modifier elements depends on the alloy

composition; a higher silicon content requires more modifying agent. Typical

retained Na levels are in the range 0.005 to 0.01 %; Sr amounts of 0.02% are

sufficient to modify a 7%Si alloy, but up to 0.04% is needed to modify 12%Si

(eutectic). To evaluate the modification efficiency, it is sometimes useful to

quantify the microstructure. The structures have been divided into six classes. A

weil modified structure lies in class 5, undermodified in classes 2-4, lameilar in

class 2 and a very fine structure, called supermodified, in class 6. The latter class

is not weil understood at the present time. The vast majority of modified castings

will have structures of the 1 to 5 type. Fig 3.7 illustrates the rating system for

modified microstructures. For example, in a sample which contains 20% class 3,

50% class 4 and 30% class 5, the modification rating (M.R.) would then be

calculated as:

M.R. =(0.2x3)+(0.5 x4)+(0.3 x5)=4.l

and the sample can be said to be reasonably, but not perfectly, modified.4

On the other hand, excess modifiers in the melt can cause overmodification.

A detailed theory of modification is beyond the scope of this , .. ,:sis and only the

effect of overmodification on the microstructure will be discussed briefly.

Strontium overmodification causes coarsening ofthe silicon structure and Ieversion

of the fine fibrous form to an interconnected plate form. Also, it has been shown4

that undesirable intermetallic phases such as Al4SrSiz Can be created in an

Fig. 3.7 Microstructural rating system for modification of AI-Si alloys.4

CHAPTER THREE

Fully Unmodified Structure

Class 2. Lamellar SIruc/urs

Cfass 3. Partial Modification

Class J. Absonco of Lama/laf Structure

C/ass 5. Flbrous Silicon Eu/oCfic

Clsss 6. Very Fino SIructuro

58

/

overmodified microstructure. In terms of sodium over-modification, at

concentrations higher than 0.02%, crystals of the AlSiNa compound appear and

small sodium bubbles are sometimes found. The AlSiNa intermetallic often

nucleates silicon crystals.72

• MIITALLURGICAL ASPECfS 59

3.4 Thermal Analysis

It has always been the foundryman's goal to predict the grade of casting produced

beforc it is cast. One approach is to develop a control technique to obtzin on-line

feedback regarding the melt quality. If the quality of the melt is unacceptable, in

most cases, some liquid metal processing can be performed to restore the melt

quality before casti"g. This is accomplished through micro-processor assisted

thermal analysis of the melrs which has been called a practical technique for the

"instantaneous" quality determination at the casting station.74 Thennal analysis for

quality control was first applied to cast iron, and since the ea"ly 1980' s, it has

been accepted as a valuable tool for evaluating liquid aluminum alloys.S Since this

technique yields important information about alloy composition as well as the

microstructure which will be obtained after solidification, it is sometimes referred

to as a "non-destructive microstructure control" method.4•16

When a liquid metal solidifies, it forms a crystalline structure that has more

order and less randomness than the liquid from which it was formed. As the

crystalline structure forms, and because it is more ordered, it releases heat energy.

The quantity of energy released depends on what crystals ~re being formed, and

how much is crystallizing at that time. The amount of energy released can be

enough to totally stop the cooling of the sample, or, more commonly, slow down

the cooling rate7S•

In thermal analysis, the temperature of a solidifying sample is recorded as

• CHAPTER THREE 60

it freezes from the liquid state, through the solidification range (if any), to the

solid state. The resultant plot of temperature versus time forms the basis for

thermal analysis. The shape of this so called "cooling curve" will vary depending

on a number of important parameters such as cooling rate, chemical composition

of the melt, reactions involving evolution and adsorption of heat such as phase

transformations, and formation of intermetallics. Analysis of the cooling curve

with a standard mathematical algorithm allows one to determine a number of

useful pararneters that characterize the liquid and solid state of the material. It also

allows one to perform necessary melt treatments such as grain f<:finement or

eutectic modification. For example, in terms of chemiC':ll composition, sorne

elements like Na and P exist in ppm quantities. Chemical analysis of samples taken

from the melt are not accurate enough, although this level of concentration

produces a remarkable change in the cooling curve. In other words, cooling curves

produced by the thermal analysis technique resemble "fingerprints" of the melts

and incorporate the solidification history of the particul2.l' casting or sample.76

Fig. 3.8 shows a typical cooling curve for an Al-Si foundry alluy. As seen,

the curve is divided into three regions A, B and C. The region A indicates the

extent of grain refinement that has taken place in the melt. The existence of an

underl.Ooling in this region associates with the formation of the primary phase.

Between regions A and B, in the time interval between t1 and ~, the sample is in

the two-phase (mushy) region of the cooling curve where the .~oiid and liquid

phases cœxist. As temperature decreases, more liquid freezes and the solid phllSe

fraction increases. At time ~, the liquid phase surrounding the solid dendritic

network is enriched in composition by nearly all of the Si (solute element) and

undergoes an eutectic transformation such that the liquid phase transforms to two

soUd phases at a constant temperature.The eutectic transformation, then, occurs

between the time period ~ to t3• The eutectic region of the cooling curve indicates

• METALLURGICAL ASPECTS 61

the extent of modification (see 3.4.2). In the region C, solidification is cOl~plete.

However, when appreciable amounts of impurities are aIso present, the formation

of other phases such as MgzSi after point C llIe observed.

Major phase changes are usually obvious on the cooling curve (e.g. points

~Tc

-/ \<::: TuA

tl t2Time

t3

Fig. 3.8 A typical cooling curve of an off-eutectic AI-Si alloy.es

A, B and C in Fig. 3.8), but depending on the composition, some of the other

minor reactions may be scarcely detectable. In order to reveal the exact

temperatures at which such reactions occur, it is usually necessary to employ the

fust derivative curves in which the cooling curve slope (dT/dt) is plotted versus

time. The main benefit of the derivative curves lies in their ability to magnify the

important slope changes w!Uch are found on the cooling curve.4,7.6S.77 Fig. 3.9

shows the cooling curv,~ and the fust derivative curve for a typical Al-Si 356 alloy.

• CHAPTER THREE 62

In aluminum silicon casting alloys, the thermal analysis technique is

primarily used to control grain size and the degree of eutectic modifica­tion.4•5•6,65.74,76,77.78,79

3.4.1 Thermal Analysis Control of Grain Size: Thermal analysis can he

utilized to evaluate the level of grain refinement in Al-Si casting alloys. Once grain

650 0.2

1 0.1

" 12

" 3600 " 0

t.ldT/dt

0 -0.1

Pai:;1ü 550 -0.2 .;Q; "0Q, j::'E -0.3 "0Q)....

soo -0.4

-0.5

4500

-0.6200 400 600 800 1000 1200 1400 1600

T\me, sec.

Fig. 3.9 Typical cooling curve and its first derivative of a 356 alloy at

approximately O.soC/s. 1) Primary AI phase nucleation; 2) AI-Si eutectic

reaction; 3) Minor intermetallic formation reaction (e.g. M92Si).7

refi'lement treatment is applied (by any means), it affects the ~hape of the cooling

curve at the very beginning ofliquidus solidification. In a weil (chemically) refined

alloy, for example, with a sufficient number of effective nuclei, nucleation will

occur in a shorter time, and a supercooling as 10w as O.3°C is sufficient to start

primary soli~fication. This indicates that there is almost no energy barrier for

nucleation and that the grain size of the casting will be fine. This is illustrated in

curve 1 in Fig. 3.10. If the melt is not grain refined or partially refined, a greater

driving force in the form of undercooling will be necessary to start solidification

• METALLURGICAL ASPECTS 63

of the primary grains. Once nucleation is complete evolution of latent heat tends

to decrease the undercooling and recaIescence occurs. Eventua1ly, the cooling

curve will follow a sinusoida;. arrest pattern and resemble curve 2 in Fig 3.10. In

this figure, the larger the amount of dT (apparent supercooling), the larger the

sizes of the grains and the less the grain refinement. The apparent supercooling,

TO; T~rlH-~":r'"

; T1H-4'"a.E ATt!!

tl

Curvel: a grain refined alloy

Curve 2: an unrefined alloy

Ta = temperature at star! of freezlng of a well-refined alloy;

Tl=temperature at star! of freezlng of an unrefined alloy;

tl=perlod of apparent supercoollng

T2=recalescence temperature

g=T2-T1: the apparent supereoo11ng

tl=perlod of apparent supereoollng

tlme

Fig. 3.10 The cooling curve at the beginning of solidification80;

curve 1: a grain refined aUoy;

curve 2: an unrefined aUoy.

then, is defined as the differentiaI between the minimum temperature relating to

the beginning of solidification and the maximum temperature reached by the a1loy

during solidification (recalescence temperature). This apparent supercooling, dT,

is aIso shown in Fig. 3.10.

The period of apparent supercooling gives another effect on the solidificntion curve

relative to grain size. At larger grain sizes, the undercooling lalols for an extended

period of time because of the time factor required for nucleation menticmed il1

3.2.1. Tnis period (tl on Fig. 3.10) is characterized by the elapsed lime between

• CHAPTER. THREE 64

the moment solidification begins at temperature Tl, and the time at which the

recalescence temperature, T2 is attained. The question of whether the above

temperature difference or the time difference is the preferred parameter in

assessing grain refinement is somewhat controversial. Sorne alloys exhibit a better

correlation between grain size and arrest time. Others (most likely casting alloys)

exhibit a good correlation between the arrest temperature and grain size. It has

been observed that for wrought aluminum alloys, in the cases that the liquidus

temperature lies below 610°C (1200°F) the apparent supercooling can be used for

grain size evaluation, whereas in cases with the liquidus temperature greater than

610°C, a horizontal arrest occurs, and the time difference can be used for grain

refinement evaluation74• In aluminum casting alloys both the value of apparent

supercooling and period of supercooling are suggested for the best estimation of

grain size, but because of the simplicity in the measurement of supercooling over

the complex and time consuming time difference method, the temperature

difference method is routinely used.78

3.4.2 Thermal Analysis Control of Eutectic Modification: In aluminum­

silicon hypoeutectic alloys, modification treatment targets the eutectic and solidull

parts ofthe cooling curve. Therefore, the thermal analysis technique can determin,~

the degree of modification. The cooling curve of a modified alloy has the

following characteristics when compared to one of an unmodified alloy4:

i) The temperature of the eutectic plateau is depressed.

li) The duration of the eutectic plateau is increased.S

iii) The required supercooling to start eutectic freezing is increased.

iv) The duration of the supercooling is enlarged.

These effects are depicted in Fig. 3.11.

Among the above mentioned features, the deprp.ssion ofeutectic temperature

• METALLURGICAL ASPECTS 65

at a certain cooling rate is most often used in thermal analysis control of

modification. 4,7,76,78 The lower the eutectic temperature, the greater the

modification and the finer the silicon eutectic structure.

ln an unmodified hypoeutectic aluminum-silicon alloy of high purity, the

eutectic temperature is 577°C +0.381 and an eutectic temperature arrest depression

of about 10°C by modification has been observed.65 ln commercial alloys, the

Unmodified

Modifled

Time

...........\

.......

ÂT-_._._ .._-_.~-l1

Fig. 3.11 A comparison of the eutectic regions of the cooling curves ofmodified and unmodified alloys5.

minor presence of other elements such as Mg, Mn, Fe, Cu and Ni tends to lower

the eutectic temperature from 577°C. Thus, depending on the amount and nature

of impurities, a lower eutectic temperature depression is expected by modification

treatment.

Modification can be controlled using more sophisticated approaches. For

example, since the greatest temperature depression happens in the unmodified to

• CHAPIER 1HREE 66

modified transition, it is not very easy to detect overmodification by using the

temperature alone. It has been observed4•6 that with modification, the undercooling,

âeE, increases and then falls as the structure tums overmodified. Also, the values

of âT are typically only a few degrees and probably lie within the accuracy of

commercial thermocouples. Therefore, incorporation of the above four effects

(particularly items i, iii and iv) leads to more information and helps correct errors

that might have been made by considering only the eutectic temperature.4•7S Fig.

3.12 shows the effects of items i, iii and iv on modification evaluation for an Al-Si

356 alloy.

Temperature 01 eutectlc plateau

/Apparent supercoollng

/'--:-----

1Fig. 3.12 Relationship between eutectic structure and eutectic temperature,

apparent eutectic supercooling and period of supercooling.4.78

Also, Tenekedjiev and Gruzleski5 investigated time and temperature change effects

on the eutectic region of the cooling curve by modification on several Al-Si alloys

at different cooling rates. They used strontium as the modifier agent and observed;

• METALLURGICAL ASPECTS 67

.Depression of the nucleation temperature and the eutectic growth

temperature.

• Greater value of Â6E with the presence of modifiers .

• Considerable enlargement of the eutectic reaction.

They concluded that at low cooling rates (about 1°C/sec), with the

exception of 413 alloy, a time difference parameter was also sensitive to strontium

treatment. The main advll:1tage of using a time difference parameter was that it

was thennocouple independent and easier to measure than was temperature. They

also found that the primary arrest was not affected by strontium. Therefore, it

would not interfere with the ability of thermal analysis to assess grain refinement.

