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A New and Unexpected Spatial Relationship Between Interaction Volume and Diffraction Pattern in Electron Microscopy in Transmission

Published online by Cambridge University Press:  05 December 2018

Etienne Brodu  and
Emmanuel Bouzy
Etienne Brodu*
Affiliation:
Laboratoire d’Etude des Microstructures et de Mécanique des Matériaux (LEM3), Université de Lorraine, UMR CNRS 7239, 57045 Metz, France Laboratory of Excellence on Design of Alloy Metals for low-MAss Structures (DAMAS), University of Lorraine, 57045 Metz, France
Emmanuel Bouzy*
Affiliation:
Laboratoire d’Etude des Microstructures et de Mécanique des Matériaux (LEM3), Université de Lorraine, UMR CNRS 7239, 57045 Metz, France Laboratory of Excellence on Design of Alloy Metals for low-MAss Structures (DAMAS), University of Lorraine, 57045 Metz, France
*
Authors for correspondence: Etienne Brodu, E-mail: [email protected]; Emmanuel Bouzy, E-mail: [email protected]
Authors for correspondence: Etienne Brodu, E-mail: [email protected]; Emmanuel Bouzy, E-mail: [email protected]
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Abstract

The finding of this study is that the interaction volume in electron microscopy in transmission is well ordered laterally, with a remarkable and unexpected consequence being that lateral subsections of the interaction volume produce subsections of the Kikuchi diffraction pattern. It makes the microstructure of samples directly visible in Kikuchi patterns. This is first illustrated with polycrystalline Ti–10Al–25Nb with an on-axis transmission Kikuchi diffraction set-up in a scanning electron microscope. It is then shown via a Monte Carlo simulation and a large-angle convergent-beam electron diffraction experiment that this phenomenon finds its origin in the nature of the differential elastic and quasi-elastic cross sections. This phenomenon is then quantified by a careful image analysis of Kikuchi patterns recorded across a vertical interface in a silicon sample specifically designed and fabricated. A Monte Carlo simulation reproducing all the geometric parameters is conducted. Experiments and simulations match very well qualitatively, but with a slight quantitativity gap. The specificity of the thermal diffuse scattering cross-section, not available in the simulation, is thought to be responsible for this gap. Beside Kikuchi diffraction, the case of diffraction spots and diffuse background present in the pattern is also discussed.

Keywords

electron microscopytransmission Kikuchi diffractioninteraction volumediffraction patternMonte Carlo simulation
Type
Materials Science Applications
Information
Microscopy and Microanalysis , Volume 24 , Issue 6 , December 2018 , pp. 634 - 646
Copyright
© Microscopy Society of America 2018 

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Footnotes

Cite this article: Brodu E, Bouzy E (2018) A New and Unexpected Spatial Relationship Between Interaction Volume and Diffraction Pattern in Electron Microscopy in Transmission. Microsc Microanal. 24(6), 634–646. doi: 10.1017/S1431927618015441

