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The world of X-ray diffraction is no longer flat EMPYREAN The Analytical X-ray Company

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Page 1: EMPYREAN: THE WORLD OF X-RAY DIFFRACTION IS NO LONGER FLATanalytical.ru/empyrean.pdf · analytical software suite ... SAXS XRD 108 106 104 0 10 20 30 40 50 60 70 80 0 0.05 ... THE

1

The world of X-ray diffraction is no longer flat

EMPYREAN

The Analytical X-ray Company

-6000 -4000 -2000 0 2000 4000 600010

100

1K

10K

100K

1M

10M

100M

Omega/2Theta [s]

Inte

nsi

ty [

cou

nts

]

Position 2Theta [deg.] (Copper (Cu))

Inte

nsi

ty [

cou

nts

]

4000

3000

2000

1000

020 30 40 50 60 70 80 90 100 110 120 130 140

Inte

nsi

ty [

cou

nts

]

2000

1000

0

21 21.20 21.40 21.60

Position 2Theta [deg.] (Copper Cu))

FWHM = 0.026 °2θ

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Pioneering X-ray diffraction

PANALYTICAL

Truly innovative, daringly different, Empyrean brings the idea of a

perfect XRD platform to life

The new Empyrean from PANalytical

PANalytical, formerly known as Philips Analytical, has a rich history of innovation in X-ray analysis.

Philips starts to repair and

manufacture X-ray tubes in Eindhoven

First X-ray diffractometer with Geiger-Müller counter tube

First goniometer, based on Direct Optical Position

Sensing (DOPS)Invention of PreFIX optics. Introduction of X'Pert MRD

Introduction of the X’Celerator detector, the world’s first solid state 1D detector

Introduction of the PIXcel detector, based on Medipix2 technology

PIXcel

The world’s first commercially

available X-ray diffractometer

PW1050 X-ray diffractometer and PW1520, the world's first commercially available X-ray fluorescence spectrometer

APD1700: first complete analytical software suite

X’Pert PRO MPD. PreFIX for powder diffraction

X’Pert MPD, the first multi-purpose powder diffractometer with flip-focus tube

First thin film diffractometer with four-bounce (Bartels) monochromator

First X-ray diffractometer with Geiger-Müller

First goniometer, based on Direct Optical Position

Sensing (DOPS)

flip-focus tube

PreFIX for powder diffraction

X’Pert MPD, the first multi-purpose powder diffractometer with flip-focus tube

Introduction of the

Introduction of the PIXcel detector, based on Medipix2 technology

In developing Empyrean, PANalytical has redesigned many of the key parts of the XRD platform from the ground up.

The X-ray source, the goniometer, the sample stages and the detection system are all brand-new. Such innovation comes to the market just once in a gen-eration and sets the benchmark for oth-ers to follow. Empyrean not only meets the high expectations of scientists and XRD experts today, but will continue to do so as research themes evolve. The world of materials science is constantly changing and the life of a high perform-ance diffractometer is much longer than the typical horizon of any research project. With Empyrean, you are ready for anything the future holds.

One platform, one instrument, no compromise in data quality whatever the application

The widest sample range

The highest performance goniometer

Exceptional tube performance

Proven PreFIX pre-aligned optics

The widest range of sample stages and non-ambient environments

Easy access for fast reconfiguration

Unmatched 2D detector dynamic range, linearity and resolution

The world’s first 3D detector

Flexible, high-performance software packages

Established PANalytical support

Introduction of

Truly innovative, daringly different, Empyrean brings the idea of a

perfect XRD platform to life

The new Empyrean

Introduction of PIXcel3DIntroduction of

1917

1945

1954

1990

1990

1999

20062006

2001

2010

1993

1995

1983

19481948

The only XRD platform that does it allThe only XRD platform that does it all4

Sample types

6Powders

8Thin films

10Nanomaterials

12Solid objects

14Innovation in

every area

16PIXcel3D -

cutting-edge technology

18Partnership with PANalytical

- ultimate commitment

What’s in a name?The term Empyrean is derived from Aristotelian cosmology (384 -322 B.C.) in which spherical earth was surrounded by concentric celestial spheres containing the moon and known planets1. The highest sphere, later referred to as Empyrean in the Middle Ages, is represented by the element ‘fire’. The Empyrean XRD system is the product of the fire of innovation, and is truly above all others, capable of the most analytical applications on a single XRD platform.1. G. E. R. Lloyd, Aristotle: The Growth and Structure of his Thought, Cambridge: Cambridge Univ. Pr., 1968, pp. 133-139, ISBN 0-521-09456-9.

