Laboratory Diffraction Contrast Tomography (LabDCT) is a recent analytical development that allows for non-destructive microstructural characterisation of crystalline materials using a laboratory-scale X-ray microscope. In this study, we apply LabDCT to investigate magmatic olivine crystals hosting melt inclusion populations with preferential alignment. Melt inclusions provide valuable insights into magmatic and volcanic processes, and are often the subject of extensive geochemical investigation. Destructive sample preparation can prematurely erase contextural information such as inclusion geometries, population characteristics, and the relationship between the inclusion and its host crystal. The approach used in this study shows a clear crystallographic control on melt inclusion orientations where a visual alignment is identified. Melt inclusions consistently align parallel with the a-axis ([100]) of their olivine hosts. This alignment suggests that inclusion entrapment occurred during rapid, skeletal olivine growth, likely the result of thermal disequilibrium and undercooling within the magmatic system. This insight was gained without destructive sample preparation, highlighting the value of these X-ray imaging techniques for microstructural investigation and sample characterisation. This study demonstrates the range of opportunities available by applying non-destructive, three-dimensional X-ray imaging techniques to investigate geomaterials. The method described and applied in this study can be used to compare the orientation of any internal feature to its mineral host, such as melt inclusions and their host olivine crystals.

Combining electron backscatter diffraction (EBSD) with X-ray computed tomography (XCT) offers a comprehensive approach to investigate shock deformation and rock texture in meteorites, yet such integration remains uncommon. In this study, we demonstrate the synergistic potential of XCT and EBSD in revealing deformation metrics, thereby enhancing our understanding of petrofabric strength and shock-induced deformation. Our analysis focuses on the Ozerki (L6, S4/5, W0) meteorite fall, which was instrumentally observed on June 21, 2018, and subsequently recovered by the Ural's branch of the Russian Fireball Network (UrFU) recovery expedition a few days later. The trajectory analysis conducted by the Finnish Fireball Network facilitated the prompt retrieval of the meteorite. We show that Ozerki is deformed, with a moderate strength foliation fabric defined by metal and sulfide grain shapes. Microstructural analysis using EBSD shows that the parent body was likely still thermally active during this impact event. Our data suggest that these microstructures were likely produced during an impact while the Ozerki's parent body was still warm.

The Winchcombe meteorite is a CM chondrite breccia composed of eight distinct lithological units plus a cataclastic matrix. The degree of aqueous alteration varies between intensely altered CM2.0 and moderately altered CM2.6. Although no lithology dominates, three heavily altered rock types (CM2.1-2.3) represent >70 area%. Tochilinite-cronstedtite intergrowths (TCIs) are common in several lithologies. Their compositions can vary significantly, even within a single lithology, which can prevent a clear assessment of alteration extent if only TCI composition is considered. We suggest that this is due to early alteration under localized geochemical microenvironments creating a diversity of compositions and because later reprocessing was incomplete, leaving a record of the parent body's fluid history. In Winchcombe, the fragments of primary accretionary rock are held within a cataclastic matrix (similar to 15 area%). This material is impact-derived fallback debris. Its grain size and texture suggest that the disruption of the original parent asteroid responded by intergranular fracture at grain sizes <100 mu m, while larger phases, such as whole chondrules, splintered apart. Reaccretion formed a poorly lithified body. During atmospheric entry, the Winchcombe meteoroid broke apart with new fractures preferentially cutting through the weaker cataclastic matrix and separating the breccia into its component clasts. The strength of the cataclastic matrix imparts a control on the survival of CM chondrite meteoroids. Winchcombe's unweathered state and diversity of lithologies make it an ideal sample for exploring the geological history of the CM chondrite group.