References

Abbasi, M, Kim, DI, Guim, HU, Hosseini, M, Danesh-Manesh, H and Abbasi, M (2015) Application of transmitted Kikuchi diffraction in studying nano-oxide and ultrafine metallic grains. ACS NANO 9, 10991–11002.Google Scholar
Borrajo-Pelaez, R and Hedstrom, P (2018) Recent developments of crystallographic analysis methods in the scanning electron microscope for applications in metallurgy. Crit Rev Solid State Mater Sci 43, 455–474.Google Scholar
Brodu, E and Bouzy, E (2017) Depth resolution dependence on sample thickness and incident energy in on-axis transmission Kikuchi diffraction in SEM. Microsc Microanal 23, 1096–1106.Google Scholar
Brodu, E, Bouzy, E and Fundenberger, J-J (2017) Diffraction contrast dependence on sample thickness and incident energy in on-axis transmission Kikuchi diffraction in SEM. Ultramicroscopy 181, 123–133.Google Scholar
Brodusch, N, Demers, H and Gauvin, R (2013) Nanometres-resolution Kikuchi patterns from materials science specimens with transmission electron forward scatter diffraction in the scanning electron microscope. J Microsc 250, 1–14.Google Scholar
Callahan, PG and De Graef, M (2013) Dynamical electron backscatter diffraction patterns. Part I: Pattern simulations. Microsc Microanal 19, 1255–1265.Google Scholar
Chen, YH, Park, SU, Wei, D, Newstadt, G, Jackson, MA, Simmons, JP, Graef, M. De and Hero, AO (2015) A dictionary approach to electron backscatter diffraction indexing. Microsc Microanal 21, 739–752.Google Scholar
Chinga, G and Syverud, K (2007) Quantification of paper mass distributions within local picking areas. Nord Pulp Pap Res J 22, 441–446.Google Scholar
Chukhovskii, FN, Alexanjan, LA and Pinsker, ZG (1973) Dynamical treatment of Kikuchi patterns. Acta Crystallogr A 29, 38–45.Google Scholar
de Jonge, N, Poirier-Demers, N, Demers, H, Peckys, DB and Drouin, D (2010) Nanometer-resolution electron microscopy through micrometers-thick water layers. Ultramicroscopy 110, 1114–1119.Google Scholar
Demers, H, Poirier-Demers, N, Réal Couture, A, Joly, D, Guilmain, M, De Jonge, N and Drouin, D (2011) Three-dimensional electron microscopy simulation with the CASINO Monte Carlo software. Scanning 33, 135–146.Google Scholar
Drouin, D, Couture, AR, Joly, D, Tastet, X, Aimez, V and Gauvin, R (2007) CASINO V2.42 - A fast and easy-to-use modeling tool for scanning electron microscopy and microanalysis users. Scanning 29, 92–101.Google Scholar
Fundenberger, JJ, Bouzy, E, Goran, D, Guyon, J, Yuan, H and Morawiec, A (2016) Orientation mapping by transmission-SEM with an on-axis detector. Ultramicroscopy 161, 17–22.Google Scholar
Friedrich, T, Bochmann, A, Dinger, J and Teichert, S (2018) Application of the pattern matching approach for EBSD calibration and orientation mapping, utilising dynamical EBSP simulations. Ultramicroscopy 184, 44–51.Google Scholar
Høier, R (1973) Multiple scattering and dynamical effects in diffuse electron scattering. Acta Crystallogr A29, 663–672.Google Scholar
Joy, DC (1995) Monte Carlo Modeling for Electron Microscopy and Microanalysis. Oxford, New York: Oxford University Press.Google Scholar
Keller, RR and Geiss, RH (2012) Transmission EBSD from 10 nm domains in a scanning electron microscope. J Microsc 245, 245–251.Google Scholar
Marquardt, K, De Graef, M, Singh, S, Marquardt, H, Rosenthal, A and Koizuimi, S (2017) Quantitative electron backscatter diffraction (EBSD) data analyses using the dictionary indexing (DI) approach: Overcoming indexing difficulties on geological materials. Am Mineral 102, 1843–1855.Google Scholar
Morniroli, JP (2002) Large-angle convergent-beam electron diffraction (LACBED) - Application to crystal defects, Monograph of the French Society of Microscopies, Paris.Google Scholar
Muller, DA, Edwards, B, Kirkland, EJ and Silcox, J (2001) Simulation of thermal diffuse scattering including a detailed phonon dispersion curve. Ultramicroscopy 86, 371–380.Google Scholar
Naresh-Kumar, G, Vilalta-Clemente, A, Jussila, H, Winkelmann, A, Nolze, G, Vespucci, S, Nagarajan, S, Wilkinson, AJ and Trager-Cowan, C (2017) Quantitative imaging of anti-phase domains by polarity sensitive orientation mapping using electron backscatter diffraction. Sci Rep 7, 10916.Google Scholar
