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 Cluster of Research Infrastructures for Synergies in Physics (CRISP) under the 7th Framework Programme Grant Agreement 283745. Page 1 l XRI BM05 - CRISP l 17th March 2014 l T. A. Lafford
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 Page 2 l XRI BM05 - CRISP l 17th March 2014 l T. A. Lafford
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 Page 3 l XRI BM05 - CRISP l 17th March 2014 l T. A. Lafford
HOW DOES TOPOGRAPHY WORK? Extended, homogeneous, white or monochromatic, low divergence X-ray source Transmitted beam Radiograph Forward-diffracted Wide incident beam beam intensity “Contrast” Crystal with Bragg’s Law: defect 2D detectors λ = 2 d sin θ Diffracted beam intensity Page 4 l XRI BM05 - CRISP l 17th March 2014 l T. A. Lafford
WHITE BEAM XRDI Diffraction images Detector Polychromatic (“white”) X-ray beam Beamstop Sample (Beam sizes not to scale) Page 5 l XRI BM05 - CRISP l 17th March 2014 l T. A. Lafford
SYNTHETIC DIAMOND – WHITE BEAM XRDI (TOPOGRAPHY) 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 Inclusions Stacking faults Dislocations Dislocations Equal-thickness fringes Growth sectors Optical microscope, type Ib diamond Scratches? Diamond from Element6. Images courtesy Jürgen Härtwig, ESRF, and Page 6 l XRI BM05 - CRISP l 17th March 2014 l T. A. Lafford Simon Connell, University of Johannesburg
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 ~1 mm Czochralski silicon Mono-like silicon ~defect-free Dislocations h - tangles and bundles - parallel lines, dislocation walls Page 7 l XRI BM05 - CRISP l 17th March 2014 l T. A. Lafford
MONOCHROMATIC BEAM XRDI AND ROCKING CURVE IMAGING (RCI) FReLoN camera Diffraction image Sample Sample Monochromatic X-ray beam θ (Beam sizes not to scale) Page 8 l XRI BM05 - CRISP l 17th March 2014 l T. A. Lafford
SECTION XRDI Previous methods integrate images through the thickness of the sample Defect images overlap Little depth information � Section XRDI Page 9 l XRI BM05 - CRISP l 17th March 2014 l T. A. Lafford
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 Page 10 l XRI BM05 - CRISP l 17th March 2014 l T. A. Lafford
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 of diffraction spot Paste 1 Paste 2 Paste 3 So… So… Section topography Distribute the defect images according to their depth through the thickness of the sample Solar cells fabricated from neighbouring mono-like Si wafers Back-planes made from three different Al pastes Page 11 l XRI BM05 - CRISP l 17th March 2014 l T. A. Lafford
FULL SOLAR CELL STRUCTURES – SECTION RCI Inhomogeneous Paste C Paste A Paste B distortion arising from back-plane Least distortion 0 FWHM / ° � best PV 600 µ m conversion 600 Si 220 F efficiency 200 µ m h T. N. Tran Thi et al., CSSC7; T. N. Tran Thi , et al ., sub. Prog. Pholtovolt. Page 12 l XRI BM05 - CRISP l 17th March 2014 l T. A. Lafford
MICRO-ELECTRONICS TEST PATTERN – ROCKING CURVE IMAGING Deep Trench Isolation (DTI) 1.5 mm A A mm Part of test Part of test / ° 1.5 m FWHM / pattern Sample courtesy ST Crolles, under the IRT Nanoelec CGI project Page 13 l XRI BM05 - CRISP l 17th March 2014 l T. A. Lafford
MICRO-ELECTRONICS TEST PATTERN – ROCKING CURVE IMAGING Deep Trench Isolation (DTI) Sample courtesy ST Crolles, under the IRT Nanoelec CGI project l XRI BM05 - CRISP l 17th March 2014 l T. A. Lafford
IN SITU CRYSTAL GROWTH – COMBINED RADIOGRAPHY-TOPOGRAPHY Solidification of silicon for photovoltaic applications Grain growth, orientation and competition White beam topography Radiography h 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 Page 15 l XRI BM05 - CRISP l 17th March 2014 l T. A. Lafford
COMBINED RADIOGRAPHY-TOPOGRAPHY (1) In situ solidification studies Polychromatic (white) beam topography Film changer FReLoN Translation Camera device Polychromatic Polychromatic (white) beam Post-specimen monochromator Si(111) crystals UHV chamber Beam stop Guillaume Reinhart, IM2NP, Marseille; Euromat 2011 Page 16 l XRI BM05 - CRISP l 17th March 2014 l T. A. Lafford
COMBINED RADIOGRAPHY-TOPOGRAPHY (2) In situ solidification studies Post-sample monochromation for radiography Film changer Translation FReLoN device Camera Polychromatic (white) beam Post-specimen monochromator Si(111) crystals UHV Beam chamber stop Guillaume Reinhart, IM2NP, Marseille; Euromat 2011 Page 17 l XRI BM05 - CRISP l 17th March 2014 l T. A. Lafford
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 Page 18 l XRI BM05 - CRISP l 17th March 2014 l T. A. Lafford
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? tamzin.lafford@esrf.fr Page 19 l UM/FME workshop l 3Feb2014 l T. A. Lafford l
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