3.4.3 Thermal Analysis Equipment: Thennal analysis is relatively simple

and inexpensive to perfonn. It is carried out by pouring a relatively smallliquid

sample of the melt into a sampling cup. The liquid metal is then allowed to

solidify. The temperature of the solidifying sample is recorded as it cools through

the solidification range, and eventually the cooling curve is drawn. The equipment

that is required includes a sampling cup and a thermocouple, and may also include

a PC-based Data Acquisition System for data logging and analysis as well as an

appropriate software package. The thennocouple is placed in the centre of the cup

(or in sorne cases two thennocouples are used; one fixed at the centre; and the

other on the cup wall to detect any changes of cooling rates). The physical and

thennal characteristics of the sampling cup in any one given test determine the

effective cooling rate. Control of the cooling rate is a very important issue in

conventional thennal analysis and it is difficult to control in tenns of

reproducibility. For example, Tenekedjiev and Gruzleskis used a fire clay cup pre­

heated to 400°C and encased in a fiberfrax insulation box to achieve equilibrium

(very slow) cooling conditions. They used the Sllll!"~ arrangement to simulate sand

• CHAPTER DmEE

Centrethermocouple

Wallthermocouple

$30mm

68

Thermocouple

L.=:==--1~~ ToMicroprocessor

Fig. 3.13 Two typical sampling cups used for thermal analysis.

casting except that the cup was maintained at room temperature. Finally, a faster

cooled sample was obtained by using a steel cup pre-heated to 300°C. Fig. 3.13

illustrates two typical sampling cups used for thermal analysis.

Experience has shown that, in thermal analysis, a low pouring temperature,

poor contact between the melt and the thermocouple resulting from, for example,

vibration, and rapid freezing can give incorrect results.74

In practice, this classical thermal analysis technique also has the following

limitations:

• Il is a batch method.

• The cooling rate is not readily changeable.

• MEfALLURGICAL ASPECTS 69

With this method, the choke of cooling rate norrnJ1ly involves the selection of a

suitable sampling cup to produce the desired cooling rate. Thus, to be able to

simulate a range of cooling rates, one requires a variety of cups. In other words.

it is not practical to simulate different types of casting methods with a givcn cup.

• It is i!!!possible to automate and computerize the entire analysis process .

CHAPTER4

THE HEAT PIPE PROBE

4.1 Introduction

The primary objective of this doctorate research work is to develop a heat

pipe probe for conductint, thermal analysis of aluminum and aluminum casting

al1oys. This new probe for conducting thermal analysis will make the process

semi-continuous rather than batch as is currently available with the conventional

method. AIso, the cooling rate will be readily changeable over a wide range for

the same sample. The evaporator of the probe which is agas loaded annular

thermosyphon, resides in a large bath of liquid metal and does not need to he

withdrawn as it solidifies a smal1 sample (Le. button) at a predetermined cooling

rate. Once the instantaneous rates of cooling have been obtained, the probe can be

instructed to remelt the frozen button and await instruction for analyzing a fresh

sample. In this chapter the probe specifications and design will be presented in

detail.

4.2 Cbaracteristics of the Probe

• THE HEAT PIPE PROBE 71

Accorciing to the defined task for the probe (see 4.1) the basic

characteristics are defined regarding the following:

1) The positioning of the probe.

2) Flexibility to alter the rate of heat dissipation [Tom high rates to almost

zero (tumed off).

3) The ability to take a proper sample from the liquid metal.

The probe should be used vertically since one end will stay in the liquid

metal to take the sample while the other end must be in the ambient environmenl

to dissipate the heat extracted from :he sample. Therefore, to satisfy the above

condition and because ofthe higherefficiency and structural simplicity (see 2.4.1),

a gravity-assisted heat pipe (thermosyphon) is to be used. To satisfy the second

criterion a gas loaded thermosyphon with variable inert gas pressure can be

employed in which the heat transfer rate is readily changeable over a wide range

ià!

J1

IlSIIf4lllng Roglan

Fig. 4.1 The basic appearance of the thermosyphon probe.

(see Fig. 2.5). Finally, a concentric annular shape ofthermosyphon (Fig. 2.3) was

found necessary to have a proper sampling region in addition to its higher heat

• CHAYfER FOUR 72

dissipation efficiency. The sampling region is, in effect, about 0.1 m long inside

the smal1er diameter pipe at the bottom end of the probe. It resides in the Iiqnid

metal bath and forms the evaporator of the thermosyphon. Therefore, a gas-loaded

annular thermosyphon (with a changeable inert gas pressure) has to he designed

for this new method of thermal analysis. Fig. 4.1 presents a sl:hematic of the:: cross

section of the probe basic sections.

4.3 Probe Design

Genera1ly, a heat pipe for a special application is designed with respect to

sorne key criteria such as:

• The expected task of the heat pipe for a given application (as determined

in 4.2).

• The optimum size of the heat pipe.

• The temperature r&l1ge that the heat pipe is supposed to work in.

• The environments to which the heat pipe is exposed, including the

environments both at the evaporator and condenser (heat source and heat

sink) and the internal environment (inside the pipe).

The physica1 size must he determined with respect to the particular

application. Here, the proper size of the sampling region is the starting point. The

sampling region that is a cylindrical shaped bar must have a volume that is

representative of the whole batch of liquid metal. Therefore, the diameter of the

inner pipe is equal to the minimum acceptable diameter of the sample. The outer

pipe diameter is then determined by considering the behaviour of the working

substance inside the thermosyphon. The regular cycling (vaporizationl

condensation) of an annular thermosyphon occurs in the space between the two

concentric pipes. This space must be large enough to reduce high shear stresses

• THE BEAT PIPE PROBE 73

at the liquid/vapor interface to the point that the entrainment limil (see 2.5.3) is

not exceeded. Since the inner pipe diameter is already fixed by the sampling

region, the outer pipe diameter is to be determined in this regard.

In terms of pipe thicknesses, since heat is conducted from the hot medium

into the thermosyphon through the eV<lporator wall, a thinner pipe ttansfers heat

at a higher rate. However, for reasons of safety and to exlend the life span of the

probe, one can decide on a minimum thickness that satisfies safety and endurance

criteria. Finally, the thermosyphon probe should be long enough 10 provide

sufficient space for the dissipation of heat by the vapor. In addition, one must

factor in the maximum length of the inert gas section when the probe is operating

at the highest heat extraction rate.

4.3.2 MateriaIs Selection: Following the design criteria mentioned in 4.2,

the materials for a given application are generally selected with respect 10

operating temperature anù the nature of the environments (internal and external)

of the thermosyphon probe. AIso, in any particular application other conditions

must be satisfied. In the present work, materials for the working substance, inert

gas, and container must be selected.

4.3.2.1 Working substance selection- As was mentioned in section 2.6.1,

Fig. 2.11 can be used for selection of the working substance on the basis of the

operation temperature range. As the probe is to be used in the thermal analysis of

aluminum and aluminum-silicon hypoeutectic alloys, the temperature range can be

deterrnined as follows. From the AI-Si phase diagram (Fig. 3.1), it is seen that in

aluminum with the silicon content in the range of 0-12%, the maximum melting

temperature is that of pure aluminum with a melting point of 660oe. In practice,

however, the melt is poured with a superheat of as much as lOOoe. Therefore, the

upper limit of the operating temperature lies at about 760oe. On the other hand,

• CHAPTER FOUR 74

for the thermal analysis method, once solidification of the sample is complete and

the sample temperature drops to a level below the solidus, the thermal analysis

procedure is complete. Again, according to the AI-Si phase diligram, the lowest

temperature in the hypoeutectic range is the eutectic point of 577°C. Taking into

account sorne undercooling from the eutectic point, it was decided that 550°C

would constitute the lower temperature boundary. Consequently, the temperature

range for this application is bounded between 760 and 550°C. Referring to Fig.

2.11, it is seen that both potassium and cesium can be used effectively in this

temperature range. Nevertheless, another restriction has to now be considered. The

corresponding pressures for the temperature ranges presented in Fig. 2.11 vary

from 6900 to 690000 N/m2 C 0.07 to 7 atm.).IS For reasons related to safety, the

choice between potassium and cesium requires that the preference be the substance

not exceeding 1 atm. of pressure at the maximum operating (liquid metal bath)

temperature. In other words, to prevent any kind ofexplosion danger, the pressure

inside the container must not exceed 100000 N/m2 Cl atm.) under any

circumstances. This shortens the alIowable temperature range. Thus, the decision

was made to use potassium in the thermosyphon probe used in the higher

temperature range as it is necessary to analyze liquid pure aluminum, and cesium

in the lower temperature range for analyzing hypoeutectic and eutectic aluminum

alIoys. The properties of potassium and cesium are listed in tables 4.1 and 4.2.

The temperature/pressure relationship for saturated vapors of the above materials

can be represented as:

4.1

•where a and b are constants given in Table 4.1 for a specifie vapor, Tv is in K and

Py is in N/m2•

• THE BEAT PIPE PROBE 75

Table 4.1 Constants in the pressure-temperature equation for saturated vapor. 15

Vapor a b

Potassium 9.1542 4282

Cesium 8.9333 3711

As an unsuccessful experience, sulfur initially was chosen as the working

substance material. According to the literature sulfur has been successfully used

in heat pipeS.34 However, some ofits properties, and in particular its viscosity, are

extremely temperature sensitive. At 159°C liquid sulfur suddenly changes into a

very viscous material82•84

•87 that can cause difficulties in the normal circulation of

the working substance. AIso, the vapor pressure of sulfur in the operating

temperature range was found to be tao high. In order to improve on these

deficiencies and because of the inherent similarity in the behavior and position of

selenium in the periodic table relative to sulfu~·85.86, selenium was chosen to be

added to sulfur. Preliminary tests showed that an alloy of SO%S-50%Se would

lower the total vapor pressure and improve the viscosity in the operating

temperature range. AIso it has been observed34 that an addition of 5-10% iodine

would dramatically reduce the sulfur viscosity. Therefore, a compound of S­

SO%Se containing 5 % iodine was finally chosen and charged in the thermosyphon.

After a short period, the thermosyphon stopped working and a build up of solid

material on the condenser wall was observed (bridging).

The possible drawbacks making this material unsuitable for the application

are as follows:

i) X-ray analysis of the solid material taken from the thermosyphon showed

that the solid compound had an amorphous structure that would make it impossible

to deduce its composition from the formation temperature.

• CHAPTER FOUR 76

Table 4.2 Selected properties of potassium and cesium as heat pipe working

fluidsl~.

Temp.

(K)

Vapordensity(kg/m3)

Liquid

kinematicviscosity(m2/s)x1~

Surfacetension(N/m) x 10.1

Latentheat(JIkg)X107

Liquidtransport factor(W/m~x1012

Potassium

880 0.1086 0.2197 0.7319 0.2006 0.6688890 0.1217 0.218G 0.7253 0.1999 0.6648900 0.1360 0.2165 0.7187 0.1994 0.6619910 0.1516 0.2149 0.7121 0.1989 0.6588920 0.1686 0.2134 0.7055 0.1984 0.6556930 0.1871 0.2120 0.6989 0.1978 0.6522940 0.2071 0.273 0.6923 0.1973 0.6487950 0.2288 0.2092 0.6857 0.1968 0.6450960 0.2522 0.2079 0.6791 0.1963 0.6412970 0.2775 0.2066 0.6725 0.1958 0.6373980 0.3048 0.2053 0.6659 0.1953 0.6333990 0.3341 0.2041 0.6593 0.1948 0.62921000 0.3656 0.2029 0.6527 0.1943 0.6250

Cesium

770 0.2924 0.1332 0.5201 0.05134 0.2004780 0.3224 0.1320 0.5150 0.05121 0.1998790 0.3766 0.1308 0.5099 0.05109 0.1991800 0.4253 0.1297 0.5047 0.05096 0.1983810 0.4788 0.1286 0.4995 0.05086 0.1974820 0.5375 0.1276 0.4943 0.05071 0.1964830 0.6016 0.1266 0.4891 0.05058 0.1954840 0.6716 0.1257 0.4838 0.05045 0.1942850 0.7477 0.1248 0.4785 0.05032 0.1929860 0.8305 0.1240 0.4732 0.05019 0.1916870 0.9203 0.1231 0.4678 0.05006 0.1902880 0.101801 0.1224 0.4624 0.04993 0.1887890 0.1123D1 0.1217 0.4570 0.04979 0.1871900 0.123601 0.1210 0.4516 0.04966 0.1854• 910 0.135801 0.1203 0.4462 0.04953 0.1837

• THE BEAT PIPE PROBE 77

ü) The condenser temperature was too cold so that the condensed vapors on

the condeœcr wall became so cold that the liquid could not easily flow down 10

the evaporator.

ili) Due to instability of the compound at high temperatures, the composition

of fluid inventory in the evaporator would keep changing which could cause

uncertainty in the vapor pressure at the same temperature.

4.3.2.2 Inert gas selectiun-During normal operation of the thermosyphon

(Fig. 2.5 band c) inert gas and working substance vapor are separated from each

other by the convective forces of the vaporizing working substance. In other

words, the inert gas is separated and pushed up to the top of the thermosyphon by

the high velœity of the vapor (flat front). However, since the vapor velocity

decelerates from the evaporator to the vapor/gas interface, sorne inter-diffusion of

inert gas and working substance vapor is expected. On the other hand, the nature

of vapor and gas in terms of their densities has a key role on the desired separation

of gas and vapor. In fact, the gravitational body force that acts on both vapor and

gas can remarkably affect the flatness of the vapor/gas separation. If the inert gas

has a higher density than the working substance vapor, the front would not remain

flat. As gas and vapor tend to mix, sorne of the lighter vapor molecules would

move up to the inert gas section and condense there while sorne of the hcavier

molecules of the inert gas are pulled down to the bottom part of the thermosyphon.

As a result, there will he an accumulation of solidified working substance material

in the top section of the thermosyphon (Le. in those cases where working

substance is in the solid state at the temperature of the inert gas section).

Eventually, such a condition will cause the evaporator section to dry-out. If the

vapor density is higher than the inert gas density, the role of the gravitational body

force becomes less significant and a sharp vapor/gas interface (flat front) is

expected. Since the working substance selection is done according to other factors

• CHAPTER FOUR 78

prior to inert gas selection, one can recommend the use of heliurn iner. gas if a fiat

front is to be maintained.

