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Non-destructive three-dimensional crystallographic orientation analysis of olivine using laboratory diffraction contrast tomography

  • Matthew J Pankhurst (a1) (a2), Nicolas Gueninchault (a3) (a4), Matthew Andrew (a4) and Edward Hill (a5)


X-ray laboratory diffraction contrast tomography (LabDCT) produces three-dimensional (3D) maps of crystallographic orientation. The non-destructive nature of the technique affords the key benefit of full 3D context of these, and other, in situ measurements. This study is the first to apply the technique to any material other than a metal or silicon. We report the first 3D measurements of the crystallographic orientation of olivine, which also makes this study the first to apply LabDCT to (1) a non-metallic, non-cubic system and (2) geological material. First, we scanned fragments of olivine set in resin alongside glass microbeads using LabDCT and absorption contrast tomography (ACT). Then we reconstructed these data assuming an orthorhombic crystal system. We show that: (1) the regions within the sample that index well according to the orthorhombic system correspond to olivine fragments in the ACT image; (2) crystalline regions not corresponding to olivine are not indexed assuming the same lattice parameters; and (3) the diffraction data discriminates crystalline from non-crystalline materials as expected. Finally, we demonstrate that the method resolves sub-degree orientation differences between distinct regions within individual olivine fragments. We conclude that DCT can be applied to the study of rocks and other crystalline materials, and offers advantages over conventional techniques. We also note that LabDCT may offer a solution to the crystallographic measurement of substances that would otherwise be difficult to measure due to challenges in obtaining a perfect sample polish. Future developments to accommodate larger experimental volumes and additional crystallographic systems within a sample promises to expand the applicability and impact of DCT.


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*Author for correspondence: Matthew J Pankhurst, Email:


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Associate Editor: Koichi Momma