The remarkable physical properties of dental enamel can be largely attributed to the structure of the hydroxyapatite (HAp) crystallites on the sub-micrometre scale. Characterising the HAp microstructure is challenging, due to the nanoscale of individual crystallites and practical challenges associated with HAp examination using electron microscopy techniques. Conventional methods for enamel characterisation include imaging using transmission electron microscopy (TEM) or specialised beamline techniques, such as polarisation-dependent imaging contrast (PIC). These provide useful information at the necessary spatial resolution but are not able to measure the full crystallographic orientation of the HAp crystallites. Here we demonstrate the effectiveness of enamel analyses using transmission Kikuchi diffraction (TKD) in the scanning electron microscope, coupled with newly-developed pattern matching methods. The pattern matching approach, using dynamic template matching coupled with subsequent orientation refinement, enables robust indexing of even poor-quality TKD patterns, resulting in significantly improved data quality compared to conventional diffraction pattern indexing methods. The potential of this method for the analysis of nanocrystalline enamel structures is demonstrated by the characterisation of a human enamel TEM sample and the subsequent comparison of the results to high resolution TEM imaging. The TKD - pattern matching approach measures the full HAp crystallographic orientation enabling a quantitative measurement of not just the c-axis orientations, but also the extent of any rotation of the crystal lattice about the c-axis, between and within grains. Results presented here show how this additional information highlights potentially significant aspects of the HAp crystallite structure, including intra-crystallite distortion and the presence of multiple high angle boundaries between adjacent crystallites with rotations about the c-axis. These and other observations enable a more rigorous understanding of the relationship between HAp structures and the physical properties of dental enamel.

Based on petrological association, cathodoluminescence (CL), trace element signatures and orientation relationships, two generations of kyanite are distinguished in a high temperature, high pressure garnet-biotite-aluminosilicate bearing migmatite of South Harris, NW Scotland. The migmatite shows a garnet and biotite rich domain (Grt-Bt domain) which is cut at a low angle by a dominantly coarse-grained plagioclase-quartz leucosome. In addition, a fine-grained plagioclase-quartz-kyanite domain (Plag-Qtz-Ky domain) is present intercalated with the Grt-Bt domain and subparallel to the plagioclase-quartz domain. Type 1 kyanite is coarse grained and associated with Bt clusters and garnet within the Grt-Bt domain. It grew relatively early, syn- to post-garnet growth, in a suprasolidus environment resulting in crystallographically determined oscillatory CL and trace element zoning. Grains record evidence of progressive deformation in the crystal plastic regime, where deformation is accommodated by dislocation glide, climb and deformation twinning. The dominant activated slip system is (100)<001> with minor component of <100>, while deformation twins show a similar to 180 degrees rotation around similar to<001> axis and a twin plane near (001). Grains appear to be impervious to deformation induced diffusion with all zoning remaining sharp despite crystal plastic deformation. Grains in direct contact with the Plag-Qtz-Ky domain show late modification of the CL and trace element signature suggesting melt-mediated interface-coupled dissolution-precipitation reaction. This modification resulted in crosscutting lobate high trace element regions and irregular rims with low Cr and V content. These rims show similar CL and trace element characteristics as Type 2 kyanite which are exclusively seen within the Plag-Qtz-Ky domain suggesting that Type 2 grains are cogenetic with Type 1 rims. Type 2 grains are finer grained than Type 1 grains and show near uniform CL and trace element distributions with rare oscillatory zoned and relatively higher Cr & V bright cores. Type 2 show either no or very localized internal deformation features. However, they exhibit a clear shape preferred orientation which coincides with a crystallographic preferred orientation where the longest shape axis is parallel to <001>. We propose that Type 2 kyanite grains underwent melt-present deformation by rigid body rotation in an externally derived melt with different trace element chemistry than the host rock. This melt thus interacted chemically by melt-mediated interface-coupled dissolution-precipitation reactions with the surrounding rocks forming the Type 1 rims. Our study shows detailed analysis of kyanite is an important tool for giving constraints on the deformation, P-T and melting history of high-grade metamorphic rocks and migmatites.

