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Electron backscatter diffraction (EBSD) analysis enables a unique perspective of the internal microstructure of foraminiferal calcite. Specifically, EBSD provides crystallographic data from within the test, highlighting the highly organised “mesocrystal” structure of crystallographically aligned domains throughout the test, formed by sequential deposits of microgranular calcite. We compared EBSD maps across the test walls of both poorly preserved and well-preserved specimens of the planktonic foraminifera species Globigerinoides ruber and Morozovella crater. The EBSD maps, paired with information about intra-test distributions of Mg/Ca ratios, allowed us to examine the effects of different diagenetic processes on the foraminifera test. In poorly preserved specimens EBSD data show extensive reorganisation of the biogenic crystal microstructure, indicating differing phases of dissolution, re-precipitation and overgrowth. The specimens with the greatest degree of microstructural reorganisation also show an absence of higher concentration magnesium bands, which are typical features of well-preserved specimens. These findings provide important insights into the extent of post-depositional changes, in both microstructure and geochemical signals that must be considered when utilising foraminifera to generate proxy archive data.

Grain growth can modify the microstructure of natural ice, including the grain size and crystallographic preferred orientation (CPO). To better understand grain-growth processes and kinetics, we compared microstructural data from synthetic and natural ice samples of similar starting grain sizes that were annealed at the solidus temperature (0 ∘C) for durations of a few hours to 33 d. The synthetic ice has a homogeneous initial microstructure characterized by polygonal grains, little intragranular distortion, few bubbles, and a near-random CPO. The natural ice samples were subsampled from ice cores acquired from the Priestley Glacier, Antarctica. This natural ice has a heterogeneous microstructure characterized by a considerable number of air bubbles, widespread intragranular distortion, and a CPO. During annealing, the average grain size of the natural ice barely changes, whereas the average grain size of the synthetic ice gradually increases. These observations demonstrate that grain growth in natural ice can be much slower than in synthetic ice and therefore that the grain-growth law derived from synthetic ice cannot be directly applied to estimate the grain-size evolution in natural ice with a different microstructure. The microstructure of natural ice is characterized by many bubbles that pin grain boundaries. Previous studies suggest that bubble pinning provides a resisting force that reduces the effective driving force of grain-boundary migration and is therefore linked to the inhibition of grain growth observed in natural ice. As annealing progresses, the number density (number per unit area) of bubbles on grain boundaries in the natural ice decreases, whilst the number density of bubbles in the grain interiors increases. This observation indicates that some grain boundaries sweep through bubbles, which should weaken the pinning effect and thus reduce the resisting force for grain-boundary migration. Some of the Priestley ice grains become abnormally large during annealing. We speculate that the contrast of dislocation density amongst neighbouring grains, which favours the selected growth of grains with low dislocation densities, and bubble pinning, which inhibits grain growth, are tightly associated with abnormal grain growth. The upper 10 m of the Priestley ice core has a weaker CPO and better-developed second maximum than deeper samples. The similarity of this difference to the changes observed in annealing experiments suggests that abnormal grain growth may have occurred in the upper 10 m of the Priestley Glacier during summer warming.

Ice fabrics – the distribution of crystal orientations in a polycrystal – are key for understanding and predicting ice flow dynamics. Despite their importance, the characteristics and evolution of fabrics produced outside of the deformation regimes of pure and simple shear flow has largely been neglected, yet they are a common occurrence within ice sheets. Here, we use a recently developed numerical model (SpecCAF) to classify all fabrics produced over a continuous spectrum of incompressible two-dimensional deformation regimes and temperatures. The model has been shown to accurately predict ice fabrics produced in experiments, where the ice has been deformed in either uniaxial compression or simple shear. Here we use the model to reveal fabrics produced in regimes intermediate to pure and simple shear, as well as those that are more rotational than simple shear. We find that intermediate deformation regimes between pure and simple shear result in a smooth transition between a fabric characterised by a girdle and a secondary cluster pattern. Highly rotational deformation regimes are revealed to produce a weak girdle fabric. Furthermore, we provide regime diagrams to help constrain deformation conditions of measured ice fabrics. We also obtain predictions for the strain scales over which fabric evolution takes place at any given temperature. The use of our model in large-scale ice flow models and for interpreting fabrics observed in ice cores and seismic anisotropy provides new tools supporting the community in predicting and interpreting ice flow in a changing climate.