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The only XRD platform that does it all Empyrean delivers the best quality data, whatever your sample type and experience

EMPYREAN

• What is in my sample? - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

• In which ratios? - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

• What is the amorphous content? - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

• What is the crystal structure? - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

• Can I see preferred orientation? - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

• What is in my well plates? - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

• Influence of temperature, pressure, humidity? - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

• What is in my nano-powder? - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

• What is the particle size distribution and specific surface? - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

• What is the average crystallite size and defect density? - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

• Are my powders truly crystalline? - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

• Is my sample amorphous or nano-crystalline ? - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

• How do my samples crystallize? - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

• Influence of temperature, pressure, humidity? - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

• What is in my layer(s)? - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

• What is the layer thickness, roughness and density? - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

• Is there residual stress? - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

• Is there preferential growth? - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

• Can I get information about in-plane reflections? - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

• Is the layer (hetero)epitaxial? - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

• Is the layer strained or relaxed? - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

• Influence of temperature? - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

• Can I evaluate the internal (micro-) structure of my sample? - - - - - - - - - - - - - - - - - - - - - - - - - - -

• What is in my sample? - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

• What is in that spot? - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

• Did machining induce preferred orientation? - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

• Is residual stress present? - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

• Influence of temperature, pressure, humidity? - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

• Phase identification

• Phase quantification

• Crystallinity determination

• Structure determination and refinement

• Direct visualization of Debye rings

• High-throughput screening (HTS)

• Behavior under non-ambient conditions

• Phase identification

• Small angle X-ray scattering (SAXS)

• Crystallite size and micro-strain analysis

• Amorphous content determination

• Pair distribution function (PDF) analysis

• In situ crystallization analysis

• Behavior under non-ambient conditions

• Phase identification (and depth profiling)

• X-ray reflectometry

• Thin film stress analysis

• Texture analysis

• In-plane diffraction

• Epitaxy analysis

• Reciprocal space mapping

• Behavior under non-ambient conditions

• Computed tomography (CT)

• Phase identification (also in transmissiongeometry)

• Micro diffraction

• Texture analysis

• Stress analysis

• Behaviour under non-ambient conditions

Sample type Analytical question Application Example Typical resultconfiguration

0

0.05

0.10

0.15

0 5 10 15 20

Dv

(R)

R [nm]

5 nm

8 nm 14 nm

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Direct visualization of Debye rings

Every Empyrean equipped with a PIXcel3D detector is capable of 2D diffraction. 2D diffraction patterns show if a sample is fine-grained enough to produce the solid Debye rings characteristic of a randomly oriented sample (a), or is medium to coarse-grained, producing spotty Debye rings (b and c).

Powders – data that speaks for itself

EMPYREAN

Empyrean offers you a platform to measure and identify the most complex phase mixtures. The sensitivity of the instrument and the power of the software to deal withoverlapping patterns is unmatched.

Empyrean has the highest angular resolution of any laboratory powder diffractometer and delivers data closest to synchrotron quality.

Empyrean offers the widest range of non-ambient environments, under full control of the instrument software.

Empyrean is ideal for teaching purposes. It offers all relevant diffraction geometries (reflection, transmission, capillary, micro-diffraction, Debye-Scherrer) and is supported by the most comprehensive set of worked examples.

Low-angle diffraction from dry rat tail tendon collagen fibers as a function of their orientation.When the fiber axis is oriented perpendicular to the incident beam (dark blue line) equidistant meridional reflections due to the characteristic collagen molecule arrangement along the fiber axis can be clearly observed. The data shown in the insert was taken by using a hybrid monochromator for best low-angle resolution. The first diffraction peak, corresponding to a Bragg spacing of 650 Å, is readily resolved. When the fiber is oriented in parallel to the incident beam (equatorial orientation), no such peaks are observed (light blue line).

Structure solution of fayalite by a difference Fourier map - known structure is overlayed.