The Mighei-like carbonaceous (CM) chondrites have been altered to various extents by water-rock reactions on their parent asteroid(s). This aqueous processing has destroyed much of the primary mineralogy of these meteorites, and the degree of alteration is highly heterogeneous at both the macroscale and nanoscale. Many CM meteorites are also heavily brecciated juxtaposing clasts with different alteration histories. Here we present results from the fine-grained team consortium study of the Winchcombe meteorite, a recent CM chondrite fall that is a breccia and contains eight discrete lithologies that span a range of petrologic subtypes (CM2.0-2.6) that are suspended in a cataclastic matrix. Coordinated multitechnique, multiscale analyses of this breccia reveal substantial heterogeneity in the extent of alteration, even in highly aqueously processed lithologies. Some lithologies exhibit the full range and can comprise nearly unaltered coarse-grained primary components that are found directly alongside other coarse-grained components that have experienced complete pseudomorphic replacement by secondary minerals. The preservation of the complete alteration sequence and pseudomorph textures showing tochilinite-cronstedtite intergrowths are replacing carbonates suggest that CMs may be initially more carbonate rich than previously thought. This heterogeneity in aqueous alteration extent is likely due to a combination of microscale variability in permeability and water/rock ratio generating local microenvironments as has been established previously. Nevertheless, some of the disequilibrium mineral assemblages observed, such as hydrous minerals juxtaposed with surviving phases that are typically more fluid susceptible, can only be reconciled by multiple generations of alteration, disruption, and reaccretion of the CM parent body at the grain scale.

Janos Urai made major contributions to our understanding of rock deformation and the microstructural fingerprints that can be used to investigate it. One such fingerprint is intracrystalline distortion. Crystals can be distorted due to deformation or growth but the distortion gives insights into processes in either case. Distortion is generally due to the presence of dislocations which give information on slip systems, stress levels, growth mechanisms etc. Electron backscatter diffraction (EBSD) allows detailed quantification of distorted crystals, and we summarise here a method for extracting information on dislocations from such data. The weighted Burgers vector (WBV) method calculates a vector at each point on an EBSD map, or an average over a region. The vector is a weighted average of the Burgers vectors of dislocation lines intersecting the map surface. It is weighted towards dislocation lines at a high angle to the map but that can be accounted for in interpretation. The method is fast and does not involve specific assumptions about dislocation types; it assumes only that elastic strains have little effect on the calculation. It can be used, with care, to analyse subgrain walls (sharp orientation changes) as well as gradational orientation changes within individual grains. It can complement established methods for subgrain wall analysis and frees us from some assumptions made in other methods. We give examples of its use applied to olivine and plagioclase. The magnitude of the vector relates to dislocation density but, as a vector, we find its directional information particularly informative. Code to implement this approach is available from the first author (“Crystalscape”), from Oxford Instruments (a commercial version) and aspects are implemented in MTEX. Urai, J. L., Means, W. D. & Lister, G. S. 1986. Dynamic recrystallisation of minerals. In: Mineral and Rock Deformation: Laboratory Studies (edited by Hobbs, B. E. & Heard, H. C.). Geophysical Monograph 36. AGU, Washington, D.C., 161-199. Urai, J. L. & Spiers, C. J. 2007. The effect of grain boundary water on deformation mechanisms and rheology of rocksalt during long-term deformation. In: 6th Conference on the Mechanical Behavior of Salt. Proceedings and Monographs in Engineering Water and Earth Sciences, Fed Inst Geosci & Nat Resources, Hannover, 149-+. Wheeler, J., Piazolo, S., Prior, D. J., Trimby, P. W. & Tielke, J. A. 2024. Using crystal lattice distortion data for geological investigations: the Weighted Burgers Vector method. Journal of Structural Geology 179, 105040.

The spatial resolution of transmission Kikuchi diffraction (TKD) depends on experimental parameters such as atomic number, accelerating voltage, sample backtilt and thickness. In this work, the dependence of spatial resolution on these parameters is explored by using bilayered coarse-grained/nanocrystalline samples to determine the depth resolution. Digital image correlation of the Kikuchi patterns across grain boundaries is used to measure the lateral resolution. The depth resolutions of TKD in aluminium, copper and platinum at 30 kV for an untilted sample were 80, 32 and 14 nm respectively. These worsened with increasing sample backtilt and slightly improved with decreasing accelerating voltage. The best physical lateral resolution obtained was 6 nm, at 30 keV in a 41 nm thick aluminium sample with no backtilt. The lateral resolution worsened with increasing sample thickness and backtilt, contrasting with some previous reports. Accelerating voltage and atomic number did not have a significant impact on the measured lateral resolution within the scatter in the data.