The flow properties of middle crustal rocks are commonly represented by viscous flow. Examples of pinch and swell structures found in a high strain zone at St. Anne Point (Fiordland, New Zealand) and Wongwibinda (N.S.W., Australia) suggest pinch and swell structures may be initiated by brittle failure of the more competent layer in conjunction with subsequent material softening. On this basis we develop a numerical model where Mohr–Coulomb constitutive strain localising behaviour is utilised to initiate pinch and swell structure development. Results show that pinch and swell structures develop in a competent layer in both Newtonian and non-Newtonian flow, provided the competent layer has sufficient viscosity contrast and can localise strain to form shear bands. The flow regime and strain localising characteristics of the surrounding country rock appear not to impact pinch and swell structure formation. The degree of material softening after the initial strain localising behaviour is shown to impact pinch and swell characteristics, while extensive material softening causes the formation of thick necks between swells by limiting the focused localisation of strain into shear bands. To aid analysis of the structures and help derive the flow properties of rocks in the field, we define three stages of pinch and swell development and offer suggestions for measurements to be made in the field. Our study suggests that Mohr–Coulomb strain localising behaviour combined with viscous flow is a viable alternative representation of the heterogeneous rheological behaviour of rocks seen in the middle crust. This type of mid-crustal rheological behaviour can have significant influence on the localisation of strain at all scales. For example, inclusion of Mohr–Coulomb strain localising behaviour with viscous flow in just some mid-crustal layers within a crustal-scale model can result in significant strain localisation, extending from the upper crust into the middle crust. This localisation also influences the development of near-surface structures.

This study focuses on physiochemical processes occurring in a brittle–ductile shear zone at both fluid-present and fluid-limited conditions. In the studied shear zone (Wyangala, SE Australia), a coarse-grained two-feldspar–quartz–biotite granite is transformed into a medium-grained orthogneiss at the shear zone margins and a fine-grained quartz–muscovite phyllonite in the central parts. The orthogneiss displays cataclasis of feldspar and crystal-plastic deformation of quartz. Quartz accommodates most of the deformation and is extensively recrystallized, showing distinct crystallographic preferred orientation (CPO). Feldspar-to-muscovite, biotite-to-muscovite and albitization reactions occur locally at porphyroclasts' fracture surfaces and margins. However, the bulk rock composition shows very little change in respect to the wall rock composition. In contrast, in the shear zone centre quartz occurs as large, weakly deformed porphyroclasts in sizes similar to that in the wall rock, suggesting that it has undergone little deformation. Feldspars and biotite are almost completely reacted to muscovite, which is arranged in a fine-grained interconnected matrix. Muscovite-rich layers contain significant amounts of fine-grained intermixed quartz with random CPO. These domains are interpreted to have accommodated most of the strain. Bulk rock chemistry data show a significant increase in SiO2 and depletion in NaO content compared to the wall rock composition. We suggest that the high- and low-strain microstructures in the shear zone represent markedly different scenarios and cannot be interpreted as a simple sequential development with respect to strain. Instead, we propose that the microstructural and mineralogical changes in the shear zone centre arise from a local metasomatic alteration around a brittle precursor. When the weaker fine-grained microstructure is established, the further flow is controlled by transient porosity created at (i) grain boundaries in fine-grained areas deforming by grain boundary sliding (GBS) and (ii) transient dilatancy sites at porphyroclast–matrix boundaries. Here a growth of secondary quartz occurs from incoming fluid, resulting in significant changes in bulk composition and eventually rheological hardening due to the precipitation-related increase in the mode and grain size of quartz. In contrast, within the shear zone margins the amount of fluid influx and associated reactions is limited; here deformation mainly proceeds by dynamic recrystallization of the igneous quartz grains. The studied shear zone exemplifies the role of syn-deformational fluids and fluid-induced reactions on the dominance of deformation processes and subsequent contrasting rheological behaviour at micron to metre scale.

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., Competing Interests: Declaration of competing interest The authors declare the following financial interests/personal relationships which may be considered as potential competing interests: Patrick Trimby reports a relationship with Oxford Instruments NanoAnalysis that includes: employment., (Copyright © 2024 Elsevier B.V. All rights reserved.)