Charge-flipping is a fast ab initio structure solution method Developed for single crystal data in 2004, it was extended for powder diffraction measurements later and is now used successfully for both small and large, inorganic and organic structures. A difference Fourier map offers an alternative way to locate (heavy) atoms in an unknown structure.Both methods provide a 3-dimensional electron density map for evaluation.

Rietveld standardlessstandardless quantitativeanalysis has become an important analysis has become an important method for characterizing complex method for characterizing complex mixtures.

Inte

nsi

ty [

cou

nts

]

2Theta [deg.]

105

105

104

104

1st

1st (d = 650 Å)

2nd2nd

3rd

4th5th

6th

7th 8th 9th

10th 11th

12th13th

14th103

0.5

0.1 0.2 0.3

1.0 1.5 2.0

Color-coded display of samples on a well

plate with similar composition or

mixtures

6 8 10 12 14 16 18 20 22 24 26 28

0

10000

20000

30000

40000

50000

60000

70000

Inte

nsi

ty [

cou

nts

]Te

mp

erat

ure

[ °

C]

2Theta [deg.]

Relative humidity [%rH]

RH = 1 %rH; Anhydrate + Dihydrate + Amorphous content

RH = 20 %rH; Amorphous

RH = 40 %rH; Recrystallization into another phase

RH = 60 %rH; Recystallized

RH = 80 %rH; Again a phase change

100

80

60

40

20

00 50

80 °C

95

Full pattern quantification

Non-ambient analysis

Structure determination and refinement

High-throughput screening

Transmission diffraction

α, α, α α- Trehalose-dihydrate measured at 80°C in an Anton Paar CHC plus+

temperature-controlled humidity chamber: with increasing relative humidity several phase transitions can be observed.The upper graph shows the temperature-controlled humidity range that can be used with the system.

The analysis of powders and polycrystalline materials is probably the most common application of XRD.

a)

b)

c)

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Thin films – data that speaks for itself

EMPYREAN

Diffractometers for the analysis ofthin films have typically been highly specialized for this purpose. Now, with Empyrean, the demand for high- resolution epitaxy analysis has been combined with the advantages of a multi-purpose vertical diffractometer to offer you the largest range of analyses on one system.

Empyrean is the perfect analysis tool to place next to your layer growth equipment.The new Empyrean cradlesallow you to fully map wafers and wafer fragments up to 2 inches, and handle up to 4-inch wafers.

Analysis of a polycrystalline Fe3N/Fe4N coating on steel. The stress measurement was performed in grazing incidence. Repeated measurement with different grazing incidence angles allow to probe for the possible existence of a stress gradient.

Fast reciprocal space map on a Si/SiGe sample measured with a scanning PIXcel detector. Speed gain about a factor of 10 compared to usual setup

Comparison of the rocking curve performance of different incident beam monochromators on a periodic epitaxial multilayer around the InP (004) reflection. Differences in resolution and intensities are obvious. A range of modules is available that offer a range of angular resolutions matching any analytical need.

NbAl thin film multilayers grownon sapphire and silicon substrates show fiber texture. Reflectivity and wide angle scanning provide information in just 5 minutes. Reflectivity gives data about multilayer thickness and interface roughness. Wide angle scanning can be supported with texture studies using pole figures and or 2theta/omega scans at different omega offsets. Note that the Nb(121) reflection, for example, is absent from the symmetric scan but can be observed with omega offset of 30°. A pole figure shows the Nb(121) reflection as a ring also illustrating that the film orientation israndom in-plane.

Reciprocal space mapping

Reflectometry and texture analysis

Epitaxy analysis Phase identifications, stress analysis and depth profiling

30 40 50 60 70 80 90 100 110 120 130 1400

10000

20000

Fe4

N, F

e 3N

Fe4

N

Fe4

N

Fe4

N

Fe4

N

Fe4

N

Fe4

N

Fe3

N

Fe3

N

Fe3

N

Fe3

N

Fe3

NFe

3 N

Fe3

N

Fe3

N

Inte

nsi

ty [

cou

tns]

Position 2Theta [deg.] (Cobalt (Co))

0 2 4 6 8 10

500

250

0

-250

-500

-750

-1000

Grazing incidence angle [deg.]