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Andrew, M. (2018) A quantified study of segmentation techniques on synthetic geological XRM and FIB-SEM images. Computational Geosciences, 22, 15031512.
Bachmann, F., Bale, H., Gueninchault, N., Holzner, C. and Lauridsen, E.M. (2019) 3D Grain reconstruction from laboratory diffraction contrast tomography. Journal of Applied Crystallography, 52, 643651.
Berg, S., Saxena, N., Shaik, M. and Pradhan, C. (2018) Generation of ground truth images to validate micro-CT image-processing pipelines. The Leading Edge, 37, 412420.
Bestmann, M. and Prior, D.J. (2003) Intragranular dynamic recrystallization in naturally deformed calcite marble: diffusion accommodated grain boundary sliding as a result of subgrain rotation recrystallization. Journal of Structural Geology, 25, 15971613.
Calcagnotto, M., Ponge, D., Demir, E. and Raabe, D. (2010) Orientation gradients and geometrically necessary dislocations in ultrafine grained dual-phase steels studied by 2D and 3D EBSD. Materials Science and Engineering: A, 527, 27382746.
Darling, J.R., Moser, D.E., Barker, I.R., Tait, K.T., Chamberlain, K.R., Schmitt, A.K. and Hyde, B.C. (2016) Variable microstructural response of baddeleyite to shock metamorphism in young basaltic shergottite NWA 5298 and improved U–Pb dating of Solar System events. Earth and Planetary Science Letters, 444, 112.
Deer, W.A., Howie, R.A. and Zussman, J. (1992) An Introduction to the Rock-Forming Minerals. Longman, London.
Demouchy, S., Tommasi, A., Barou, F., Mainprice, D. and Cordier, P. (2012) Deformation of olivine in torsion under hydrous conditions. Physics of the Earth and Planetary Interiors, 202–203, 5670.
Díaz Aspiroz, M., Lloyd, G.E. and Fernández, C. (2007) Development of lattice preferred orientation in clinoamphiboles deformed under low-pressure metamorphic conditions. A SEM/EBSD study of metabasites from the Aracena metamorphic belt (SW Spain). Journal of Structural Geology, 29, 629645.
Dohmen, R., Becker, H.-W. and Chakraborty, S. (2007) Fe–Mg diffusion in olivine I: experimental determination between 700 and 1,200°C as a function of composition, crystal orientation and oxygen fugacity. Physics and Chemistry of Minerals, 34, 389407.
Hansen, L.N., Zimmerman, M.E., Dillman, A.M. and Kohlstedt, D.L. (2012) Strain localization in olivine aggregates at high temperature: A laboratory comparison of constant-strain-rate and constant-stress boundary conditions. Earth and Planetary Science Letters, 333–334, 134145.
He, Y., Godet, S., Jacques, P.J. and Jonas, J.J. (2006) Crystallographic relations between face- and body-centred cubic crystals formed under near-equilibrium conditions: Observations from the Gibeon meteorite. Acta Materialia, 54, 13231334.
Holtzman, B.K., Kohlstedt, D.L., Zimmerman, M.E., Heidelbach, F., Hiraga, T. and Hustoft, J. (2003) Melt segregation and strain partitioning: implications for seismic anisotropy and mantle flow. Science, 301, 12271230.
Holzner, C., Lavery, L., Bale, H., Merkle, A., McDonald, S., Withers, P., Zhang, Y., Jensen, D.J., Kimura, M., Lyckegaard, A., Reischig, P. and Lauridsen, E.M. (2016) Diffraction contrast tomography in the laboratory – applications and future directions. Microscopy Today, 24, 3443.
Hunter, N.J.R., Weinberg, R.F., Wilson, C.J.L., Luzin, V. and Misra, S. (2018) Microscopic anatomy of a “hot-on-cold” shear zone: Insights from quartzites of the Main Central Thrust in the Alaknanda region (Garhwal Himalaya). GSA Bulletin, 130, 15191539.
Keinan, R., Bale, H., Gueninchault, N., Lauridsen, E.M. and Shahani, A.J. (2018) Integrated imaging in three dimensions: Providing a new lens on grain boundaries, particles, and their correlations in polycrystalline silicon. Acta Materialia, 148, 225234.
Kemppainen, A., Mattila, O., Heikkinen, E.-P., Paananen, T. and Fabritius, T. (2012) Effect of H2–H2O on the Reduction of Olivine Pellets in CO–CO2 Gas. ISIJ International, 52, 19731978.
