X-ray imaging at BM05, European Synchrotron Radiation Facility - - PowerPoint PPT Presentation

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CRISP WIN WORKSHOP X-ray imaging at BM05, European Synchrotron Radiation Facility Tamzin Lafford Tamzin Lafford Beamline Scientist The Workshop on Imaging with Neutrons has received funding from the European Commission in the frame of the

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CRISP WIN WORKSHOP

X-ray imaging at BM05, European Synchrotron Radiation Facility Tamzin Lafford Tamzin Lafford Beamline Scientist

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The Workshop on Imaging with Neutrons has received funding from the European Commission in the frame of the Cluster of Research Infrastructures for Synergies in Physics (CRISP) under the 7th Framework Programme Grant Agreement 283745.

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OUTLINE

X-ray Bragg diffraction imaging (XRDI; topography)

What can we learn? How does it work? Examples

Combined radiography-topography

Example: in situ crystal growth

X-ray micro-tomography X-ray micro-tomography

Available but not discussed here

Characteristics of BM05

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X-RAY DIFFRACTION IMAGING (TOPOGRAPHY)

We can see…

Defects in near-perfect crystals

Dislocations, slip planes, stacking faults, scratches, cracks, grains/sub-

grains, grain boundaries, agglomerations of inclusions, growth sectors and striations, magnetic domains…

How?

…via local distortion of the lattice induced by the defects

How does that work?

…Bragg diffraction of X-rays from crystal lattice planes

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HOW DOES TOPOGRAPHY WORK?

Extended, homogeneous, white or monochromatic, low divergence X-ray source

Wide incident beam

Transmitted beam Radiograph Forward-diffracted beam intensity

2D detectors

Bragg’s Law: λ = 2dsinθ

Crystal with defect

Diffracted beam intensity

“Contrast”

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WHITE BEAM XRDI

Detector Diffraction images

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Polychromatic (“white”) X-ray beam Sample Beamstop

(Beam sizes not to scale)

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Are [synthetic] diamonds a girl’s best friend?

High pressure, high temperature seed-grown diamond Type IIa-D1, 100-oriented; white beam topograph, -220 reflection

SYNTHETIC DIAMOND – WHITE BEAM XRDI (TOPOGRAPHY)

Stacking faults Dislocations Inclusions

Optical microscope, type Ib diamond

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Diamond from Element6. Images courtesy Jürgen Härtwig, ESRF, and Simon Connell, University of Johannesburg

Dislocations Equal-thickness fringes Growth sectors Scratches?

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CZOCHRALSKI AND MONO-LIKE SILICON WAFERS – WHITE BEAM XRDI

Wafers cut perpendicular to the growth direction ~220 µm thick Magnifications of parts of Si 220 diffraction spots Agfa Structurix D3 film, grain size ~5 µm

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Czochralski silicon ~defect-free Mono-like silicon Dislocations

tangles and bundles
parallel lines, dislocation walls

~1 mm h

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MONOCHROMATIC BEAM XRDI AND ROCKING CURVE IMAGING (RCI)

Sample Diffraction image FReLoN camera

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Monochromatic X-ray beam Sample

(Beam sizes not to scale)

θ

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SECTION XRDI

Previous methods integrate images through the thickness of the sample

Defect images overlap Little depth information

Section XRDI

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DEVELOPMENT OF DEFECTS IN THE MONO-LIKE SI INGOT – RCI

M. G. Tsoutsouva et al., CSSC7;

See M. G. Tsoutsouva, et al., Journal of Crystal Growth (2013),http://dx.doi.org/10.1016/j.jcrysgro.2013.12.022

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EFFECT OF THE AL BACK-PLANE – SECTION ROCKING CURVE IMAGING (RCI)

Topographs of volume dominated by “orange peel” effect from the back-plane Overall stress distorts shape

f diffraction spot

So…

Paste 1 Paste 2 Paste 3

So… Section topography

Distribute the defect images according to their depth through the thickness of the sample

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Solar cells fabricated from neighbouring mono-like Si wafers Back-planes made from three different Al pastes

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FULL SOLAR CELL STRUCTURES – SECTION RCI

Inhomogeneous distortion arising from back-plane Least distortion best PV conversion

600 µm 0 FWHM / ° Paste A Paste B Paste C

efficiency

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h 600 200 µm Si 220 F

T. N. Tran Thi et al., CSSC7; T. N. Tran Thi , et al., sub. Prog. Pholtovolt.

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MICRO-ELECTRONICS TEST PATTERN – ROCKING CURVE IMAGING

Deep Trench Isolation (DTI)

1.5 mm mm

/ ° A

Part of test

A

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1.5 m

FWHM /

Sample courtesy ST Crolles, under the IRT Nanoelec CGI project

Part of test pattern

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MICRO-ELECTRONICS TEST PATTERN – ROCKING CURVE IMAGING

Deep Trench Isolation (DTI)

l XRI BM05 - CRISP l 17th March 2014 l T. A. Lafford

Sample courtesy ST Crolles, under the IRT Nanoelec CGI project

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IN SITU CRYSTAL GROWTH – COMBINED RADIOGRAPHY-TOPOGRAPHY

Solidification of silicon for photovoltaic applications Grain growth, orientation and competition

h

Radiography White beam topography

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t t+8 min t+15 min t+22 min

h

N. Mangelinck-Noël, A. Tandjaoui

and G. Reinhart IM2NP Marseille, Campus Scientifique de Saint Jérôme, 13397 Marseille Cedex 20, France

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In situ solidification studies Polychromatic (white) beam topography

FReLoN Camera

Film changer

Polychromatic Translation device COMBINED RADIOGRAPHY-TOPOGRAPHY (1)

Post-specimen monochromator Si(111) crystals

Polychromatic (white) beam UHV chamber Beam stop Guillaume Reinhart, IM2NP, Marseille; Euromat 2011

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In situ solidification studies Post-sample monochromation for radiography

Polychromatic Translation device Film changer FReLoN Camera COMBINED RADIOGRAPHY-TOPOGRAPHY (2) (white) beam

UHV chamber Beam stop

Post-specimen monochromator Si(111) crystals

Guillaume Reinhart, IM2NP, Marseille; Euromat 2011

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WRAP-UP

X-ray Bragg diffraction imaging (XRDI; topography) Radiography Micro-tomography …all available at BM05 …possibly in combination and in situ Low beam divergence (approximate to parallel) White beam few keV to ~200 keV Pink filtered beam Multilayer Monochromator ∆E/E ~10-2 Double Silicon 111 Monochromator ∆E/E ~10-4 Cameras+optics: image pixel sizes 0.7 µm to 30 µm

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THANKS AND QUESTIONS?

Thanks to:

Maria Tsoutsouva and Thu Nhi Tran Thi (BM05) José Baruchel (Emeritus Scientist, ESRF) Vanessa Amaral de Oliveira, Sébastien Dubois, Nicolas Enjalbert and Denis Camel (CEA-INES) Anne Bonnin (ID19) Nathalie Mangelinck-Noël, Amina Tandjaoui and Guillaume Reinhart (IM2NP, Marseille) Guillaume Reinhart (IM2NP, Marseille)

And to you Any questions?

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tamzin.lafford@esrf.fr

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