Stre

ss [

MPa

]

Fast reciprocal space map on a Si/SiGe sample measured with a scanning PIXcel detector. Speed gain about a factor of 10 compared to usual setup

Empyrean offers it all:

• quality inspection of incoming(powdered) materials and substrates

• depth profiling using grazingincidence geometry

• analysis of the thickness androughness of single- or multi-layer systems with X-ray reflectometry (XRR)

• orientation analysis ofpolycrystalline layers

• in-plane diffraction

• determination of residual stressesin layers and coatings

• epitaxy analysis using rockingcurves and reciprocal space maps

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Nanomaterials – data that speaks for itself

EMPYREAN

Empyrean supports many X-ray techniques for the analysis of nanomaterials, whether for thin films, powdered substances or slurries.

The unique properties of nanometersized materials have inspired the research community for the last decade.

For the analysis of nanoparticle size, shape, specific surface area or dilute dispersions, EasySAXS, PANalytical’s small angle X-ray scattering (SAXS) application, is designed for ease of use. The size of crystalline domains within nanomaterials can be obtained from the line profile analysis within HighScore(Plus). Structure analysis of amorphous or nano-crystalline materials can be undertaken with pair distribution function (PDF) analysis.

The large range of non-ambient environments available for the Empyrean can also be used beneficially for synthesizing and characterizingnano-materials. For example, the sintering of nano-particles as a function of temperature, be it in air, vacuum or other gasses, can be observed. Catalytic activity, under gas pressures up to 100 bar, can be studied. For all these applications Empyrean allows users to pick and place the right PreFIX X-ray components to give the best results.

95 % anatase 5 % rutileIn

ten

sity

2 Theta [deg.]

SAXS XRD

108

106

104

0 10 20 30 40 50 60 70 80

0

0.05

0.10

0.15

0 5 10 15 20

Vo

lum

e d

istr

ibu

tio

n D

v (R

)

Particle radius R [nm]

5 nm

8 nm 14 nm

4040

Qmax=21Å-1 (Ag)

Qmax=17Å-1 (Mo)

Qmax=7Å-1 (Cu)

14 16 18 20 22 24 26 28 30

20000

0

40000

60000

80000

100000

120000 [210]

[002]

Inte

nsi

ty [

cps]

2Theta [deg.]

pH 6 - 50 hpH 6 - 40 hpH 6 - 30 hpH 6 - 20 hpH 6 - 10 h

Analysis of multi-modal size distribution with SAXS

Pair distribution function (PDF) analysis

Crystallite size and microstrain analysis

In situ crystallization monitoring

Phase identification and Small-Angle X-ray Scattering (SAXS)

Combined XRD and SAXS measurement on nano-titania.Besides anatase, the phase analysis indicates low amounts of rutile in the material (small peaks marked by arrows). The very broad diffraction peaks of the anatase phase indicate a small crystallite size, as can be expected for a nanopowder sample.The SAXS signal can be used for the determination of the size distribution of the nanoparticles

PDF analysis is preferably performed with high-energy radiation. Every Empyrean supports the use of Mo or even Ag radiation, with slit optics or dedicated mirror optics. The graphs show that the use of longer-wavelength radiation significantly reduces the quality of the experimental PDF. Results obtained with Ag radiation on Empyrean compare very well with beam line experiments.

PANalyticals EasySAXS software allows the analysis of multi-modal size distributions without a priori assumptions about the type of distribution. Here a tri-modal particle size distribution of a dilute silica dispersion

On-line investigation of DL-alanine crystallization at pH 6 measured in

a slurry flow cell installed on the Empyrean.

After a starting crystal growth withpronounced peaks at the [311] and

[002] reflections, the crystals starts to grow stronger in the [210] direction

after around 38 hours.

Crystallite size and microstrain analysis

Information on the microstructure of crystalline materials (crystallite size and microstrain; also known Information on the microstructure of crystalline materials (crystallite size and microstrain; also known Information on the microstructure of crystalline materials (crystallite size and microstrain; also known as size-strain analysis) is obtained from the width and the shape of X-ray diffraction peak profiles. HighScore (Plus) can calculate size and strain information for each diffraction peak.The screen shot also shows the Williamson-Hall plot giving the average size and strain results.

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Solid objects – data that speaks for itself

EMPYREAN

Sometimes samples must be analyzed without any sample preparation.

Examples are widespread: • geologicalsamples• pharmaceuticaltablets• engineeredcomponentssuchasball

bearings, joints and axles

Empyrean can handle all of these samples.