King, A., Reischig, P., Adrien, J. and Ludwig, W. (2013) First laboratory X-ray diffraction contrast tomography for grain mapping of polycrystals. Journal of Applied Crystallography, 46, 17341740.
Lienert, U., Li, S.F., Hefferan, C.M., Lind, J., Suter, R.M., Bernier, J.V., Barton, N.R., Brandes, M.C., Mills, M.J., Miller, M.P., Jakobsen, B. and Pantleon, W. (2011) High-energy diffraction microscopy at the advanced photon source. JOM, 63, 7077.
Ludwig, W., Reischig, P., King, A., Herbig, M., Lauridsen, E.M., Johnson, G., Marrow, T.J. and Buffière, J.Y. (2009) Three-dimensional grain mapping by x-ray diffraction contrast tomography and the use of Friedel pairs in diffraction data analysis. Review of Scientific Instruments, 80, 033905.
Maitland, T. and Sitzman, S. (2007) Electron Backscatter Diffraction (EBSD) Technique and Materials Characterization Examples. Springer, Berlin.
McDonald, S.A., Reischig, P., Holzner, C., Lauridsen, E.M., Withers, P.J., Merkle, A.P. and Feser, M. (2015) Non-destructive mapping of grain orientations in 3D by laboratory X-ray microscopy. Scientific Reports, 5, #14665.
McDonald, S.A., Holzner, C., Lauridsen, E.M., Reischig, P., Merkle, A.P. and Withers, P.J. (2017) Microstructural evolution during sintering of copper particles studied by laboratory diffraction contrast tomography (LabDCT). Scientific Reports, 7, 5251.
Michibayashi, K., Mainprice, D., Fujii, A., Uehara, S., Shinkai, Y., Kondo, Y., Ohara, Y., Ishii, T., Fryer, P., Bloomer, S.H., Ishiwatari, A., Hawkins, J.W. and Ji, S. (2016) Natural olivine crystal-fabrics in the western Pacific convergence region: A new method to identify fabric type. Earth and Planetary Science Letters, 443, 7080.
Miyamoto, M., Mikouchi, T. and Jones, R.H. (2009) Cooling rates of porphyritic olivine chondrules in the Semarkona (LL3. 00) ordinary chondrite: A model for diffusional equilibration of olivine during fractional crystallization. Meteoritics & Planetary Science, 44, 521530.
Mizukami, T., Wallis, S.R. and Yamamoto, J. (2004) Natural examples of olivine lattice preferred orientation patterns with a flow-normal a-axis maximum. Nature, 427, 432.
Niverty, S., Sun, J., Williams, J., Bachmann, F., Gueninchault, N., Lauridsen, E.M. and Chawla, N. (2019) A forward modeling approach to high reliability grain mapping by Laboratory Diffraction Contrast Tomography (LabDCT). The Journal of the Minerals, Metals & Materials Society, 110.
Oddershede, J., Sun, J., Gueninchault, N., Bachmann, F., Bale, H., Holzner, C. and Lauridsen, E. (2019) Non-destructive Characterization of Polycrystalline Materials in 3D by Laboratory Diffraction Contrast Tomography. Integrating Materials and Manufacturing Innovation, Ausgabe 2/2019.
Pankhurst, M.J., Dobson, K.J., Morgan, D.J., Loughlin, S.C., Thordarson, T., Courtios, L. and Lee, P.D. (2014) Directly monitoring the magmas fuelling volcanic eruptions in near-real-time using X-ray micro-computed tomography. Journal of Petrology, 55, 671684.
Pankhurst, M.J., Walshaw, R. and Morgan, D.J. (2017) Major element chemical heterogeneity in Geo2 olivine microbeam reference material: a spatial approach to quantifying heterogeneity in primary reference materials. Geostandards and Geoanalytical Research, 41, 8591.
Pankhurst, M.J., Morgan, D.J., Thordarson, T. and Loughlin, S.C. (2018 a) Magmatic crystal records in time, space, and process, causatively linked with volcanic unrest. Earth and Planetary Science Letters, 493, 231241.
Pankhurst, M.J., Vo, N.T., Butcher, A.R., Long, L., Wang, H., Nonni, S., Harvey, J., Guðfinnsson, G., Fowler, R., Atwood, R., Walshaw, R. and Lee, P.D. (2018 b) Quantitative measurement of olivine composition in three dimensions using helical scan X-ray micro tomography. American Mineralogist, 103, 18001811.
Piatak, N.M., Parsons, M.B. and Seal, R.R. (2015) Characteristics and environmental aspects of slag: A review. Applied Geochemistry, 57, 236266.