Fusion crusts form during the atmospheric entry heating of meteorites and preserve a record of the conditions that occurred during deceleration in the atmosphere. The fusion crust of the Winchcombe meteorite closely resembles that of other stony meteorites, and in particular CM2 chondrites, since it is dominated by olivine phenocrysts set in a glassy mesostasis with magnetite, and is highly vesicular. Dehydration cracks are unusually abundant in Winchcombe. Failure of this weak layer is an additional ablation mechanism to produce large numbers of particles during deceleration, consistent with the observation of pulses of plasma in videos of the Winchcombe fireball. Calving events might provide an observable phenomenon related to meteorites that are particularly susceptible to dehydration. Oscillatory zoning is observed within olivine phenocrysts in the fusion crust, in contrast to other meteorites, perhaps owing to temperature fluctuations resulting from calving events. Magnetite monolayers are found in the crust, and have also not been previously reported, and form discontinuous strata. These features grade into magnetite rims formed on the external surface of the crust and suggest the trapping of surface magnetite by collapse of melt. Magnetite monolayers may be a feature of meteorites that undergo significant degassing. Silicate warts with dendritic textures were observed and are suggested to be droplets ablated from another stone in the shower. They, therefore, represent the first evidence for intershower transfer of ablation materials and are consistent with the other evidence in the Winchcombe meteorite for unusually intense gas loss and ablation, despite its low entry velocity.

Journal Article High-temperature EDS and EBSD Analysis – Enabling In Situ Heating for Direct Observation of Phase Transformations in the SEM Get access Haithem Mansour, Haithem Mansour Oxford Instruments NanoAnalysis, High Wycombe, United Kingdom Corresponding author: Haithem.mansour@oxinst.com Search for other works by this author on: Oxford Academic Google Scholar Simon Burgess, Simon Burgess Oxford Instruments NanoAnalysis, High Wycombe, United Kingdom Search for other works by this author on: Oxford Academic Google Scholar Patrick Trimby, Patrick Trimby Oxford Instruments NanoAnalysis, High Wycombe, United Kingdom Search for other works by this author on: Oxford Academic Google Scholar Kim Larsen, Kim Larsen Oxford Instruments NanoAnalysis, High Wycombe, United Kingdom Search for other works by this author on: Oxford Academic Google Scholar Jack Donoghue, Jack Donoghue Henry Royce Institute, Department of Materials, The University of Manchester, United Kingdom Search for other works by this author on: Oxford Academic Google Scholar Jiaqi Xu, Jiaqi Xu Henry Royce Institute, Department of Materials, The University of Manchester, United Kingdom Search for other works by this author on: Oxford Academic Google Scholar Albert Smith Albert Smith TESCAN-UK, Cambridge, United Kingdom Search for other works by this author on: Oxford Academic Google Scholar Microscopy and Microanalysis, Volume 29, Issue Supplement_1, 1 August 2023, Pages 2085–2086, https://doi.org/10.1093/micmic/ozad067.1079 Published: 22 July 2023

Deformation is a near ubiquitous process that is observed within nearly all naturally forming rocks. Electron backscatter diffraction (EBSD) is a technique that enables slip‐systems (a form of plastic deformation) to be inferred from intracrystalline misorientations at a comparable scale to the representative CPO analysis (≥300 crystals for the nakhlites). Extensive laboratory and studies on naturally occurring samples have identified preferential mantle condition extrinsic parameters for specific slip‐system signatures within olivine and clinopyroxene. Intracrystalline misorientation patterns for olivine and augite (high Ca‐clinopyroxene) for 16 different Martian nakhlite meteorites (21 sections) were analyzed and assessed against these known parameters. Investigation of high and low deformation regions within the nakhlites revealed a shift in intracrystalline misorientation patterns for 10 of the 21 sections. Interpreted as both shock (high deformations) and emplacement (low deformation) signatures, the observed variations in deformation patterns for the two main regimes of deformation indicate heterogeneous sampling of the nakhlite source crater. Our findings indicate that shock deformation is prevalent throughout the nakhlites, and that great care needs to be taken when interpreting intracrystalline misorientations of crystals within apparent lower deformation regions.