4.3.2.3 Container material selection-In most cases, the choice of heat pipe

container is controlled by the environment in which the heat pipe will have to

operate53 • The general design criteria for the container material selecûon were

stated in 2.6.2. In terms of compatibility between the working substance material

and the envelope, it is reported that for potassium, stainless steel is the most

compatible material. 1&,\5,34,53,88 For the cesium case, bath titanium and stainless steel

are compatible. 15•53 011 the other hand, since the evaporator of the thcrmosyphon

probe is immersed and kept inside liquid aluminum and its alloys, this part of the

probe must either be neutral to the liquid metal or protected against liquid metal

attack. ln terms of compatibility of the probe container with the liquid metal, it

was observed that both titanium and stainless steel were dissolved in liquid

aluminum-silicon alloy to sorne extent. However, stainless steel was attacked less.

This shows that it is necessary to protect the evaporator surface against the molten

metal attack. Finally, f:-r the container, th:l optimum choices were found to be

potassium/stainless steel and cesiumfstainless steel.

In terros of evaporator linings, two aspects that are to be considered are as

follows:

i) The whole surface of the evaporator must be coated such that a natural

layer separates the stainless steel container from the hquid metal.

ü) The outer surface and the bottom of the evaporator must allow for what

is deemed to be adequate heat transfer from the liquid metal to the thermosyphon

probe. Therefore, when the probe is used in the solidification mode (Fig. 2.5 b

and c) heat will be mostly extracted from the sampling region, whereas in the

remelting mode (Fig. 2.5 a) conductance from the outer side through the working

substance and to the solidified sample will help the solidified sample to remelt

• THE HEAT PIPE PROBE 79

along with heat from the hot liquid bath.

Regardi!\g the first condition, boron nitride in suspension was brushed on

the surfaces chosen to be protected. Boron nitrid.: is an inexpensive coating

mat~rial widei:! used in aiuminum casting shops. Ii sticks firmly to stainless steel

and is nO( wettr.d by liquid aluminum.

Concerning item ii, a graphite block with wall thickness of about 0.01 fi

that covered the bottom and the outer surface of the evaporator was chosen to be

used. Fig 4.2 shows the evaporator of the designed thermosyphon probe.

Fig. 4.2 The cross section of the evaporator elements .

CHAPTER5

EXPERIMENTAL

5.1 introduction

As described in Chapter Four, a novel probe based on heat pipe principles

was designed for controlling the quality of aluminum casting alloys. The probe

was, in effect, a "gas-Ioaded, concentric, two phase closed thermosyphon" and

consisted of three main zones: the evaporator, the condenser and the inert gas

section. The rationale was to replace the conventional thermal analysis set-up with

the new probe in order to develop an alternative thermal analysis method especially

suitable for aluminum casting alloys.

This chapter describes sorne details of the experimental set-up including the

probe elements, sensors and peripheral equipment as weIl as the experimental

procedure.

5.2 Experimental Set-up

S.~.l Probe Elements: The three basic components of the probe were: the

container, the working substance and the linings. The container consisted of a pipt;

• EXPERIMENTAL 81

within a pipe (annulus) with plates welded at the ends to form a closed section.

There were also IWo access ports on the upper part of the outer pipe that provided

acccss to the inside of the probe. One was used to house a thermocouple which

lesided in the probe and was used to check the temperature behaviour of the

working substance during operation, and the other branch was used to make

pressure adjustments and was connected to a low pressure and a high pressure

reservoir. This branch was also used to house the pressure sensor.

Il will be recalled that material selection for the contai ner was discussed in

section 4.3.2.3, and that 304 stainless steel was found to be the optimum material

Inner pipe - 304 ss

21mm 0.d.x17mm Ld.

Outer pipe - 304 ss

60mm o.d. x55mm Ld.

Fig. 5.1 Dimensions and materials of the laboratoryscale thermosyphon probe container.

tested. The lance was machined and welded. The welding of the lance was an

important task and had to be done properly. Great care was taken to ensure that

the welds were both strong, and leak praof, and that the container could maintain

vacuum indefinitely.9 Il was also important to use valves and fittings on the

• CHAPTER FIVE 82

branches that ensure good sealing in a rather hot environrnent. Fig. 5.1 shows

schematically the laboratory scale model of the designed probe container.

Selection of the working substance material was explained in section

4.3.2.1. Potassium and cesium were selected for this application. The potassium

thennosyphon was used in higher temperature applications while the cesium one

was used in lower liquid metal bath temperatures. The practical problem associated

with these two alkaline metals was charging them into the annular probe.

Potassium is a very reactive element which has a high affinity for oxygen. In the

liquid state, it will ignite when in contact with oxygen, and explode if contacted

by water because of the generation of hydrogen gas. Botos9 experimented with a

number of methods for charging sodium, a material which behaves very much like

potassium, into the heat pipe. He found that the simplest and safest way to charge

sodium was in solid fonn. In his proposed method, sodium was cut into pieces in

an inert atmosphere (e.g. under a positive pressure of argon) where the sodium

could be manipulated. Under the same controiled environment, the sodium was

charged into the feed tube (one of the above mentioned branches) of the heat pipe.

Once the pipe was filled, it was closed by using the proper fittings and valves. The

heat pipe then was evacuated to remove any air and moisture in order to prevent

oxidation.

Because of the inherent similarity in the behaviour of sodium relative to

potassium, the above filling method was foilowed to charge potassium to the

probe. However, in the cesium case, this method was not found to be practical.

Cesium has a melting point of28°C whereas the melting point of potassium

is 6ZOC. Titus, it is difficult to have cesium in the solid state at room !emperature.

In addition, cesium is remarkably more reactive than potassium with oxygen and

any kind of moisture. Therefore, the filling has to be perfonned in a very weil

controiled atmosphere.

• EXPERIMENTAL 83

Cesium is usuaIly kept in sealed glass ampoules. A glove-box must be used

to successfuIly transfer the cesium into the annulus. A glove box is a sealed

chamber that has an inlet and outlet of inert gas. Any kind of manipulation inside

the box is done by gloves which are located inside the box and sealed from the

environment. The probe, a cesium ampoule, and an electric dryer were put inside

the glove box and the box was closed. Then, an inert gas inlet was opened to flush

out oxygen and moisture from the chamber. Once the inside atmosphere was

completely inert and while the inert gas was flowing into and out of the chamber,

the dryer was used to melt down cesium material inside the ampoule. When the

temperature of the liquid cesium was weil above the melting point, the ampoule

was broken and the liquid cesium was poured through one of the branches into the

annulus. The annulus, then, was closed by using fittings and valves and

pressurized by an inert gas. Once the annulus was sealed, the probe was removed

from the box and the filling process was complete.

5.2.2 Sensors: Two kinds of sensors were needed for the set-up; one was a

temperature sensor (thermocouple) and the other was a pressure sellsor (pressure

transducer) .

Thermocouples come in a wide varlety of sizes and shapes. A K type­

stainless steel sheathed thermocouple (Chromel-Alumel junction) with an outer

diameter of about O.OO6m was chosen for this application.

Two thermocouples were used in the experimental set-up. One was installed

inside the thermosyphon probe and sea1ed from the environment by means of a

compression fitting. This thermocouple measured the working substance

temperature during operation. The other one was passed ail the way through the

inner pipe such that its tip was located in the centre of the sampling region. It was

with this thermocouple that the thermal behaviour of the sample during each

experiment was controlled and the cooling curve was produced.

A pressure transducer was connected to the system that measured the

chamber pressure. Pressure transducers employa strain gauge situated in front of

a pressure sensitive diaphragm. When the diaphragm is compressed by a pressure

change, it changes the resistance in the Wheatstone bridge arrangement within the

strain gauge. The pressure transducer was connected to a power supply and aJong

with the thermocouples to a data acquisition system. The readings from the

pr~ssure transducer were calibrated according to a simple equation in the data

acquisition system.

• CHAPTER FIVE 84

5.2.3 Peripheral Equipment:ln the routine operation of a laboratory scale

thermosyphon probe, a number of pieces of peripheral equipment must also be

Fig. 5.2 The probe positioning inside the Iiquid metal bath.

• EXPERIMENTAL 85

'ISOO. A holder was necessary to maintain the evaporator of the probe insidc the

liquid metal bath. The holder must be able to move the probe up and down in

order to position the probe at the right location in the liquid metal bath. Fig. 5.2

shows the probe held in position. The pressure inside the probe was adjusted by

means of a vacuum pump, a vacuum stabilizer tank, and a high pressure inert gas

tank. The vacuum pump pro",.idOO the desirOO vacuum to the stabilizer tank and the

probe chamber, once the probe was in solidification mode. Also, the vacuum

_---?G)~1~ ---, CD ThermocoUlJlelnside the pipe

CV ®Thermocouplelnslde thellquid AI

CD Pressure lransduc...•NcrrlUSCALt

Condonsor..~e"~ EYaporaoroC

~

Fig. 5.3 The experimental set-up.

stabilizer provided a larger evacuated volume connectOO to the probe so that small

changes of pressure during vaporization/condensation did not effectively change

the vacuum inside the probe while in solidification mode. Thus, a relatively

constant heat transfer rute across the wal1s of the thermosyphon necessary for the

sake of reproducibility of the cooling curves was ensurOO. The high pressure tank

was equipped with a pressure regulator to al10w adjustment for the inert gas

CHAPTER FIVE

pressure in the chamber at a maximum of one atmosphere. Fig. 5.3 depicts a

schematic of the experimental set-up.

In terms of data logging, a data acquisition card instal1ed in a PC along with

propcr software was employed. Raw data signais in the form of millivolts were

delivered to the data acquisition system from the thermocouples and the pressure

transducer. In the thermocouple case, the compensation voltage was added to the

raw signais, and eventual1y the real temperature was calculated. In the case of

pressure signais, the correlation between voltage and pressure, whieh had already

been introduced to the system, was applied and the pressure in atmospheres was

calculated. These data were managed simultaneously in three ways during the test.

First they were stored in the computer memory for further investigation. Secondly

they could be displayed as transient curves and, final1y they might be displayed as

numbers on the screen.

Fig. 5.4 The data acquisition monitor during a routine test.

• EXPERIMENTAL 87

Fig. 5,4 shows the monitor of the data acquisition system during a test. As

seen, the ongoing cooling curve plus simultaneous working substance temperature

and pressure readings are displayed.

The liquid metal was prepared in an electric resistance fumace. The ladle

capacity was about 10 kg of which about 0.3% fills the sampling region. The

fumace was equipped with an electric temperal.ure on/off controller to keep the

liquid metal bath temperature (relatively) constant during operation.

5.3 Experimental Procedure

The experimental procedure was divided into Iwo periods; the cooling or

solidification period and the heating or remelting period. However, since this was

a liquid metal thermosyphon for use at relatively high temperatures, there was a

start-up procedure from the frozen state.

At room temperature, the working substance was in the solid state, whereas

during the routine operation of the probe it existed as liquid and vapour phases.

According to the literature89•90 the heat must he loaded to the evaporator graduaIly.

Also, a small amount of heat input at the condenser and low heat rejection from

the condenser helps start-up.

In the frozen state, the probe was kept in an inert gas atmosphere Le. the

probe was evacuated and the chamber filled with an inert gas. When the liquid

metal was ready, the probe was held above the liquid bath to be preheated. Then,

it was lowered down gradually into the liquid metal. This caused the liquid metal

bath temperature to decrease. Since the pressure of the inert gas inside the probe

was kept at one atmosphere, there was aImost no heat dissipation by the probe

during the start-up process. The probe was ready for the experiment when the

liquid bath temperature increased to the set temperature on the fumace controller

• CHAPTERFNE

and the evaporator core was thennally equilibrated with the melt.

88

5.3.1 Cooling (Solidification): A thennal analysis test was started with the

probe in the pressurized state (Fig. 2.5a). A vacuum pump was used to evacuate

inert gas from the probe through the pressure stabilizer tank. Depending on the

desired cooling rate for the sample, the appropriate pressure of inert gas was left

in the probe. For instance, if a high cooling rate was required, the vacuum pump

was allowed to evacuate the probe until the inside pressure dropped down to a

certain pressure (vacuum), depending on the nature of the working substance. In

this case, the working substance experienced a greater evaporation rate which

resulted in the activation of a longer length of condenser (Fig. 2.5c). Since the

temperature and pressure of the working substance were correlated by the

Clausius-Clapeyron equation (Bq. 4.1), it followed that an increase in the heat flux

extracted by the evaporator section was the result of a lower pressure setting.

Conversely, when a higher pressure was applied to the probe's chamber, less

evaporation occurred and a shorter condenser length was used to reject heat from

the system (Fig. 2.5b). Consequently, by having an inert gas lmd a vacuum pump

hooked up to the system, a wide range of cooling rates could be achieved.

5.3.2 Heating (Remelting): Once the sample temperature reached the

desired temperature and solidification of the button-shaped sample was complete,

the resultant cooling curve was drawn, and the probe was instructed to remelt the

unseen sample. In this case, the valve connecting the probe to the pressure

stabilizer was closed and the probe was connected to the inert gas tank. The outlet

of the pressure regulator on the gas tank was set to one atmosphere to fil1 the

evacuated probe to about one atmosphere. The inert gas then impeded the

movement of the working substance vapour to the portion of the condenser that it

• EXPERIMENTAL 89

occupied and acted as a diffusion barrier to the flowing vapeur. The active length

of the condenser was reduced to the working substance pool level in the

evaporator, and heat transfer from the probe was blocked (Fig. 2.5a). At this point

the solidified button gained energy from the hot liquid bath directly and also

through the graphite block covering the outer evaporator surface. Eventually, the

sample was remelted and the probe was ready for the next thermal analysis test.

cllAP'J'}3ltfi

MODELLING HEAT TRANSFER

6.1 Introduction

In order to better understand both the regular operation of the heat pipe and

the freezing of the solidifying sample by the heat pipe probe, a mathematical

approach was found to be necessary. A mathematica1 model which inc1udes the

heat transfer governing equations cao he of benefit in the understanding of the

process and cao lead to better designs.

In the current chapter, two mathematical models will be presented; one is

HEATPIPE which incorporates the heat pipe operating parameters regardless of

the defined task for the heat pipe, and the other is SOLIDIFICATION which

models the freezing of the button shaped sample taken by the heat pipe probe.