Nolze, G, Winkelmann, A and Boyle, AP (2016) Pattern matching approach to pseudosymmetry problems in electron backscatter diffraction. Ultramicroscopy 160, 146–154.Google Scholar
Nolze, G, Jurgens, M, Olbricht, J and Winkelmann, A (2018) Improving the precision of orientation measurements from technical materials via EBSD pattern matching. Acta Mater 159, 408–415.Google Scholar
Omoto, K, Tsuda, K and Tanaka, M (2002) Simulations of Kikuchi patterns due to thermal diffuse scattering in MgO crystals. Japanese Soc Electron Micros 51, 67–78.Google Scholar
Pascal, E, Singh, S, Callahan, PG and De Graef, M (2018) Energy-weighted dynamical scattering simulations of back-scattered electron diffraction modalities. Ultramicroscopy 187, 98–106.Google Scholar
Ram, F and De Graef, M (2018) Phase differentiation by electron backscatter diffraction using the dictionary indexing approach. Acta Mater 144, 352–364.Google Scholar
Ram, F, Wright, S, Singh, S and De Graef, M (2017) Error analysis of the crystal orientations obtained by the dictionary approach to EBSD indexing. Ultramicroscopy 181, 17–26.Google Scholar
Reimer, L and Lodding, B (1984) Calculation and tabulation of Mott cross-sections for large-angle electron scattering. Scanning 6, 128–151.Google Scholar
Rice, KP, Keller, RR and Stoykovich, MP (2014) Specimen-thickness effects on transmission Kikuchi patterns in the scanning electron microscope. J Microsc 254, 129–136.Google Scholar
Sneddon, G, Trimby, P and Cairney, J (2017) The influence of microscope and specimen parameters on the spatial resolution of transmission Kikuchi diffraction. Microsc Microanal 23(Suppl 1), 532–533.Google Scholar
Sousa, AA, Hohmann-Marriott, MF, Zhang, G and Leapman, RD (2009) Monte Carlo electron-trajectory simulations in bright-field and dark-field STEM: Implications for tomography of thick biological sections. Ultramicroscopy 109, 213–221.Google Scholar
Steinmetz, DR and Zaefferer, S (2010) Towards ultrahigh resolution EBSD by low accelerating voltage. Mater Sci Technol 26, 640–645.Google Scholar
Vespucci, S, Winkelmann, A, Mingard, K, Maneuski, D, O’Shea, V and Trager-Cowan, C (2017) Exploring transmission Kikuchi diffraction using a Timepix detector. J Instrum 12, 1–8.Google Scholar
Vespucci, S, Winkelmann, A, Naresh-Kumar, G, Mingard, KP, Maneuski, D, Edwards, PR, Day, AP, O’Shea, V and Trager-Cowan, C (2015) Digital direct electron imaging of energy-filtered electron backscatter diffraction patterns. Phys Rev B 92, 205301.Google Scholar
Wang, ZL (2003) Thermal diffuse scattering in sub-angstrom quantitative electron microscopy—phenomenon, effects and approaches. Micron 34, 141–155.Google Scholar
Wallis, D, Hansen, LN, Britton, TB and Wilkinson, AJ (2016) Geometrically necessary dislocation densities in olivine obtained using high-angular resolution electron backscatter diffraction. Ultramicroscopy 168, 34–45.Google Scholar
Wilkinson, AJ, Moldovan, G, Britton, TB, Bewick, A, Clough, R and Kirkland, AI (2013) Direct detection of electron backscatter diffraction pattern. Phys Rev Lett 111, 065506.Google Scholar
Wilkinson, AJ and Randman, D (2010) Determination of elastic strain fields and geometrically necessary dislocation distributions near nanoindents using electron back scatter diffraction. Philos Mag 90, 1159–1177.Google Scholar
Winkelmann, A (2008) Dynamical effects of anisotropic inelastic scattering in electron backscatter diffraction. Ultramicroscopy 108, 1546–1550.Google Scholar
Winkelmann, A (2010) Principles of depth-resolved Kikuchi pattern simulation for electron backscatter diffraction. J Microsc 239, 32–45.Google Scholar
Winkelmann, A and Nolze, G (2010) Analysis of Kikuchi band contrast reversal in electron backscatter diffraction patterns of silicon. Ultramicroscopy 110, 190–194.Google Scholar
Winkelmann, A and Nolze, G (2015) Chirality determination of quartz crystals using electron backscatter diffraction. Ultramicroscopy 149, 58–63.Google Scholar
Winkelmann, A, Trager-Cowan, C, Sweeney, F, Day, AP and Parbrook, P (2007) Many-beam dynamical simulation of electron backscatter diffraction patterns. Ultramicroscopy 107, 414–421.Google Scholar