TexTOM: bringing crystallographic texture analysis to the third dimension
Texture tomography (TexTOM) is a cutting-edge 3D crystallographic texture-analysis tool for polycrystalline materials, now available at beamlines ID13 and ID15A, with future expansions planned for additional beamlines. TexTOM offers rapid, quantitative texture analysis with enhanced spatial resolution, making it ideal for complex materials like biominerals, deformed metals, and technical alloys. This technique enables in-situ and operando studies, expanding the possibilities for real-time texture investigations.
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Crystallographic texture plays a crucial role in determining the mechanical, electronic, magnetic, and optical properties of polycrystalline materials. Existing techniques, such as 3D X-ray diffraction (3DXRD) [1] and dark-field X-ray microscopy [2], are effective for analyzing well-aligned, narrow structures in technical materials. However, they are limited in their ability to provide comprehensive quantitative texture information in 3D analysis for broader more complex textures, which are typically found in biomaterials, biominerals, or deformed technical materials.
While wide-angle X-ray scattering (WAXS) tensor tomography [3] (derived from small-angle X-ray scattering tensor tomography [4,5,6]) has facilitated more detailed 3D orientation analysis, it lacks a fully quantitative approach due to its reliance on a reciprocal space model of single Bragg reflections. In contrast, typical diffraction patterns contain multiple crystalline reflections, whose intensity and distribution offer valuable additional information.
TexTOM is a new tool developed by Tilman Grünewald’s group at the Institut Fresnel, Marseille, in collaboration with beamlines ID13 and ID15A, designed to fill the gap in 3D crystallographic texture analysis. The technique utilizes a hyperspherical harmonics [7] approach to model local orientation distribution functions (ODF), enabling the description of crystallographic texture in 3D. By incorporating prior knowledge of crystal symmetry, TexTOM reduces the data required compared to WAXS tensor tomography, thereby accelerating the measurement process and minimizing sample exposure.
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Fig. 1: Texture tomography (TexTOM). a) Data collection involves raster-scanning a sample through a focused X-ray beam at multiple rotation and tilt angles, capturing a 2D diffraction pattern at each scan point. b) Selected diffractlets form the basis for structural reconstruction. c) Successful reconstruction of a silica biomorph, where a full orientation distribution is determined for each voxel, allowing detailed analysis.
Data acquisition involves raster-scanning a focused X-ray beam across the sample at various rotation and tilt angles, collecting a diffraction pattern at each point (Figure 1a). The dataset is then processed and aligned for inversion. The hyperspherical harmonic basis simplifies the forward model of diffractlet summation (Figure 1b), while the inversion process employs a gradient-descent backtracking technique to optimize the local ODFs, matching simulated diffraction patterns with experimental data (Figure 1c). The outcome is an ODF that describes the full quantitative texture for each voxel of the tomogram.
TexTOM enables the determination of 3D quantitative texture information across a wide range of materials. Its efficient use of diffraction data significantly reduces acquisition times – down to 30 minutes in some cases – while maintaining high-quality reconstructions. Operation at higher energies at ID15A allows for the study of large bulk samples and working devices. The integration of the new Pilatus 4 detector at ID15A further enhances the potential for fast in-situ or operando studies.
The spatial resolution is primarily constrained by the X-ray beam size, which can reach 20 nm at ID13, while maintaining enough flux for rapid, detector-limited data acquisition. Although this high spatial resolution limits the sample size, it enables detailed investigation of complex, hierarchically structured materials such as bone, tendon, and their interfaces, as well as other biominerals like shells and teeth, alongside advanced technical materials such as alloys, energy materials, and ceramics.
Principal publication and authors
Texture tomography, a versatile framework to study crystalline texture in 3D, M.P.K. Frewein (a), J. Mason (b), B. Maier (c), H. Cölfen (c), A. Medjahed (d), M. Burghammer (d), M. Allain (a), T.A. Grünewald (a), IUCrJ 11(5), 809-820 (2024); https://doi.org/10.1107/S2052252524006547
(a) Aix Marseille Univ, CNRS, Centrale Med, Institut Fresnel, Marseille (France)
(b) University of California, Davis, California (USA)
(c) University of Konstanz, Konstanz (Germany)
(d) ESRF
References
[1] H.F. Poulsen et al., J. Appl. Crystallogr. 34, 751-756 (2001).
[2] H. Simons et al., Nat. Commun. 6, 6098 (2015).
[3] T.A. Grünewald et al., Sci. Adv. 6, eaba4171 (2020).
[4] M. Liebi et al., Nature 527, 349-352 (2015).
[5] F. Schaff et al., Nature 527, 353-356 (2015).
[6] L.C. Nielsen et al., Acta Crystallogr. A Found. Adv. 79, 515-526 (2023).
[7] J.K. Mason & C.A. Schuh, Acta Mater. 56, 6141-6155 (2008).