For the phase identification of roughand irregularly shaped objects, parallel beam geometry is often used.PANalytical’s philosophy for this geometry is consistent with all our set-ups - optimize, not compromise.

Empyrean can also analyze large and heavysamplesupto10kg,auniquecapability for a flexible multi-purpose X-ray system. The 3-axes Empyrean cradle allows you to mount components of up to 2 kg, and perform preferred orientation (texture) and residual stress using the chi-tilt or omega-tilt method.

AfurtheruniquepossibilitywithEmpyrean is to see inside small solid objects without having to cut them.

Computed tomography (CT) analysis determines the area of interest for subsequentX-raydiffractionanalysis,orcan be used to check for the presence of pores.

Typical ECAP-processed sample and pole figures determined for three different reflections

2Th

eta

[deg

.]

sin2 [Psi]

124.2

124.0

123.8

123.6

123.4

123.20.0 0.1 0.2 0.3 0.4 0.5 0.6

Stress: -470.1 ± 34.0 MPaPhi = 0.0°

Inte

nsi

ty [

cou

nts

]In

ten

sity

[co

un

ts]

Without glass

With glass

2Theta [deg.]

2Theta [deg.]

18 19 20 21 22 23 24 25 26 27 28 29 30

2500

10000

22500

40000

18 19 20 21 22 23 24 25 26 27 28 29 30

2500

10000

22500

40000

Portlandite

Portlandite

Calcite

Quartz

Calcite

Quartz

In this example two concrete samples with different properties are shown. The X-ray patterns on the right show a clear presence of Portlandite and a reduced amount of calcite in the upper sample (prepared with glass). The other sample shows a significantly lower amount of Portlandite and an increased amount of calcite (sample prepared without glass). This can be explained by the microstructure that is visualized by CT: The upper sample shows a more dense microstructure inhibiting carbonatization whereas the other sample shows more pores and cracks that allow for a stronger carbonatization – affecting the long term stability.

Stress analysis

Radiography, computed tomography and microdiffraction

Texture analysis

Computed tomography and phase identification

Empyrean offers unrivalled possibilities for non-destructive analysis on natural or historical objects. As example we analyzed a river shell combining CT and XRD data:The radiograph on the right side exhibits some voids in the shell that are not visible from the outside. The CT reconstruction of the shell (middle) allows in addition slicing the shell in planes and analyzing the structure in more detail. At the position of the arrow (connection of the shell muscle) – also marked in the picture by the green spot - an analysis of the aragonite phase orientation has been performed: The strong preferred orientation of the aragonite is easily visible in the 2D diffractograms measured with small variation in the orientation of the shell (three arrows).

Stress measurement was made on an inner ball bearing ring probing the bottom of the raceway. The graph shows the sin2ψ plot of the data determined in raceway direction.

Texture analysis of aluminium processedbyequalchannelangular pressing (ECAP) – an effective method to reduce grain size and enhance mechanical properties of metals and alloys.

CT can be used to visualize the fabric, defects and inclusions of a sample. The density of the sample can be obtained and differences can be calculated. This provides a valuable new tool for researchers and gives new possibilities for the interpretation of the XRD data. Especially the combination from 1D and 2D diffraction information with 3D–CT supplies the first time a complete picture of the sample.

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Cutting-edge technologyin every aspectCutting-edge technology

EMPYREAN

In order to make the ultimate X-ray diffractometer for powders, thin films, nanomaterials and 3D objects, all essential components have been newly developed by our experienced R&D team.

PANalytical’s PANalytical’s Empyrean Tubes: robust : robust exchange of exchange of tube focus tube focus position and position and largest variety largest variety of tube anode of tube anode materials

A heart with a brain

The heart of the Empyrean is a new revolutionary high- resolution goniometer evolving upon a long PANalytical tradition in precision goniometers. It makes use of the next generation of Direct Optical Encoding System (DOPS2), featuring precisely aligned Haidenhain encodersand Path Tracking Technology (PTT) for continuous advanced motion control based on Digital Signal Processing (DSP). Due to this advanced motion control the goniometer offers highest resolution and differential accuracy and positions its arms faster and more precisely than ever before.