The heat pipe model was initially developed to simulate the heat pipe

injection lance used in copper smeltingS2• However, this simulator was also used

successfully for the present application, since the same heat transfer fundamentals

govern both the heat pipe injection lance and this heat pipe solidification probe.

The solidification model written from first principles, is a two dimensional

heat transfer FORTRAN program. This model uses the boundary conditions

computed by HEATPIPE to predict the temperature and heat transfer behaviour

• MODELLlNG BEAT TRANSFER

of the freezing cylindrica1 samp1e with time.

6.2 Beat Transfer Model of the Beat Pipt! Probe

91

HEATPIPE 1.OS2 is a control volume, finite difference software simulation

package created to model the steady state behaviour of annular reflux

thermosyphon injection lances. HEATPIPE 1.0 which employs a flat-front (see

4.3.2.2) mode1 has been used at the McGiIl Metals Processing Centre in the design

and analysis of heat pipes. HEATPIPE 1.0 has been written in FORTRAN for

MS-DOS PCs.

Users ofHEATPIPE 1.0 employa graphica1 user interface in order to input

data pertaining to the pipe, working substance and boundary conditions. The model

includes 57 unknowns which are ca1culated iteratively using the Newton-Raphe~on

method. Model results are presented graphically to the user following the

successful completion of a simulation.

6.2.1 Model Construction:

6.2.1.1 Nodes-Vertically, the pipe is sectioned into 6 discrete areas. The

inert gas section contains no nodes because it is assumed that negligible heat

transfer takes place in this zone. As is the case with the condenser section, the

length of the inert gas section is not known prior to execution of the model. In a

gas loaded thermosyphon, the position of the gas/vapour front (and, thus, the

lengths of the inert gas and condenser sections) is an unknown parameter.

Vertically, the condenser c.Jntains 3 nodal slices, the adiabatic section l, and the

evaporator section contains 2. The lengths of both evaporator and adiabatic

sections are known. Figs. 6.1 and 6.2 show the allocation of nodes in the

Temperature Nodesof the Bottom of the Pipe

Tb.c

• CHAPTER SIX

--"-r"-IlgJI

L _ __ ]"

'.T----- J

a

L -- l1.

~J

Inert Gas sectionoNodal Rings

Condenser Section3 Nodal Rings

Adlabatlc Sectionl Nodal Ring

Evaporator section2 Nodal Rings

92

TlpAree

Fig. 6.1 Vertical sections and allocation of nodes in the HEATPIPE model•

• MODELLING HEAT TRA!';SFEP. 93

Tws

InnerPlpe

Outer Pipe

Protectlve Coating

Fig. 6.2 Cross section of a nodal ring in the HEATPIPE model.

••

• CHAPTER SIX 94

HEATPIPE 1.0 model.

6.2.1.2 Beat pipe types-HEATPIPE 1.0 may be used to model type 1and

type II thermosyphons. In a type 1 thermosyphon, the inert gas inventory is a

fixed parameter and system pressure is unknown. In a type II thermosyphon. the

system pressure is fixed by adjusting the inert gas inventory. In this case. the

precise inventory of inert gas contained within the pipe is a variable which must

be solved for. In either case. the total number of system variables remain

um:hanged.

Table 6.1 Variables employed in HEATPIPE model.

Variables Description #

'It,. for i= 1••6 Energy transfer from environment to worlcing substance. ith Dode, W. 6

'IJ..fori= 1..6 Energy expeUed from w"rlcing substance la reagent gas. ith Dode, W 6

'!tJp Energy absorbed by worlcing substance through lance tip, W. 1

T... for i=1..6 Bulk temperature of reagent gas, ith Dode, K. 6

T,. fori= 1..6 Temperature of inner wall of inner pipe, ith. K. 6

T" for i=I..6 Temperature of outer wall of inner pipe, ith. K. 6

T... for i=1..6 Temperature of inner wall of outer pipe, ith. K. 6

T" for i=1..6 Temperature of inner wall of protective coating, K. 6

T,a for i= 1..6 Temperature of outer wall of protective coating, ith, K. 6

T.....T...,T... Temperature at bollom of the pipe. K. 3

l, Length of active condenser, m. 1

1,.,« Length of blocked off region predicted by flat front model=lt-lc. m. 1

V" Volume consumed by inert gas plug, m'. 1

TM Temperature of worlcing substance, K. 1

P(Type 1 pipe) System pressure or Moles of inert gas contained in the pipe. 1

or~(Type n)

Total 57

6.2.1.3 Variables and equations-HEATPIPE 1.0 uses user-input boundary

• MODELLING HEAT TRANSFER 95

conditions and material properties to solve a system of 57 equations and 57

urJmowns.The unknowns are listed in Table 6.1.

Table 6.2 lists the equations used to solve for the variables listed in Table

6.1. Equations 6.2, 6.3 and 6.6 represent the forms for steady 1-0 radial

conduction heat transfer for a circular cross section. Equations 6.1 and 6.8

represent the forms for steady 1-0 r.tdiative and convective heat transfer to an

exposed surface. Equations 6.4,6.5,6.7 and 6.11 represent the heat flow from a

surface to a fluid by a purely convective mechanism. Equations 6.9 and 6.10

represent the conduction equation for a 1-0 Cartesian system. Equation 6.12

represents the energy balance on the reagent gas with two terms: one representing

the temperature increase in the gas, the other representing the loss of energy dur;

to depressurization of the gas stream. Equation 6.13 represents the global energy

balance on the working fluid. Equation 6.14 represents the relation between

pressure and temperature which exists for a given working substance. Equations

6.15 and 6.16 represent geometric identities. Equation 6.17 is the equation of state

for an ideal gas.

6.2.2 Input: HEATPIPE 1.0 solves the steady-state representation of a

thermosyphon using user-input parameters. Figs 6.3, 6.4, 6.5 and 6.6 illustrate,

respectively, the main menu screen, the working substance screen, the boundary

condition screen and the pipe configuration screen for the simulation of a Type II,

laboratory scale, thermosyphon probe for thermal analysis of aluminum casting

alloys.

As pointed out earlier, HEATPIPE 1.0 was initially developed for a

thermosyphon injection lance applicable in copper smelting. In order to apply the

package to the solidification probe, the appropriate boundary conditions are to be

entered. Fig. 6.5 depicts the boundary condition screen. Since no reagent gas

• CHAPTER SIX

Table 6.2 Equations employed in HEATPIPE model.

96

Description Equation #

q from environment 'Ii.•=2.n.r;,.h;..,,(T•.r T,.,) + PEP.~•.i-T\,) Eq.6.1 6

q through outer coaling 'Ii,.=2.n.~.k".!n[r;ir;.ll • (Ti.,-T;'I) Eq.6.2 6_.q through outer pipe ahell 'Ii,.=2.n.~.k..!n[rdr;.J . (T;.rT;.J Eq.6.3 6

q from outer pipe sbell la 'Ii, =2.n.r· .~.h; (T. r T.,.) Eq.6.4 6• loe..... l,

working substance

q from outer pipe sheU la 'li,b=2.lt.r,·4·h;.n(Tn-T,.J Eq.6.5 6

working lubstance, Dode i

q lhrough inner pipe sheU 'h.b=2.lt.4.k,.ln[r,lr"J . (TI~-TI.,) Eq.6.6 6

q inla reagent gas 'li,b= 2.n. rb.1;.1's..(T;.b·Ti.'> Eq. 6.7 6

q la the lance tip 'Itip=hooaom.Aoouom(Tcnv,tipTb,J+PEF.~CllV,tiprb,J Eq.6.8 1

q through outer coaling, q tip = k,,·Aoouom·(Tb,.-Tb.bJ/lc Eq.6.9 1

lance tip

q through outer coaling, q tip = k,,·Aoouom·(Tb,b-Tb,'>/t. Eq.6.10 1

lance tip

q from outer pipe sheU la CLip= h,;,.......At..a..,.(Tb.,-T.,.} Eq.6.11 1 Il

working substance, lance tip

Reagent gas heat accum. 'li,b= ProV,.As·c;....·(T;..-TI-I.J-V,.As.(dP.../dz) Eq.6.12 6

Working substance q balance CLip+ I('Ii,."'Ii,tJ= 0 Eq.6.13 1

Clausius.Clapeyron !n( P/IOI.3 X103) = (afr.,.)+ b Eq.6.14 1

Length conservation !;,.rr + 1" = 1, Eq.6.15 1

IG lenglh/volume ratio V;, = n (flril.> . l;,.ff Eq.6.16 1

Ideal gas law P.".V;, = n;,.R.T;, Eq.6.17 1

Total 57

MODELLING BEAT TRANSFER

exists the "Reagent Gas Characteristics" column must be set for the liquid meral

sample inc1uding the sample temperature, density and heat capacity.

6.2.3 Output: Following the successful execution of the simulation, the user may

examine the values of the calculated variables. Fig's. 6.7, 6.8 and 6.9 illustrate

sorne typica1 output screens for the input conditions. Fig. 6.7 illustrates the outpt'!

of the pipe's temperature profile. The temperature indication in the sampling

region is the steady state temperature of the working substance corresponding to

the pressure of the system. Fig. 6.8 illustrates the output of the main system

parameters. Unlike Fig. 6.7, thi~ is a screen output to scale and contains severa1

quantities ofinterest, inc1uding, among other results, the maximum vapour velocity

within the pipe, the percentage of available condenser used and the tC'ta1 power

extracted from the heat source. Finally, Fig. 6.9 illustrates the system limits

comparing the maximum allowable for the configuration and operating parameters

with the computed values. Il is seen that the conditions for the routine operation

of the thermosyphon probe are remarkably lower than the critical (maximum

allowable) quantities.

6.2.4 Evaluation of Model Results: Although the HEATPIPE 1.0 package was

not originally intended to be applied to this thermosyphon probe, the computer

code has been used successfully to simulate this probe. The data presented in Figs

6.3 through 6.9 represent actual input parameters that were used to perform

simulations in parallel with the routine experiments using a cesium thermosyphon

used for the thermal analysis of a 356 aluminum alloy. Table 6.3 illustrates the

agreement between the predicted model results and the experimental data. The

model is a very useful tool in the design and analysis of the laboratory scale

thermosyphon probe since sorne important parameters such as heat transfer

• CHAPTER SIX 98

Fig. 6.3 Main menu screen for HEATPIPE 1.0

Fig. 6.4 Worklng substance screen for HEATPIPE 1.0

• MODELLING HEAT TRAN5FER 99

Fig. 6.5 Boundary condition sereen for HEATPIPE 1.0

Fig. 6.6 Configuration sereen for HEATPIPE 1.0

• CHA l'TER SIX 100

\A!ORI'.ING suas TANCE'5643·

INERT GAS600

.,....... ', ......

......ADIA8ATIC

EVAP NODE 1

EVAP NODE 2

CONDENSER

·....·......·.. 599.1

.. .' 625.0.~.,.

.....5981.,. .....

................-. 625.0

559.6

555.8

564.3

564.3

....

.,t'••.........;.....

578.3

............'648.2

,.: ';: ., .::: •••••• ~iI ••••••:i:·.·.·.~: ., ••••••::: •••••• ~: ,:! ••••••Il •••••• ,'' " ••••••

" . ::: :: .: .....>..... :i •••••• ~': ::: ••••••

. .. -: ~:: ::: ...:::: ',. ;:; .:;; :; .

····:::4\:::.,::::: li[ ;'1:::::::::''iI!.~...... ~:: ..••••••"j .'.~ "':;'.' • 'ii ! ••••••

. • 4 .•,,. ,.. ": ••••••

:;:; .. ' ' .'.. :~;; ;; .:::······~:f " .\:1·······:: il······,,: •••••••!: u······. . .. : ; ; .

",.:::. ". • ••••••!; ": ••••••.: " :.. : .".::->. •••••• .::: .••••••

. '.::: •••••••:g !'i •••••• ·mi". ',::: •••••• !1I ": •••••• J:::

'''''••••••• i U ~,\ •••••• ·:u:~i~.~ .• •••• ~~~ ...•••••••..,.:.; "! :: •••••• (' ..

~:: :::;::,;~,l : :':::;;.: ~i ..•••• '::: ... '::!':"::. :'::;:1 ;! :: ::::$>

~! ~.~~~,::~'~J ::..........

CONDENSER

564.3'364.3"

EVAP NODE 1

564.3564.3'"

EVAPNQOE :2564.3

~64.3 ...:""

AOIABATlC

564,J·

5G4.3·.

Rq. 6.7 Temperature profile screen for HEATPIPE 1.0

CERAMIC

"" .-"" METAL SHELL

It-iERTGAS

REAGEt~T(3A5

WQRI<,rHG SUSST...\NCt:::: (EV.... t-')

..... WORKING SIJSSTAHCE

• MODELLING HEAT TRANS FER

RACIAl. STRETCH FACTOR IN THIS GRAPHie

;:

MOLE':! OF INERT lJ""S \.. 10001 ..

tu l..UAOINU "'HI:. S-,UHI:; 1...... t ..I.1 ..

CONOENSER LENOTH (m.'.u)"

SYSTEM PRESSURE IP ...<, ..I.\ ..

MA',IMUM VAPOF=l 3PEEO {lIYII"

"OF AVAlLA9LE CONDENSER USEO

"OF HEAT REC",'CLI::O

TOTALWI\TT~E~TRACTEO

PIDG' ConllQUIJIUon SOLIDIFleATiON PROUE

rncss c:t~TCR TC! E <.IT

LEGEHD

~,J)

.,33"000('1

].:;..~H 49

1() 1

Fig. 6.8 System parameter screen for HEATPIPE 1.0

Fig. 6.9 System Iimits screen for HEATPIPE 1.0

•CHAPI'ER SIX

coefficients can he evaluated.

Table 6.3 Results from experimental data and computed simulation.