Piazolo, S., Austrheim, H. and Whitehouse, M. (2012) Brittle-ductile microfabrics in naturally deformed zircon: Deformation mechanisms and consequences for U-Pb dating. American Mineralogist, 97, 15441563.
Poulsen, H.F. (2012) An introduction to three-dimensional X-ray diffraction microscopy. Journal of Applied Crystallography, 45, 10841097.
Poulsen, H.F., Nielsen, S.F., Lauridsen, E.M., Schmidt, S., Suter, R.M., Lienert, U., Margulies, L., Lorentzen, T. and Juul Jensen, D. (2001) Three-dimensional maps of grain boundaries and the stress state of individual grains in polycrystals and powders. Journal of Applied Crystallography, 34, 751756.
Prior, D.J., Mariani, E. and Wheeler, J. (2009) EBSD in the Earth Sciences: Applications, Common Practice, and Challenges. Pp. 345360 in: Electron Backscatter Diffraction in Materials Science (Schwartz, A.J., Kumar, M., Adams, B.L. and Field, D.P., editors). Springer US, Boston, MA.
Reddy, S.M., Timms, N.E., Pantleon, W. and Trimby, P. (2007) Quantitative characterization of plastic deformation of zircon and geological implications. Contributions to Mineralogy and Petrology, 153, 625645.
Rudraswami, N.G., Prasad, M.S., Jones, R.H. and Nagashima, K. (2016) In situ oxygen isotope compositions in olivines of different types of cosmic spherules: An assessment of relationships to chondritic particles. Geochimica et Cosmochimica Acta, 194, 114.
Shahani, A.J., Bale, H., Gueninchault, N., Merkle, A. and Lauridsen, E.M. (2017) Integrated Imaging in Three Dimensions: The Sum is Greater than the Parts. 2. Acta Materialia, 148, 225234.
Shea, T., Costa, F., Krimer, D. and Hammer, J.E. (2015 a) Accuracy of timescales retrieved from diffusion modeling in olivine: A 3D perspective. American Mineralogist, 100, 20262042.
Shea, T., Lynn, K.J. and Garcia, M.O. (2015 b) Cracking the olivine zoning code: Distinguishing between crystal growth and diffusion. Geology, 43, 935938.
Spiess, R., Bertolo, B., Borghi, A. and Centi, M.T. (2001) Crustal-mantle lithosphere decoupling as a control on Variscan metamorphism in the Eastern Alps. Australian Journal of Earth Sciences, 48, 479486.
Spiess, R., Groppo, C. and Compagnoni, R. (2007) When epitaxy controls garnet growth. Journal of Metamorphic Geology, 25, 439450.
Spiess, R., Dibona, R., Rybacki, E., Wirth, R. and Dresen, G. (2012) Depressurized Cavities within High-strain Shear Zones: their Role in the Segregation and Flow of SiO2-rich Melt in Feldspar-dominated Rocks. Journal of Petrology, 53, 17671776.
Storey, C.D. and Prior, D.J. (2005) Plastic deformation and recrystallization of garnet: a mechanism to facilitate diffusion creep. Journal of Petrology, 46, 25932613.
Sun, J., Zhang, Y., Lyckegaard, A., Bachmann, F., Lauridsen, E.M. and Juul Jensen, D. (2019) Grain boundary wetting correlated to the grain boundary properties: A laboratory-based multimodal X-ray tomography investigation. Scripta Materialia, 163, 7781.
Tasaka, M., Michibayashi, K. and Mainprice, D. (2008) B-type olivine fabrics developed in the fore-arc side of the mantle wedge along a subducting slab. Earth and Planetary Science Letters, 272, 747757.
Timms, N.E., Reddy, S.M., Fitz Gerald, J.D., Green, L. and Muhling, J.R. (2012) Inclusion-localised crystal-plasticity, dynamic porosity, and fast-diffusion pathway generation in zircon. Journal of Structural Geology, 35, 7889.
Timms, N.E., Erickson, T.M., Pearce, M.A., Cavosie, A.J., Schmieder, M., Tohver, E., Reddy, S.M., Zanetti, M.R., Nemchin, A.A. and Wittmann, A. (2017) A pressure-temperature phase diagram for zircon at extreme conditions. Earth-Science Reviews, 165, 185202.
Trimby, P.W., Prior, D.J. and Wheeler, J. (1998) Grain boundary hierarchy development in a quartz mylonite. Journal of Structural Geology, 20, 917935.


Non-destructive three-dimensional crystallographic orientation analysis of olivine using laboratory diffraction contrast tomography

  • Matthew J Pankhurst (a1) (a2), Nicolas Gueninchault (a3) (a4), Matthew Andrew (a4) and Edward Hill (a5)


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