9

21

4

6

7

7

3

8

5

• Compact 5-axes ¼-circle cradle• Compact 3-axes ¼-circle cradle,

capable of holding samples up to 2 kg• CT sample spinner stage• Computer-controlled height

alignment and temperature-compensating stage for non-ambient chambers

• All sample stages are interchangeablein minutes

• All large stages and non-ambientchambers can be completely removed from the system – without power-down

1

New, unique sample stages

The unique PiXcel3D detector, co-developed with CERN and

other leading European scientific institutes - more on next pages

Comprehensive software suite for data collection and

analysis. Supports multiple users, unattended and remote operation, and automatic data collection, analysis and reporting.

Universal PreFIXThe Empyrean system is

equipped with universal PreFIXoptics, stages and accessories, PANalyticals proven proprietary kinematic mounting concept for Pre-aligned Fast Interchangeable X-ray modules. The robust hardened tool steel mounts allow a reproducible positioning of optics and stages in three dimensions with microns precision eliminating any need for re-alignment.

4

3

8

7

The world’s most accurate high-resolution goniometer

Step size 0.0001°, 2θ linearity ±0.01°.

"We combined long-time experience and the latest technology to make a high-performance workhorse with ultimate flexibility for today's and future applications".

0

1000

2000

Inte

nsi

ty [

cou

nts

]

Position [°2Theta] (Copper (Cu))

21 21.20 21.40 21.60

LaB6 Alpha-1 Empyrean LaB6 standard Empyrean

FWHM = 0.026 °2θ

Empyrean sets the new bar for laboratory X-ray system resolution, with a FWHM of 0.026 degrees 2-theta for the first reflection of NIST SRM660a LaB6.

9

2

Meets all relevant world wide regulationsworld wide regulations,

for X-ray, electrical and mechanical safety

5

other leading European scientific institutes - more on next pages

Meets all relevant world wide regulationsworld wide regulations

for X-ray, electrical and mechanical safety

5

19” rack mounts

for non-ambient controllers and integrated vacuum system

6 Enclosure is on wheels for

easy installation and relocation

7

Wide opening cabinet gives easy access to the

experimental area

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The introduction of PIXcel3D adds a new dimension to XRD analysis. This unique photon counting detector isthe most advanced in the world. The combination of high spatial resolution with no point spread function, highest dynamic range and low noise sets a new standard of performance. In addition, the 2D scanning possibilities of this detector make it the most versatile ever to be available on a commercial diffractometer.

PIXcel3D is the result of PANalytical’s partnership in the Medipix2 collaboration – a consortium of more than 16 leading particle physics research institutes across Europe, headed by CERN. As state-of-the-art detector developments have become more complex, only the largest groups active in fundamental research can deal with the planning and investment involved.

PANalytical is an industrial partner to this collaboration and has secured the exclusive rights to commercialize the resulting technology for analytical X-ray applications, putting you at the forefront of detector developments for many years to come.

PIXcel3D - cutting edge technology

A strong partnership with CERN

Detector mode PIXcel and PIXcel3D Typical applicationsadvantages

0D mode: All pixels are added up to give one intensity value as a function of time

Rocking curve on epitaxial layer structure without the need for a beam attenuator

The point detector with the highest dynamic range, highest maximum count rate and lowest background

The line detector with the highest dynamic range and the smallest strip size

1D mode: All pixels in one column are added up to form a position-sensitive detector in one direction

LaB6 measurement 6 measurement 6in Bragg-Brentano geometry and with alpha-1 Johansson monochromator

2D pattern of coarse aspirin

The area detector combining the advantages of highest spatial resolution, high dynamic range per pixel and low noise - not requiring any calibration

2D mode*: All pixels are read out independently: direct observation of the X-ray image

3D mode*: All pixcels are read out independently: many 2D images are combined to reconstruct the voxels of the object: computed tomography

CT reconstruction of pharmaceutical capsules in the original blister package, virtual dissection

The computed tomography

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Position 2Theta [deg.] (Copper Cu))

FWHM = 0.026 °2θ

3D mode*: All pixcels are read out independently: many 2D images are combined to reconstruct the voxels of the object: computed

The computed tomography detector with the smallest pixel size and the highest dynamic range

“The Medipix2 chip technology, combines high spatial resolution, high dynamic range and low noise. The Medipix2 Collaboration is happy that this leading-edgetechnology is being exploited by PANalytical for materials analysis.”