Experimental HEATPIPE Error

data 1.0 %

Sample temperature 566°C 564.3°C

839K 837.3K 0.2

% of condenser used 75.3 68.5 9.9

Outside condenser wall temperature 568°C 555.8°C

841K 828.8K 1.5

6.3 Beat Traosfer Model of Solidification

102

6.3.1 Model Construction: To provide a general mathematical view of

...•..- .(" )1.> '" ." j;i l1 .1 l• ,i!,' ,.' ..-....... l(., ,.\" /

,.'.................Idenlical planes

•A B

Fig. 6.10 Geometry and configuration of the sample•

solidification of the sarnple in the designed heat pipe probe, a relatively simple

model has been developed. Tlùs model, in which no commercial computer code

has been employed, basically uses a two dimensional finite difference method in

cylindrical coordinates. A mathematical formulation will he established for

solidification of the sarnple geometry as shown in Fig. 6.10.

The latent heat release during solidification is determined by the total

enthalpy method in which only one energy equation in terms of enthalpy is used

for both solid and liquid phases. The governing equation for a general three­

dimensional heat conduction problem with phase change, based on the total

enthalpy formulation in cylindrical coordinates, can be written as follows39 :

• MODELLING BEAT TRANSFER

opH 1 0 (fI' 1 0 oT 0 CT-=--(rk-)+--(k-)+-(k-)éJt r fJr fJr r 2 ae ae Oz Oz

103

6.18

In the above equation, convective heat transfer has been ignored. Also, according

to the axi-symmetry of the domain in the S direction (i.e. aTlaS =0, see Fig.

6.10B), equation 6.18 can he converted into the following 2-D equation for an axi­

symmetrical plane

where the total specific enthalpy (li) is related to temperature as:

T

Total ent1ullpy=H"fc,dT+hf,(l-f)o

6.19

6.20

•In the above equation the first term on the right hand side represents the sensible

heat, while the second one is the latent heat released during solidification. Note

that in equation 6.20 the release oflatent heat is assumed proportional to the solid

• CHAPTERSIX 104

fraction (f,) in the samp1e. A linear relationship between the solid fraction and the

sample temperature that assumes linear release of latent heat between the liquidus

temperature, Tb and the solidus temperature, TlOb has also been assumed. This

relationship yields;

T-TJ._-=-'=­

T,-T"",6.21

6.3.2 Initial and Boundary Conditions: Using the symmetry at the centre line of

the domain, the energy equation is solved for half of the axi-symmetrical plane as

shown in Fig 6.1l.

The initial conditions for the solution of equation 6.19 are: Hcr,z)=Hbalhand

TCr.z)=TbaIh, where Hbalh is the total enthalpy of the liquid bath in the sampling

5ymmelryUne

z

Fig. 6.11 Schematic of the computational domain.

regicn. In terms of boundary conditions, due to 10n51tudinal symmetry, (see Figs

6.10 and 6.11) the equation can he solved for half of the domain according to the

following boundary conditions:

1. The sample bottom temperature is always kept at the bath temperature.

2. The free surface of the sample is exposed to a hot environment.

• MODELLING HEAT TRANSFER 105

Radiative cooling is assumed from the solidifying sample to the environment with

the approximate temperature equal to the working substance temperature

(corresponding to its pressure).

3. The thermosyphon wall in contact with the solidifying sample affects the

working substance temperature inside the pipe. Therefore, from the P-T correlation

for a given working substance material, (e. g. cesium), the temperature inside the

pipe is known. Thus, heat is conducted through the thickness of the pipe wall

providing a known temperature in contact with the sample.

6.3.3 Numerical Solution Techniques: In this model a "finite difference" enthalpy

method, using a control volume approach for the formulation of discretized

equations, was employed. The explicit scheme was chosen to handle the discretized

equations. A typical control volume is shown in Fig. 6.12. For the grid point P,

points S and N (denoting south and north) are its z direction neighbours, while E

N

•Fig. 6.12 A typical control volume for 2-D situation.

and W (denoting east and west) are its r direction neighbours. The control volume

is shown by the dashed perimeter line; its depth in the e direction is assumed to

he unity.

The discretized equation is derived by integrating equation 6.19 over the

control volume and over the time interval 6t. Thus,• CHAPTER SIX 106

• nt+tu 1+A.t1l e t+4te ,.

JJ Jp aHrdrdzdt=JJJ~(ra:)drdzdt+ JJJkaz~rdrdzdt 6.22W8 t at t 8 W ar t W8 az

For the representation of the term aH/at, we assume that the grid value of H

prevails through the control volume. For the representation of the temls aT/ar

and aT/az, we assume that the heat flux spreads over the control volume faces

(Le. n, s, e and w). At these points the thermal conductivity is harm<:.'nically

interpolated from the values at the neighbouring nodes. Therefore, by integrating

the terms of equation 6.22 one obtains;

Transient term (first term) = rM 6zp (H _Hald )

The second term = 6t(ABTB+ Aw Tw -(AB + Aw )Tp )

The third term = 6t(ANTN +As Ts -(AN +As )Tp )

where AN: k"rM/(ÔZ)n; As: le. rM/(Ôz).; AB: k" r,jiz/(ôr)c and Aw: kw rvJ.z/(Ôr)w

Substituting the above expressions into equation 6.22 and applying the explicit

scheme, the discretized equation becomes:

6.23

where Ap =IAm" A0p=prp6zl6t, and Am denotes the neighbour of grid point

P in the r or z direction.

To solve the above discretized equation, using a 9Ox24 uniform mesh, the

enthalpies and temperatures of nodes are initially assumed and the enthalpies of the

nodes are calculated after a time-step. Based on the relation between enthalpy and

the temperature of the solidifying sample, the new temperatures of the nodes are

calculated and then, over the next time step, the enthalpies .and the temperatures

• MODELLING HEAT TRANSFER 107

of nodes are recalculated, and so on. The initial values of thermophysical

properties are given in a separate subroutine for the liquid metal at bath

temperature. The physical properties are then updated after each time step.

6.3.4 Solution Procedure: The solution procedure for the solidification model is

shown on the flow chart in Fig. 6.13. As seen, execution of the program is

initiated with a number of input data. Input data inc1ude the specifications of the

ailoy being used such as liquidus temperature, solidus (eutectic) temperature, latent

heat of fusion, sample density, thermal conductivity, and heat capacity. Another

set of input data is the pressure inside the pipe (determines the cooling rate), bath

temperature, and time increments. The heat contents for these known temperatures

are calculated according to the corresponding temperatures and remain as input

data.

In the grid design step, the grids are drawn unifonnly. Since this is a

solidification program, the initial conditions are set for the liquid state at the bath

temperature. The coefficients of equation 6.23 and the boundary conditions are

detennined with respect to the temperature situation in separate subroutines

attached to the program. Having ail the requirements, the discretized equation (Bq.

6.23) is then solved and a new H (heat content of the sample) is determined. A

new corresponding temperature is then calculated from the new heat content and

the result is saved in the output file. In the next step, the initial conditions of heat

content and temperature are replaced with newly computed values, and the

properties including density, thermal capacity, and thermal conductivity are

updated with respect to the new temperature. The program, then, starts over again

from the time increment addition and this loop is executed altematively until the

required time is reached.

• CHAPTER SIX 108

Edesign 1

+[ t=o )

+input initialconditions

( t=t+dt)

+calculate coefficientsofdesan~edequation

implement boundaryconditions

solve for H

+

~print output

data

update initialconditions

update properties

Fig. 6.13 The flow chart of the solidification program.

6.3.5 Examples: A computer program based on the control volume finite

difference method was implemented to solve a two dimensional solidification

problem for a cylindrical shape. The cylinder is 0.06 m in height and 0.017 m in

diameter. Since the emphasis of this work is mostly on aluminum-7%silicon alloy,

typical examples to he presented are for this alloy using a cesium charged

• MODEllING HEAT TRANSFER 109

thermosyphon. Generally, in each case the program was run twice: once for slow

cooling of the samp1e with an inside pressure of 0.33 atm. and a second time for

Table 6.4 Solidification and sample specifications used in the mode!.

Fig. 6.15 Fig. 6.16

Bath temperature 700°C 700°C

Thermosyphon pressure 0.33 atm. 0.22 atm.

Sample Al-7%Si Al-7%Si

TUquidus 615°C 615°C

T_. 577°C 577°C

fast cooling with an inside pressure of 0.22 atm. According to the actual

experiments, these are the bounded limits corresponding to the lowest and the

highest cooling rates respective1y. Therefore, any other cooling rate requires an

inside thermosyphon pressure between 0.22 and 0.33 atm. for an Al-7%Si alloy

solidified by the cesium charged thermosyphon probe.

As the first example, Fig. 6.14 illustrates the temperature distribution along

the centre line of the sample for the slow cooling rate case once equilibrium is

established with the surroundings (Le. when further solidification of the sample

ceases). The results can be used to detennine an optimum location for the

thermocouple in the real tests. It is seen that, in order to acquire the complete

temperature history, the temperature sensor must not be located further than

0.015m from the top of the sample. In the other words, once the temperature

through the sample reaches steady state, beyond 0.015 m from the surface, the

temperature is still higher than the eutectic (solidus) temperature, and solidification

• CHAPTERSIX

0,..----.,....------------,

0.01

:§:c: 0.02.Q

'iii8-ëII 0.03c:

~-ê'0.04.9

0.05

110

0.06 '--~_...J.._~_l._~_...J.._~~"___'

500 550 600 650 700Temperature (' Cl

Fig. 6.14 Temperature distribution through the centre line for a. slow coolingcase.

does not proceed to completion. For the fast cooling case one can anticipate a shift

in the optimum location downwards towards the melt. Nevertheless, for the sake

of being able to compare the results, in both slow or fast cooling, the position of

0.015 m below the free surface will be taken as the location for temperature

detection.

Figs 6.15 and 6.16 illustrate the temperature history (cooling curve) at

0.015 m below the free surface in the sample for the slow and fast cooling cases

respectively. The alloy specifications and other conditions are listed in Table 6.4.

In each figure, there are two sudden changes of slope. The first change

corresponds to the sample liquidus temperature, 615°C, at which the sample starts

to release latent heat. The second change occurs at the eutectic (solidus)

temperature, 577°C, at which the solidified sample stops releasing latent heat once

it is completely transformed to solid.

• MODELLING HEAT TRANSFER III

350

Comparing the slow and fast cooling rate curves, il is seen that in the slow

cooling rate (Fig. 6.15), the delay time at the liquidus tempenlture is substantially

640

630

620-.ü0--~ 610 f--

.a~

~

8. 600 f--

E~

590 -

580 -

570 u.11_'--..J.I--...J'--..l..-1-'--_.l...-1-,--_,--1..J--_1'--...l...-...l1_J....-l

o 50 100 150 200 250 300lime (s)

Fig. 6.15 The cooling curve of an AI -7% Si sample for a slow cooling rate.

longer than in the fast cooling case. This is as expected and is a result of the effect

of temperature gradient from the sample to the probe. A simiilU" scenario occurs

at the eutectic temperature (577°C). In the slow cooling rate case, the eutectic

• CHAPTER SIX 112

temperature spans about 225 seconds versus about 20 seconds at the fast cooling

rate. These observations indicate that the mathematical model is very sensitive to

640 .--,....------------------,

620

-()o-600~.a~Q)

0. 580E~

560

o 20 40 60Time (s)

80

Fig. 6.16 The cooling curve of an AI-7%Si sample for a fast cooling rate.

the cooling rate as determined by pressure inside the thennosyphon probe.

Figs 6.17 and 6.18 show the temperature distributions at various times

during the cooling process for slow and fast cooling respectively. Recalling the

boundary conditions, the bottom part of the cylindrical sample always remains at

• MODElL1NG &AT TRANSFER 113

the bath temperature and cooling is mainly radial. Therefore, there always exists

a longitudinal heat charge to the sample from the bottom, and a radial heat 1055

from the centre to the thermosyphon wall. This makes for a symmetrical 2-D

conduction heat transfer system through the sample. An overall vi~w of the

solidification patterns shown in Figs 6.17 and 6.18 confirms these points.

RegardIess of the elapsed time, the bottom portion of the sampling chamber is

relatively hot, and the isothermal contour lines are almost parallel and are very

close together. This cao be interpreted as an indication of a high heat flux from

the liquid metal bath which prevents formation of a significant radial temperature

gradient. As one progresses up from the bottom, and depending on the time and

rate of cooling, the isotherms become more separated and a more pronounced

radial temperature gradient appears. Thus, in the upper part of the sample,

longitudinal heat transfer gradually becomes less effective and radial heat transfer

becomes dominant. AIso, for both the slow and fast cooling rates, during the

solidification process, liquid, mushy, and solid sections in the sample can he

recognized, and as time proceeds the solid and mushy portions depress the liquid

section to sorne extent.

• CHAPTER SIX

R (m)0.000 0.004 0.008

0.000

0.005

0.010

0.015

R (m)0.000 0.004 0.008

0.000

0.005

0.010

0.015

114

0.020

0.025r

3' 0.030......,0.035

0.040

0.045

0.050

0.020

0.025r

3' 0.030......,

0.D35

0.040

0.055 ~!i~10.060 ê

t= 1 (s)

•Fig 6.17 Slow cooling solidification patterns at different times during

solidification.

MODEU.ING HEAT TRANSFER

R (m) R (m)0.000 0.004- 0.008 0.000 0.004- 0.008

0.000 0.000

0.005 0.005

0.010 0.010

0.015 0.015

0.020 0.020581 581

0.025 0.025

r r

3' 0.030 589 3' 0.030 589

'-J '-'

0.035 597 0.035 597

605 6050.04-0 0.04-0

613 613

0.04-5 621 0.04-5 621

629 629

0.05~637 0.050 637

645 645

0.055 0.055

0.060 0.060

t=251 (5) t=350 (5)

Fig.6.17 Contnue d

us

• CHAPTER SIX

R Cm)0.000 0.004- 0.009

0.000

0.007

0.015

0.022

r

'3 0.030~

0.037

0.04-5

0.052

o.oso

t= 1 (s)

R Cm)0.000 0.004- 0.009

0.000

0.007

0.015

0.022

r

'3 0.030'-'

0.037

0.04-5

0.052

o.oso

t=10 (s)

116

•Fig 6.18 Fast cooling solidification patterns at different times during

solidification.