The Martian nakhlite meteorites, which represent multiple events that belong to a single magma source region represent a key opportunity to study the evolution of Martian petrogenesis. Here 16 of the 26 identified nakhlite specimens are studied using coupled electron backscatter diffraction (EBSD) and emplacement end‐member calculations. EBSD was used to determine shape preferred orientation of contained augite (high Ca‐clinopyroxene) phenocrysts by considering their crystallographic preferred orientation (CPO). Parameters derived from EBSD, and energy dispersive X‐ray spectroscopy spectra were used in basic emplacement models to assess their dominant mechanism against three end‐member scenarios: thermal diffusion, crystal settling, and crystal convection. Results from CPO analyses indicate low intensity weak‐moderate CPO. In all samples, a consistent foliation within the <001> axes of augite are observed typically coupled with a weaker lineation CPO in one of the other crystallographic axes. These CPO results agree best with crystal settling being the dominant emplacement mechanism for the nakhlites. Modeled crystal settling results identify two distinguishable groups outside of the model's resolution indicating the presence of secondary emplacement mechanisms. Comparison of the two identified groups against CPO, geochemical, and age parameters indicate random variability between individual meteorites. Therefore, coupled CPO and emplacement modeling results identify an overarching characteristic of a dominant crystal settling emplacement mechanism for the nakhlite source volcano despite exhibiting random variation with each discharge through time.

Characterisation of cement clinkers is a prerequisite to optimise properties of cements and concretes. Therefore, the protocol to prepare and characterise cement clinkers using electron backscatter diffraction (EBSD) in combination with energy dispersive X-ray spectrometry (EDS) is described. It is shown that argon broad ion beam polishing delivers surfaces with high contrast electron backscatter diffraction patterns (EBSP). EBSD data quality in high and low vacuum SEM reveals that high vacuum conditions and state-of-the-art EBSD cameras deliver EBSPs of cement clinker at improved quality. Furthermore, exemplary EBSD-EDS analysis is discussed for two Portland cement clinkers. Results clearly show that differentiation between major phases can reliably be achieved. In addition, it is revealed that crystal distortion in belite is high. Analysis of C3A phases show that differentiation of orthorhombic and cubic poly morph is possible, and that Mg incorporation leads to amorphization. Results demonstrate that EBSD-EDS analysis allows reliable phase characterisation of cement clinkers.

Metal halide perovskite (MHP) solar cells have attracted worldwide research interest. Although it has been well established that grain, grain boundary, and grain facet affect MHPs optoelectronic properties, less is known about subgrain structures. Recently, MHP twin stripes, a subgrain feature, have stimulated extensive discussion due to the potential for both beneficial and detrimental effects of ferroelectricity on optoelectronic properties. Connecting the ferroic behavior of twin stripes in MHPs with crystal orientation will be a vital step to understand the ferroic nature and the effects of twin stripes. In this work, we studied the crystallographic orientation and ferroic properties of CH3NH3PbI3 twin stripes, using electron backscatter diffraction (EBSD) and advanced piezoresponse force microscopy (PFM), respectively. Using EBSD, we discovered that the orientation relationship across the twin walls in CH3NH3PbI3 is a 90° rotation about ⟨1̅1̅0⟩, with the ⟨030⟩ and ⟨111⟩ directions parallel to the direction normal to the surface. By careful inspection of CH3NH3PbI3 PFM results including in-plane and out-of-plane PFM measurements, we demonstrate some nonferroelectric contributions to the PFM responses of this CH3NH3PbI3 sample, suggesting that the PFM signal in this CH3NH3PbI3 sample is affected by nonferroelectric and nonpiezoelectric forces. If there is piezoelectric response, it is below the detection sensitivity of our interferometric displacement sensor PFM (<0.615 pm/V). Overall, this work offers an integrated picture describing the crystallographic orientations and the origin of PFM signal of MHPs twin stripes, which is critical to understanding the ferroicity in MHPs.