M. Campbell, Spokesman, Medipix2 Collaboration

“PANalytical adopted the technology early and has been an invaluable Technology Transfer partner for CERN and the Collaboration.”

B. Denis, CERN Technology Transfer

* only available on PIXcel3D

Compact, smart and powerful 2D XRD … and more

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Partnership with PANalytical - ultimate commitment

Extending your capabilities

Expert to expert

In the know

Your decision to invest in Empyrean marks the beginning of a relationship that will last for many years. A critical goal in our development of Empyrean was to do more than provide a solid platform for each user to build their perfect XRD system. Together with our technical specialists and applications scientists, each diffractometer will be developed into the perfect instrument for your analysis needs. Your input guides our development efforts, and jointly we will get the most information out of your challenging materials.

PANalytical customers know

Almost 80 % of the world's top 50 universities* are customers and development partners of PANalytical.

*www.usnews.com/articles/education/worlds-best-universities/2009/10/20/worlds-best-universities-top-200.html

PANalytical’s track record of adding new technology and new applications to existing systems is unrivalled, thanks to consequent use of PreFIX modules over many years. Empyrean will build on this heritage.

This page shows a few examples of the technologies we are working on for further expansion of Empyrean's capabilities:

• Multi-segment, solid-state pixeldetectors

• Evacuated beam path for SAXSmeasurements on diluted samples

• Microfocus X-ray sources and optics

Training courses, instrument familiarization sessions, application workshops and remote learning channels provide important information for new and existing users. PANalytical facilities around the world deliver these, alongside more general scientific meetings on a variety of X-ray diffraction and scattering topics.

Assembly of four PIXcel3DAssembly of four PIXcel3DAssembly of four PIXcel detectors (Quad)

Artist‘s impression of evacuated beam path - SAXS

Extending your capabilities

PANalytical’s track record of adding new technology and new applications to existing systems is unrivalled, thanks to consequent use of PreFIX modules over many years. Empyrean will build on this

This page shows a few examples of the technologies we are working on for further expansion of Empyrean's

pixel

SAXSmeasurements on diluted samples

optics

Microfocus X-ray source

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PANalyticalPANalytical is the world’s leading supplier of analytical instrumentation and software for X-ray diffraction (XRD) and X-ray fluorescence spectrometry (XRF), with more than half a century of experience. The materials characterization equipment is used for scientific research and development, for industrial processcontrol applications and for semiconductor metrology. PANalytical, founded in 1948 as part of Philips, employs around 900 people worldwide. Its headquarters are in Almelo, the Netherlands. Fully equippedapplication laboratories are established in Japan, China, the USA, and the Netherlands. PANalytical’s research activities are based in Almelo (NL) and on the campus of the University of Sussex in Brighton (UK). Supply and competence centers are located on two sites in the Netherlands: Almelo (development and production of X-ray instruments) and Eindhoven (development and production of X-ray tubes). A sales and service network in more than 60 countries ensures unrivalled levels of customer support. The company is certified in accordance with ISO 9001:2000 and ISO 14001.

The product portfolio includes a broad range of XRD and XRF systems and software widely used for the analysis and materials characterization of products such as cement, metals and steel, nanomaterials, plastics, polymers and petrochemicals, industrial minerals, glass, catalysts, semiconductors, thin films and advanced materials, pharmaceutical solids, recycled materials and environmental samples.

Visit our website at www.panalytical.com for more information about our activities.

PANalytical is part of Spectris plc, the precision instrumentation and controls company.

PANalytical B.V.Lelyweg 1, 7602 EA AlmeloThe NetherlandsT +31 (0) 546 534 444F +31 (0) 546 534 [email protected]

Regional sales offices

AmericasT +1 508 647 1100 F +1 508 647 1115

Europe, Middle East, AfricaT +31 (0) 546 834 444 F +31 (0) 546 834 499

Asia PacificT +65 6741 2868 F +65 6741 2166

Global and near

ed t

o im

ply

an

y PANalyticalPANalytical is the world’s leading supplier of analytical instrumentation and software for X-ray diffraction (XRD) and X-ray fluorescence spectrometry (XRF),

PANalytical B.V.Lelyweg 1, 7602 EA AlmeloThe Netherlands

Global and near