MODELLING HEAT TRANSFER

R (m)0.000 0.004 0.009

0.000

0.007

0.015

0.022

r

3 0.030~

0.037

0.045

0.052

O.OSO

t=4D (s)

R (m)0.000 0.004 0.009

0.000

0.007

0.015

0.022

r

3 0.030~

0.037

0.045

0.052

o.oso

t=42 (s)

Fig. 6.18 Contnue d

117

• CHAPTER SIX 118

The solidification rate which is defined (in the present context) as the

velocity of the liquidus (615°C) along the sample centre line can be evaluated by

0.032

0.034

......

.s 0.036co~

':g 0.038c-m:§ 0.04;;,

=ë>c 0.042.:l

0.044

f2st cooling Slow cooling--- ""*i~1"7

1

* )l, 7

r- Il'

17 -

Il0.046

0.0060.0050.001o 0.002 0.003 0.004615° front lelocity (mis)

Fig. 6.19 A comparison of solidification rates for slow and fast cooling rates.

the simulator. Fig. 6.19 compares the 615°C front velocity (ÂL/~t) versus

longitudinal position for the slow and fast cooling cases. At slow cooling rates the

front velocity lies in the range of0 - 0.0006 (mIs) while in the fast cooling case the

velocity ranges between 0 - 0.0055 (mIs). It is seen that in no case is the liquidus

front velocity constant. Solidification of the thermal analysis sample is then non

steady state and at best one can speak of only an average freezing rate for the

sample.

CHAPTER7

RESULTS AND DISCUSSION

7.1 Introduction

A gas-Ioaded concentric thermosyphon has been designed to replace the

conventional thermal analysis set-up for aluminum casting alloys. In this system,

the evaporator of the probe is immersed in the liquid metal and the working fluid

is evaporated thereby establishing the temperature of the working substance.

Because of the temperature gradient across the evaporator wall, the latent heat of

fusion of the molten metal is extracted and a small amount of melt (in the shape

of a button) is solidified inside the core of the probe. A thermocouple located at

the centre of the evaporator measures the instantaneous temperature of the

solidifying button. During freezing, the time and temperature are recorded by a

data acquisition system. After solidification is complete, a higher pressure of inert

gas is applied ta the thermosyphon thus blocking off the vapour from the

condenser. As a result, heat transfer between the evaporator and condenser is

virtually eliminated and the relatively small solidified mass gains heat from the

liquid bath in which it remains immersed. Eventually it remelts and is

reassimilated in the melt (see Fig. 5.3). As seen in Fig. 5.3, the outer surface of

the evaporator is covered by a relatively thick graphite block. This shell protects

the evaporator booj" against dissolution in liquid aluminum, and, in addition, it

partially isolates this part of the evaporator from the hot liquid metal bath. The

thermosyphon (i.e. probe) need not be withdrawn when it is not in use. It resides

as a pressurized chamber in the melt while it awaits the signal to analyze a new

fresh sample.

It will be recalled that the main objective of this work was the design,

testing and modelling of a novel in-situ probe for conducting controlled thermal

analysis of aluminum-silicon casting alloys. Since the probe is basically a heat

transfer device and its applicability depends OIùy on the working temperature range

regardless of the nature of the hot media (i.e. liquid metal bath), three liquid

aluminum alloys were chosen for testing. The three systems were pure aluminum,

aluminum-7 %silicon (356 alloy), and aluminum-12%silicon (413 alloy). Table 7.1

shows the composition of the aluminum alloys used in this work.

• CHAPTER SEVEN 120

Table 7.1 Nominal chemical composition of the AI alloys tested.

Sample Si Cu Mg Fe Zn

356 7.0 <0.20 0.35 <0.2 <0.1

413 12.0 <0.1 <0.10 <2.0

Among these, pure aluminum has the highest melting point of 660°C at the upper

bound ofworking temperature limit for the probe, while alloy 413 is basically an

eutectic composition with the melting (eutectic) temperature of 577°C which is the

lowest limit for this application. Since most other common aluminum silicon

foundry alloys solidify between 660 and 577°C, it is reasonable to conclude that

if the probe can be successfully used for pure aluminum and eutectic aluminum

silicon alloy (413), it will be applicable for the entire range of aluminum silicon

casting alloys with the silicon content between 0-12%. In addition, because of the

• REsULTS AND DISCUSSION 121

nature of the simple eutectic composition (see Fig. 3.1), sorne hypereutectic

aluminum-silicon alloys can be tested by the probe. The third system (aluminum­

7%silicon) is a representative of alloy 356 which is one of the most commonly

used aluminum silicon foundry alloys. AIloy 356 is cast in both sand and

permanent molds and because of its properties such as excellent fluidity, resi~tance

to solidification shrinkage, resislance to corrosion, very good weldability, and

good machinability, it has found a vast variety of applications. Sorne of its

applications in sand casting are: air compressors, water jackets, and crankcases.

Permanent mold castings of alloy 356 inc1ude: aircraft fittings, impellers,

accessory housings for internal combustion engines, jet engine compressor cases,

passenger car wheels, and marine usages.91 In terms of solidification

characteristics, 356 alloy solidifies through a relatively large mushy zone with a

solidification range of about 38°C. AIso, sorne liquid processing such as

modification of silicon morphology and grain refinement are done on this alloy.

Therefore, it was found necessary to inc1ude this alloy in the testing of the

thermosyphon probe. Commercial grades of these alloys were used in order to

evaluate the sensitivity and applicability of the probe on real industrial materials.

""r-------------,'" ..,L..._. ..."'-'-'....:..:..._..__""'...._

""Ê ...

1...~ 070

""

""~o ~ ,œ ,~ B ~ ~ * ~

nM(l)

Fig. 7.1 The cooling curve obtained by the conventional method for pure AI.

7.2 Typical Results

• Chapter Seven 122

In order to prove the workability of the probe and to show how il responds, the

first set of experimental results to be presented are for the solidification of pure

Al and Al-Si eutectic alloy by a potassium ch3l'ged thermosyphon probe. Fig. 7.1

shows the cooling curve for pure aluminum obtained with conventional thermal

analysis equipment (see 3.4.3) that included a sample cup similar to a sand mould.

It is presented here as a source for comparison with the curves obtained with the

newly developed probe. This conventional cooling curve has three distinct

segments:

1) cooling in the liquid state,

2) a fiat portion which represents the liquid to solid transfonnation,

0.2

0.7

0.5 -!!

0.3 iil

~,

___________________________ 1

_....--

••,

rr;:::============;:j""'---"j'] 1

A1..I!!!'p. W.F.Temp. PrellSUre

680

620

Ô 660'-!

ii 640

t!

600 L.JL....-=::::::::;i:::====::::===~ ......__-'-_........JO

0.160 120 180 240 300 360 420 480

llme (s)

(a)Fig. 7.2 a: The general view of the results for a pure AI test by the probe.

•3) cooling in the solid state.

Fig. 7.2 presents the first resuIts acquired by the thennosyphon probe.

Generally, they contain three curves in the same figure (Fig. 7.2 a): one depicts

• REsULTS AND DISCUSSION 123

680

Ô"""660

~

1640 ~LIqu;::!:::.Id~M:::..P.:..+-__...:so=iJ:...' --<~LIq:!u::ld~~ 620

• Freezlng Remelting.. .

0.7

0.5 ~

.!.

0.3 §0.2 ~

6OO,-__~ --.J

o GO 120 180 240 300 360 420 480Tlme (s)

b

r-;=====:;;;;;;:;TI---""\1~ fli85S,",,_;,;;_,;,.!'._m1!

111

\ 11 11 11 11 11 11 11 11 :l ~

• Remeltlng.. .

o GO 120 180 240 300 360 420 4800

.1

Tlme (s)

C

\1W.FJSIJ1l. /

680 1Ê 660

IRemeltln9l!!~

Freezlng640 • . 4,

~\

1

~ 620 ,1

\ 1600

1

0 GO 120 180 240 300 360 420 480Tlme (s)

d

Fig. 7.2b: The cooling and heatlng curves,c: The pressure curve,d: The worklng fluid temperature curve.

• Chapter Seven 124

the thermal analysis curve that is the cooling and heating curve for the button( Fig.

7.2 b). The other shows the inner pressure of the probe for the freezing and

remelting periods (Fig. 7.2 c). During the freezing period the pressure is, in fact,

the saturation vapour pressure of the working substance. The third curve illustrates

the corresponding temperature of the working substance at the given pressure Fig.

(7.2 d). By comparing Figs. 7.1 and 7.2b, it can be seen that the cooling curve

depicted in Fig. 7.2b represents a higher rate of cooling as evidenced by the

shorter plateau region. Thus, one can conclude that a chamber pressure of 0.17

atm. (Fig. 7.2 a and c) yielded a faster cooling rate than that of the simulated

mould casting (Fig. 7.1). It is worth noting however that both techniques yielded

curves simiIar in every respect.

Fig. 7.2 also shows ili<l results corresponding to the remelting of the

aluminum button. Once the button had solidified and cooled to ·approximately

680 rT-'""";:::::;:;::::==;;;:;::==::;;==:::::;----.., 0.71AI Temp. W~mp. r:.r~~l!!! 1

670 - 0.5

6 _

~ 660 '--------------------J ~~Gli 650 r,------------------- ....... -------------- 0.31

\ 0.2 a.

~ ::~ l,------,--------····-----,.....--....---1.----' 0.1o 60 120 180 240 300 360 420

Time (5)

Fig. 7.3 The cooling curve oblained by the thermosyphon probe for pure AI.

630"C, the probe was pressurized to about 1 atm. with inert gas (at time=330 s) .

From Fig. 7.2 one can clearly see the effects of this action - the pressure increases

• REsULTS AND DISCUSSION 125

------'---

instantaneously (Fig. 7.2 c); the temperature of the working substance increases

rapidly (Fig. 7.2 d) as a new equilibrium is established, and the temperature of the

button begins to rise. The temperature of the batton first increases rapidly and then

decelerates as it approaches 660·C. Once remelting is complete, the temperature

heating curve resumes its steady climb towards the temperature of the melt. The

remelting of the button was accomplished in a span of about 2 minutes. Once the

button had completely remelted, the probe was ready to perform another thermal

analysis Le~(.

The next step in the experimental program was to increase the chamber

720 r---;::::;:;:;==:;:;:;;;;::=::::;;:::::=:::;---..., 0.7AI Temp. VI!,r.Temp'. P!~J1~

. 0.5

6~ ~

~~O -------------------------------.Q3 !~ 1 ~

1 1\ ~ l~ 6601-\ '---------------------1

l--640 L..._...l-_--l.__.l--_...l-_.--l.__.l--_...l-_--' 0.1o 60 120 180 240 300 360 420 480

Time (5)

Fig. 7.4 Quasi equilibrium solidification with the thfmnosyphon probe.

pressure during solidification. The results are depict';d in Figure 7.3. For this test

the chamber pressure was stabilized at 0.24 atm. initial pressure versus 0.17 atm.

used in the previous test. As is evident, the higher pressure gave rise to a slower

effective cooling rate wlùch in tum lengthened the plateau.

• Chapter Seven 126

Another test was conducted with the same batch of aluminum. The initial

pressure inside the probe was set at 0.3 atm. versus 0.24 atm used in the previous

test. As a result, the solidification time was greatly increased as shown in Fig. 704.

In this case a quasi-equilibrium was established. This feature can be of particular

interest when one is attempting to study a reaction or phase formation during

solidification.

Another series of tests was conducted with 413 aluminum-silicon alloy.

Generally, alloys of the 413 fami1y are near eutectic alloys and have simple

6OOrr---------------,590

Û 580~

~} 570

~560

550'--.....-"_-.....- .....- .....- .....- .....-..1o 60 120 180 240 300 360 420 4e)

lime (8)

Fig. 7.5 The cooling curve obtained by the conventional method for a 413allo';" .

cooling curves. The experimental procedure adopted in these tests was essentially

the same as that used for pure aluminum. Fig. 7.5 shows the conventional cooling

curve for 413 alloy. It is to be noted that the accepted eutectir '•.}mperature is

577°C which is in excellent agreement with the value obtained from the

experimental conventional cooling curve.

• REsULTS AND DISCUSSION 127

The probe was used to perfonn a thennal analysis of the same batch of 413

aluminum alloy. The cooling curve obtained with an initial pressure of 0.09 atm.

is presented in Fig. 7.6. One can see there is an abrupt change in the slope of the

cooling curve as the liquidus temperature ( about 580 oC) is crossed. Moreover,

as the solidus is reached there is another abrupt change and solidification of the

eutectic begins to dominate at the expected temperature of577°C. These events are

very distinct on the cooling curve.

As a final example, consider the cooling curve shown in Fig. 7.7. In this

test the initial pressure was set at about 0.05 atm. versus 0.09 atm. for the

previous test with the result that heat extraction was enhanced and solidification

590 nr--;:=::::;:=:::;:;;;;==::;:=::::;~-,1...._Al_1i_e_m_p_.__W_._F.1i_em_p_. ~re__..s~re_....1

0.05

0.5

'--"----------J- 0.3 i~

0.21- - - - - - - - - - - -._- - --~---::-.: 01 Il.-------- ------- _.-...-.-.-...... .

-----~~-"~~......-.........~li .•·-~,

550 .....0-.;;.---....----.....----....'------'---....o 60 120 180 240 300 360 420 480 540 600Time (s)

Fig. 7.6 The cooling curve obtained by thermosyphon probe for 413 alloy.

5806'~

Il!:::J

570 -~c.

~560

•time shortened. While the liquidus and solidus inflection points are discernible,

they are not as clearly denoted as in the previous test. High cooling rates tend to

• Chapter Seven 128

obscure these events. Also shown in Fig. 7.7 is the remelling of the 413 Al aDoy

button. When the probe was pressurized with inert gas to about 1 atm., the

temperature within the button increased then decelerated as the button me1ted and

finally increased to the melt temperature. The reme1ling of the button was

accomplished in a span of about 3 minutes and the system was ready for another

test.

In aD curves obtained by the thermosyphon probe, it is seen that the

working substance pressure (and the corresponding temperature) ooes not remain

constant during the thermal analysis test. An increase in the working sub~tance

pressure and temperature was always detected. This occurs because the low

pressure is imposed by the vacuum pump in a very short lime and disturbs the

equilibrium. The system, then, has to pass through a transient state in order to

590

1Al Temp. W.F.Temp. Pressure 1/----1---- 1-----

580 : 11 1

6 1 0.51 ~

l..-I !l!! 1

15701 l!!1 :>1 ..1

0.2 ~~111

560 11

~ 0.1\ 1

\ ... -----_.\ ---- ------

550 .. -0 60 120 180 240 300 360 420 480 540 600

Time (s)

Fig. 7.7 The cooling and heating curves of 413 alloy•

• REsULTS AND DISCUSSION 129

build up a new equilibrium by accelerating the vaporization, and increasing the

average temperature of the chamber. The increase in average chamber temperature

causes an increase in the system pressure. In order to reduce this transient

phenomenon, the experimental set-up had to be improved. An empty tank was

connected to the probe as a buffer (so called pressure stabilizer) between the

vacuum pump and the condenser, thus enlarging the condenser volume and

650

640

630

~ 620U0-I!! 610

'"ë8- 600E~ 590

560

570

0

Decreasing cooling rate

60 120 160 240 300 360 420 460 540 600 660 720

lime (s)

Fig. 7.8 Effect of cooling rate on depression of eutectic temperature of anAI-7% Si alloy.

stabilizing the pressure during the thermal analysis test. (see Fig. 5.3). With this

modification, the pressure remained acceptably constant during each test.

ln order to evaluate the effect of different inner pressures on the cooling

• Chapter Seven 130

curve of the same sample, an aluminum 7%silicon alloy was chosen to be

solidified at several inner pressures by a cesium charged probe. Fig. 7.8 illustrates

cooling curves of the same Al-7%Si alloy with different inner pressures (i.e.

cooling rates) by the thennosyphon probe.

The procedure of the experiment was such Ihat the pressure inside the probe

was set at a level that gave a very low cooling rate (e.g. 0.33 atm.). This pressure

was low enough to completely solidify the sample and high enough to give one of

the lowest cooling rates possible(curve 1). Once the desired cooling curve was

obtained, the probe was pressurized with inert gas, blocking off heat dissipation

from the sample. Consequently, the solid sample starled remelting, and the

temperature was restored to the initial temperature of the liquid bath. (Heating

Table 7.2 Variations of cooling rate and eutectic temperature with inner

pressure for the curves of Fig. 7.8.

Pressure Cooling rate Eutectic tempoCurve#

(atm.) (OC/s) (oC)

1 0.33 0.6U 578.0

2 0.31 0.80 576.1

3 0.30 0.85 575.7

4 0.28 1.00 575.0

curves are not shown in Fig. 7.8.) Then, the same procedure was followed but

with a lower inside pressure to speed up the cooling rate, and curve 2 was

obtained and so on. Table 7.2 shows the variations of cooling rate and eutectic

temperature versus the inner pressure of the probe for the curves of Fig.7.8.

As seen, by gradually increasing the cooling rate the eutectic temperature

• REsULTS A.to<D DISCUSSION 131

is depressed as expected (see 3.3.1). The cooling rates in Table 7.2 are, in effect,

the slope of the mushy zone portion of the cooling curves. The point to note here

is that all of the cooling curves were taken in the same melt, and the whole test

required a span of about 45 minutes without any need for special or extra

equipment to adjust the cooling rate.

Following investigations on the applicability of the thermosyphon probe for

different cooling rates, the probe was used in conjunction with a COll",nercial

thennal analysis system. The Meltlab7s system includes a combination of data

acquisition hardware and software. It has been developed to he used with

conventional thennal analysis equipment (see 3.4.3) and for each alloy the proper

software has to be loaded. The output of the system is Iwo graphs on one sereen

(Fig. 7.9): one graph presents the cooling curve as it is acquired, and the other

presents data regarding the rate of cooling. The rate of cooling part has Iwo

vertical axes: the left vertical axis is the fust derivative of temperature with time

(dT/dt), and the right hand one is the second derivative of temperature with time

(d2T/df). During the test, the ongoing-smoothed cooling curve plus Iwo

corresponding cooling rate curves can be seen on the screen. The current

temperature and the eutectic temperature of the alloy are also shown. This system

was attached to a cesium charged thennosyphon probe, and three distinct inner

pressures of 0.33, 029, and 0.20 atm. were tested for a 356 alloy. The results are

shown in Figs 7.9 to 7.11. Fig 7.9 illustrates the Meltlab screen for a 356 alloy

obtained by the thermosyphon probe with an inner pressure of 0.33 atm. Note that

the cooling curve is only a line chart and the horizontal axis is not necessarily in

seconds. Obviously, the cooling rate changes significantly during solidification and

il is impossible to describe the cooling rate by a simple value for the whole

solidification process. On the other hand, there is no universally accepted

definition of cooling rate, but for those alloys with a mushy zone (such as 356),

CIiA/'TER SEVES }''').)-

Fig. 7.9 The Meltlab screen for a 356 alloy obtained by the thermosyphon probein low cooling rates.

RESULTS AND DISCUSSION

Fig. 7.10 The Meltlab sereen for a 356 alloy obtained by the thermosyphon probein medium eooling rates.

•CHA l'TEK SEVEN 134

Fig. 7.11 The Meltlab screen for a 356 alloy obtained by the thermosyphon probein higher cooling rates.

• REsULTS AND DISCUSSION 135

many compute the cooling rate as the average through the mushy zone. In this

case, the cooling rate (here defined as dT/dt) in the mushy zone averages about

0.4 °C/s for the inner pressure of 0.33 atm. Fig.7.10 shows the same screen in

which the inner pressure of the probe was kept at 0.29 atm. As seen from the

length of the plateau and the cooling rate curve, a considerably higher cooling rate

was obtained. The average cooling rate in the mushy zone was about 0.8 °C/s

(twice as much as the previous case). Finally, Fig 7.11 shows the Meltlab screCl1

of the same alloy for an inner pressure of 0.20 atm. In this case the rate of cooling

in the liquid state is so fast that it lies beyond the scale of the graph since the

system has not been developed for such a high cooling rate. Also, due to the fast

cooling rate the length of the plateau is so short that it was not recognized as the

eutectic temperature (at about 563°C) by the program. Instead, the temperature at

which the solidified sample reached equilibrium with the inside temperature of the

probe (526.9 oC) was indicated as the eutectic temperature. The heating (remelting)

curve is also shown in Fig. 7.11. As a general comment, it seems that because of

heavy smoothing done by the software, the true rates of cooling are higher than

those shown.

7.2 Parametric Results

A general view of probe behaviour during thermal analysis testing and the

cooling curves obtained were featured in the previous section. As a subsequent

step in this study, Il was decided to apply the probe to investigate major liquid

metal treatments that are commonly used in industry. Treatments such as

inoculating (grain refinement) and modifying molten aluminum silicon alloys are

two major liquid metal treatments that will be discussed in the following sections.

• Chapter Seven 136

7.2.1 Grain Rermement: To study the applicability of the probe for grain

refinement investigations, a commercial grade of 356 alloy and a cesium charged

thennosyphon probe were employed. The procedure was such that first a thermal

analysis of the alloy containing no grain refiners was conducted. It was realized

that the inside pressure of 0.5 atm. was a suitable pressure to clearly illustrate the

sensitive portion of the cooling eurve. Once the desired part (liquidus portion) of

the cooling curve was obtained, a higher pressure of inert gas was applied and the

temperature of the sample restored back to the liquid bath temperature. Then,

2020600 L..&.-_...L.....................L_--' 0.05

40 60 80 100

lime (s)

630

1 ~~~MlQI1

1 ~:~~MlQI630

Unrelined Gnin-rofined

- --625 625

-,------------------- 0.5 ---------.---._---------..... 620

.....620

..-Ë 0

0 0

:..... 0.3 :!! -i 615

l!! ~:::J 615 10.2 ~...

~ 610

a..~610

0.1

605 605

Fig. 7.12 Comparison of cooling curves of an unrefined and grain refined 356alloy at the Iiquidus portion of solidification obtained by the probe.

•about 0.2% Ti was added to the melt as Al-5%Ti master alloy. The pressure was

lowered back to 0.5 atm. (macroscopic scale) and the cooling curve for the grain

refined alloy obtained. In Fig. 7.12 a comparison of the cooling curves for grain

0.55

• REsULTS AND DISCUSSION

635r------;:======:------,O.81 T~'" ~ 1

137

630

Ê 625!!.aI!"0.

620E~

815

----------------------------------------- 05

0.35

0.55 .

610<IO!::---.;8O;;---::8O,...-.......,1:!;:00:;----='I20~--:I<1O::::--*18O;;--:;!,1800.311me (a)

(a)

6351 ------;=======;----1 o.8

1 T_"'" ~~ 1

630

615

------------------------------------.------ 0.5

0.35

6101.-..J---......---'--.......,~--'----'~0.380 80 100 120 1<10 180

11me (a)

(b)

Fig. 7.13 Effect of Ti concentration on the Iiquidus portion of the cooling curve

for an AI 6%Si aUoy;

al Ti%= 0.008 L1T=1.23 D C

b) Ti%=0.076 L1T=0.56 D C•

0.55

• CHAPTERSEVEN

635 r------;::;;;;;:;:;:;;;:::::;;;;;;;:;-----1o.61 T~IUre :~s_U~ 1

138

630

6"e 625.aC1<IlC-E 620~

615

--------------------------------------- 0.5

0.35

610 L-~--_:_:~-~~-~~-~~--~---I0.360 80 100 120 140 160

Time (5)

(c)

635 ,-----;::;;;;:;;;;;:::;;;;;;----11 Te~IUre :~S-"~ 1

630

---------,-------------------------------6":... 625~

~:!l. 620E~

615

0.6

0.55

0.5

0.45i'~

~:l

'"III0.4 ~

Cl.

0.35

61040 60 80 100 120 140 168.3

Time (5)

(d)

Fig. 7.13 Cont'd

cl Ti%= 0.10 ~T=0.2°C

• dl Ti%=0.15 ~T=0.02°C.

• REsULTS AND DISCUSSION 139

refined and unrcfined 356 alloys is illustrated. It is seen that an undercooling of

about 2°C has accomplished and that the probe was sensitive enough to detect

the grain refinement effect on the cooling curve. AIso, the pressur~ inside the

chamber for both cases was identical. This was necessary to eliminate the effect

of cooling rate on chemical grain refinement. The total time consumed for this test

dealing with grain refinement was less than 4 minutes.

AIso, the same experiment as above was carried out on an aluminum

7%silicon alloy. The alloy was made artificially by melting pure aluminum and

adding a proper amount of silicon. Commercial grades of both aluminum and

silicon were used and the same procedure was followed except that the final

amount(0.24%) of grain refiner agent (Ti) was added in three steps. In each step

0.08% Ti was added, and t.'Je liquidus portion of the cooling curve was obtained.

The aim was to check the sensitivity of the probe to detect any minor changes on

the cooling curves due to the grain refinement treatment. Fig. 7.13 shows the

effect of various Ti additions on the liquidus portion of the cooling curve for an

aluminum 7%silicon alloy. The inner pressure was kept constant for all cases;

therefore, any changes on the curves are due to chemical grain refinement of the

alloy. To support this result, in each step a sample was taken from the melt and

solidified under the same conditions (i.e. the same amount, pouring temperature,

mold temperature etc.), and eventually four samples corresponding to curves (a),

(b), (c), and (d) in Fig. 7.13 were obtained. These samples were polished and

etched with Poulton's etch (60% HCl; 30% IIN03; 5% HF; 5% H20.) The

metallography results are presented in Fig. 7.14 to 7.17. As seen Ti is effective

in grain refinement.

The samples were also chemically analyzed for silicon and titanium by

vacuum emission spectrometry. AIthough during alloying 7% silicon was added

to pure aluminum, chemical analysis of the samples revealed that there was no

• CHAPTER SEVEN 140

Fig. 7.14 The microstructure of an unrefined AI-Si alloy of Fig 7.13 (a).

Fig. 7.15 The microstructure of a partially refined AI-Si alloy of Fig 7.13 lb: .

• REsULTS AND DISCUSSION 141

Fig. 7.16 The microstructure of a partially refined AI-Si alloy of Fig 7.13(c).

Fig. 7.17 The microstructure of the grain refined AI-Si alloy of Fig 7.13 (dl .

• Chapter Seven 142

Table 7.3 Summary of grain refinement results.

Ti cone. T 1 TT d 1 Avg. grain1 eonc. . U li, ercoo .

measured ~TCorresp.

sizetargetSample microst.

(%) (%) (OC) (mm)

Unrefined 0.00 0.008 1.23 Fig. 7.14 1.82

lit stage 0.08 0.076 0.57 Fig. 7.15 0.6

200 stage 0.16 0.10 0.2 Fig. 7.16 0.52

3n1 stage 0.24 0.15 0.02 Fig. 7.17 0.41

more than about 6% silicon in all the samp1es. Therefore, in an Al 6%Si alloy,

aeeording to the Al-Si phase diagram (Fig. 3.10), a higher liquidus temperature

030

Ô.... 625e.=I!u"-E 620

t!!-

.'5

.'0'" 60 60 100 120 14O 160 160

•Tine (.)

Fig. 7.18 Effect ofTi concentration on the Iiquidus portion of the cooling curve•

is expeeted. It can be clearly seen in Fig. 7.13a that the liquidus temperature for

• REsULTS AND DISCUSSION 143

the unrefined sample is about 621°C. Chemical analysis of the samples also

showed a lower Ti concentration level than the added amounts. A reason for this

can be incomplete stirring of the melt before sampling. Table 7.3 summarizes the

results of the grain refinement treatment including comparison of the target and

measured Ti concentration as weIl as the values of undercooling for primary

nucleation and the obtained average grain size of the samples. Finally, Fig. 1.18

groups all the cooling curves of Fig. 7.13 in orde!' to better illustrate the effect of

the grain refinement treatment.

7.2.2 Modification: The same materials, device and procedure as used in the

study of grain refinement were adopted to study modification. However, since

modification treatment targets the eutectic temperature on the cooling curve, a

lower (below eutectic) temperature was needed, and the eutectic part of the cooling

Fig. 7.19 The effect of modification on eutectic temperature of a 356 alloy,

~Un~ed Pressure(unmo<ified)

~-

Mo<ified Press~r.!l~ified) -~ ........f-

~-

!\ ---• .. . ........ ,1-' i -~ ...__...

0-

.. -- '..

'.

~- ... -.1- -.-.&-

............;..............................................................................

~ •.....: -, ,

610

605

600

595~

P~ 590e~ 585.,"- 580E~

575

570

565

56050 100

Tlme (5)

150

0.5

0.3 i~

e0.2 ~.,

~

Q.

0.1

0.05200

• Chapter Seven 144

curve was highlighted. Thus, a pressure ofabout 0.33 atm. inside the chamber was

imposed. In the first trial, a 356 alIoy was tested. Fig. 7.19 shows the effect of

about 200 ppm. strontium on the eutectic temperature. The master alIoy for

modification treatment was Al-lO%Sr. As shown by cooling curves obtained with

the thermosyphon probe, a lower eutectic temperature of about 4°C is the result

of modification. As before, this set of experiments was carried out at the same

pressures for both modified and unmodified melts.

The next step was to study the effect of the concentration of Sr modifier on

'" ~:===------------_.r-. J'"

.--~~:~.~ ~:;:;::=:.== -;----::-==:1~---_~_~ -_~~_~ u~»wu~~-_~~ • ç. .

- 1:'....ë':;.1fo1l."'!1'(,..~.~ .~~_ ~.. ".,......... - ... =:'~:. =-=.

,--_Urm_od_ilied 52_p_p_m__•.~_~_.~_~~_.•_. 1~: __~ ~~m ...J11 ~o.~mm·1600

596

592

588

E 584!!

~ 580l!-E 576~

572

568

564

56060 eo 100 120

lime (a)

140 160 100

Fig. 7.20 Effect of Sr concentration on eutectic temperature of a 356 alloy.

the eutectic temperature. The total amount of 200 ppm Sr was added in four stages

and cooling curves were obtained at each step. To assure complete dissolution of

the Sr, the liquid bath was he1d for about 20 minutes and then homogenized.

Because of the rapid thennal analysis method, no fading of modifiers during the

test was considered. Fig. 7.20 shows the cooling curves obtained with different

amounts of modifier. As the am~'unt of modifier was increased, the eutectic

temperature tended to a level of saturation. This phenomena is shown in Fig. 7.21

and is as expected. This confinns that the new method of thennal analysis is

completely reliable lUld can readily replace the conventional thennal analysis

method.

• REsULTS AND DISCUSSION 145

5 r---------------------.....,

Û 3•~l-

I

~ 2

Te : unmodlfied1

T: modlfied

4

0---'--........--'--"'---.......- .....-""--'--.......- .....- .......-..1o 50 100 150 200 250 300

Sr concentration (ppm)

Fig. 7.21 Effect of Sr content on eutectic temperature for 356 aUoy;

Te =eutectic temperature of the unmodified aUoy,

T=eutectic temperature of the modified aUoy.

The second series of modification tests was also carried out on a synthetic

aluminum-7%silicon alloy. Again, the total required amount (200 ppm) of

strontium was added in three steps (50, 50, and 100 ppm). For cach step the

cooling curve was obtained and a sample was taken. Samples were solidified under

• Chapter Seven 146

the same conditions (i.e. the same amount, pouring temperature, m01d temperature

etc.), in order to compare the changes in microstructure (eutectic silicon

morphology) and chemical compositions due to chemical modification treatment.

Fig. 7.22 illustrates the relevant portion of the cooling curves obtained in each

step. From this figure the depression of the eutectic temperature is seen. Figs.

7.23 to 7.26 show the micrographs of samples taken with various Sr levels. As

seen from the unmodified sample in Fig. 7.23 to the weIl modified sample in Fig.

57S

21018015012090

570L-_.....__.l...._........__...1.... .....l-__""-_--L__......._--J

6011me(o)

Fig. 7.22 Effect of graduai increase of modifier agent (Sr) on eutectictemperature of an AI-7%Si alloy.

7.26, the very long, coarse, and needle shape eutectic silicon becomes fragmented,

fine, and fibrous by the graduai addition of Sr. This is indicating a successful

silicon modification treatment. However, again chemical analysis of the samples

yielded lower silicon and strontium contents than the target amounts. According

to chemkal anaIysis, the silicon content of the samples was about 6% while 7%

• REsULTS AND DISCUSSION

Fig. 7.23 The microstructure of an unmodified AI 6%Si alloy.

147

• Fig. 7.24 The microstructure of an AI 6%Si alloy modified by 40 ppm Sr.

• CHAPTER SEVEN 148

Fig. 7.25 The microstructure of an AI 6%Si alloy modified by 85 ppm Sr.

Fig. 7.26 The microstructure of an AI 6%Si alloy modified by 130 ppm Sr.

• REsULTS AND DISCUSSION 149

Si level was expected. Table 7.4 summarizes the results of modification treatment

including comparison of the target and measured Sr concentrations as well as the

eutectic temperature of the samples.

In summary, it has been shown that grain refinement and modification of

aluminum-silicon alloys can be successfuIly trace<! using the newly developed

thermosyphon probe. The probe is sensitive enough to detect changes in the

cooling curve caused by standard industrial melt treatments.

Table 7.4 Summary of eutectic modification results.

Sr conc. Sr conc. Eutectic Corresp.

Samp1e target measured temperature microstructure.

(ppm) (ppm) ("C)

Unmod. 0 <20 579.2 Fig. 7.23

1" stage 50 40 577.8 Fig. 7.24

2ad stage lGO 85 577.1 Fig. 7.25

3'" stage 200 130 576.5 Fig. 7.26

cHAPmR8

CONCLUSIONS

8.1 Concluding Remarks

A new method of thermal analysis of aluminum silicon casting alloys has

been developed. The method takes advantage of the heat pipe for its ease of use,

its wide range of operation, and its sensitive control on the heat transfer rate

during solidification of a sample. The main steps in the development of the new

method were: the definition of the problem regarding the conventional thermal

analysis limits on the one hand and the advantages of utilizing a heat pipe based

probe 0,' the other; the design of the proper heat pipe; the manufacture of the

designed heat pipe probe on a laboratory scale and the mathematical modelling of

the process. Finally, the probe was tested to examine its defined features, and

sorne routine treatments such as grain refinement and modification were evaluated.

The experimental work focused on both pure aluminum, and 356 and 413

alloys in order to coyer hypoeutectic and eutectic aluminum-silicon alloys. The

effect of various cooling rates on the cooling curves was investigated for pure

aluminum, 356 and 413 alloys. In the pure aluminum case, it was shown that the

probe had the abilil'y to cool the superheated liquid aluminum sample down to the

• CONCLUSIONS 151

melting point and to keep its temperature at the melting point for a long period of

time by establishing a dynamic thermal equilibrium between heat gained by and

lost from the sample. Grain refinement and modification treatments were done on

356 alloy by the probe. A gradual decrease in the apparent supercooling for

nucleation by an increase in titanium concentration (as the inoculating agent) was

detected. This observation showed that the probe was sensitive enough to detect

any fine changes in liquid metal chemistry through grain refinement. AIso, eutectic

modification of a 356 alloy was extensively investigated and a gradual depression

of eutectic temperature by a gradual increase of strontium concentration (as the

modifier agent) was observed. A non linear relation between the strontium

concentration and eutectic temperature depression was also observed (Fig. 7.21)

The results are presented semi-quantitatively in this thesis, however, it is

realized that, by perfecting the method (the next generation of the probe), it can

he used to obtain fully quantitative results (see 8.3). During the course of this

work and based on the probe principles, it was noted that the key advantage of the

new thermal analysis method was the high controllability of the heat transfer rate

by the system over the conventional method. This feature enabled the system to

simulate different solidification rates for the same bath of liquid metal (sample),

and, in turn, revealed the importance of the inside pressure and its changes during

the experiment.

The mathematical model was found to be useful and precise to simulate the

heat transfer behaviour of a solidifying sample. Since a number of variables (such

as inside pressure, bath temperature, location of thermocouple in the sample, the

working substance material etc.) were involved with solidification, the model was

used for recognizing the optimum combination of these variables for a certain

application. AIso, the model enabled the estimation of solidification rate with

respect to inner pressure of the probe, a factor that was impossible to measure in

• CHAPTER EIGHT 152

practice.

In summary, the designed probe, which is agas loaded annular

thermosyphon, is found to be completely workable under the defined conditions

for thermal analysis of aluminum alloys. The results of thermal analysis with this

new technique are in good agreement with those of conventional thermal analysis.

Furthermore, the new method is amenable to a wider range ofo~ratingconditions

and is easier to use. Unlike the conventional method this new technique does not

need pre-preparation (materials, labour, pre-heating, thermocouple installation,

isolation of the sampling cup, etc.) to start thermal analysis. From a cooling rate

point of view, the system is easily controlled by adjusting the pressure inside the

probe to yield a spectrum of cooling rates which are readily available with the

same set up and for the same bath of liquid metal.

8.2 Claims to Originality

To the author's knowledge this project has resulted in several original

contributions to the prior art. Development of a novel thermosyphon in order to

innovate a new thermal analysis method for aluminum alloy melts forms the

original body of this work. The worldwide patent review on heat pipe applications

from 1950 to present showed no similar work among those of about five thousand

hell.t pipe applications.

Specific original contributions made in the present work may be summarized

as follows:

•1. The same sample can be solidified over a wide range of cooling rates with

no need for extra devices. In fact, t.ie probe has been designed such

that with a constant heat source temperature, different heat dissipation rates

cao be acbieved.

• CONCLUSIONS 153

2. Th..: continuous nature of this new method of thermal analysis is original.

The author is not aware of any other device whereby thermal analysis of the

melt is carried out in-situ with a rC:Jsable probe. Moreover, in-situ

remelting of the sample once solidified is a key feature, never reported in

the literature.

3. With this new method, a liquid sample can be cooled down to a certain

temperature and kept at that temperature for a long time (see Fig. 7.4).

4. The use of the latent heat of vaporization/condensation of the working

substance to extract the sensible and latent heats of fusion during

solidification of a melt sample is an original concept. In other words, for

the fust lime, solidification and melling have been coupled with heat pipe

technology.

5. The ability of the thermal analysis method to be fully automated and

computerized was considered as a high technology quality control tool.

6. The thermal analysis method was also novel by its nature of recycling the

solidified sample to the system.

8.3 Future Studies

According to the present work, the applicability of the novel idea of this

new thermal analysis method has been proven. The author believes that a wide

range of research can be defined based on the context of this work. Two possible

area of future work are: studies on new and different heat pipe applications in

foundry technology with the same design fundamentals as the present heat pipe

probe. In this case, an equivalent probe may be developed to be used in the

thermal analysis of cast iron melts. At present, thermal analysis of cast iron is a

weil established method for evaluation of carbon equivalent and for prediction of

• CHAPTER EIGHT 154

graphite morphollJgy. Secondly, future studies should be carried out on the

evolution of the developed method in order to upgrade the probe.

In terms of these future studies, the fust step would be to improve the

probe's 'intelligence', that is, to computerize the method of pressure adjustment

feed back with temperature. With such a system the following investigations are

proposed:

1. Quantification of cooling rate~ versus the inside pressure of the probe. The

output will then be a correlation of pressure and cooling rate for a given

working substance and aluminum alloy.

2. Quantification of silicon modification for the common aluminum-silicon

casting alloys as was done in this work.

3. Quantification of grain refinement for the alloys that are regularly refined

in practice. The result will be a correlation between the quantity of

undercooling for nucleation versus grain refiner concentration. This

standard correlation will be the source of evaluation of grain refinement

level in a similar melt with an unknown concentration of grain refiner

material.

4. Study of minor reactions occurring during solidification of the alloy. For

example, in 356 alloy due to the minor presence of iron, magnesium, and

copper in the melt chemistry, sorne post-eutectic reactions occur and SO'~le

intermetallic compounds form during solidification. Since these reactions

are normally exothermic, they affect the co,.,Hng curve and appear as small

peaks after eutectic solidification is comf>.~,e. 7 The procedure will be such

that fust the pressure is set f\JI a fast cooling rate to pass the unwanted

portions of the cooling curve and then, only before the reactions take place,

the pressure is reduced such that the cooling curve proceeds very slowly.

Therefore, the heat consumed (or produced) during the formation of

• CONCLUSIONS 155

intermetallic compounds will be magnified on the relevant portion of the

cooling curve.

5. Study of optimum amount ofgrain refiner and modifier agents for complete

grain refinement and eutectic modification treatments. In fact, the

architecture of the probe is such that it makes a perfect device for studying

the fading phenomena in grain refinement and modification.

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• BmUOGRAPHY 157

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• BmUOGRAPHY 158

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• BmUOGRAPHY 159

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