Orogenic gold deposits are comprised of complex quartz vein arrays that form as a result of fluid flow along transcrustal fault zones in active orogenic belts. Mineral precipitation in these deposits occurs under variable pressure conditions, but a mechanism explaining how the pressure regimes evolve through time has not previously been proposed. Here we show that extensional quartz veins at the Garrcon deposit in the Abitibi greenstone belt of Canada preserve petrographic characteristics suggesting that the three recognized paragenetic stages formed within different pressure regimes. The first stage involved the growth of interlocking quartz grains competing for space in fractures held open by hydrothermal fluids at supralithostatic pressures. Subsequent fluid flow at fluctuating pressure conditions caused recrystallization of the vein quartz and the precipitation of sulfide minerals through wall-rock sulfidation, with some of the sulfide minerals containing microscopic gold. These pressure fluctuations between supralithostatic to near-hydrostatic conditions resulted in the post-entrapment modification of the fluid inclusion inventory of the quartz. Late fluid flow occurred at near-hydrostatic conditions and resulted in the formation of fluid inclusions that have not been affected by post-entrapment modification as pressure conditions never returned to supralithostatic conditions. This late fluid flow is interpreted to have formed the texturally late, coarse native gold that occurs along quartz grain boundaries and in open spaces. The systematic evolution of the pressure regimes in orogenic gold deposits such as Garrcon can be explained by relative movement of fault-fracture meshes across the base of the upper crustal brittle-ductile transition zone. We conclude that early vein quartz in orogenic deposits is precipitated at near-lithostatic conditions whereas the paragenetically late gold is introduced at distinctly lower pressure., (© 2022. The Author(s).)

Antigorite serpentinite is expected to occur in parts of subduction plate boundaries, and may suppress earthquake slip, but the dominant deformation mechanisms and resultant rheology of antigorite are unclear. An exhumed plate boundary shear zone exposed near Nagasaki, Japan, contains antigorite deformed at 474°C ± 30°C. Observations indicate that a foliation defined by (001) crystal facets developed during plate-boundary shear. Microstructures indicating grain-scale dissolution at high-stress interfaces and precipitation in low-stress regions suggest that dissolution-precipitation creep contributed to foliation development. Analysis of crystal orientations indicate a small contribution from dislocation activity. We suggest a frictional-viscous rheology for antigorite, where dissolution-precipitation produces a foliation defined by (001) crystal facets and acts to resolve strain incompatibilities, allowing for efficient face-to-face sliding between facets. This rheology can not only explain aseismic behavior at ambient plate boundary conditions, but also some of the contrasting behaviors shown by previous field and laboratory studies., (© 2022. The Authors.)

When hydrated, phosphides such as the mineral schreibersite, (Fe,Ni) 3 P, allow for the synthesis of important phosphorus-bearing organic compounds. Such phosphides are common accessory minerals in meteorites; consequently, meteorites are proposed to be a main source of prebiotic reactive phosphorus on early Earth. Here, we propose an alternative source for widespread phosphorus reduction, arguing that lightning strikes on early Earth potentially formed 10-1000 kg of phosphide and 100-10,000 kg of phosphite and hypophosphite annually. Therefore, lightning could have been a significant source of prebiotic, reactive phosphorus which would have been concentrated on landmasses in tropical regions. Lightning strikes could likewise provide a continual source of prebiotic reactive phosphorus independent of meteorite flux on other Earth-like planets, potentially facilitating the emergence of terrestrial life indefinitely.

Nakhlite meteorites are ~1.4 to 1.3 Ga old igneous rocks, aqueously altered on Mars ~630 Ma ago. We test the theory that water-rock interaction was impact driven. Electron backscatter diffraction demonstrates that the meteorites Miller Range 03346 and Lafayette were heterogeneously deformed, leading to localized regions of brecciation, plastic deformation, and mechanical twinning of augite. Numerical modeling shows that the pattern of deformation is consistent with shock-generated compressive and tensile stresses. Mesostasis within shocked areas was aqueously altered to phyllosilicates, carbonates, and oxides, suggesting a genetic link between the two processes. We propose that an impact ~630 Ma ago simultaneously deformed the nakhlite parent rocks and generated liquid water by melting of permafrost. Ensuing water-rock interaction focused on shocked mesostasis with a high density of reactive sites. The nakhlite source location must have two spatially correlated craters, one ~630 Ma old and another, ejecting the meteorites, ~11 Ma ago.

The metamorphic conditions and mechanisms required to induce foundering in deep arc crust are assessed using an example of representative lower crust in SW New Zealand. Composite plutons of Cretaceous monzodiorite and gabbro were emplaced at ~1.2 and 1.8 GPa are parts of the Western Fiordland Orthogneiss (WFO); examples of the plutons are tectonically juxtaposed along a structure that excised ~25 km of crust. The 1.8 GPa Breaksea Orthogneiss includes suitably dense minor components (e.g. eclogite) capable of foundering at peak conditions. As the eclogite facies boundary has a positive dP/dT, cooling from supra-solidus conditions (T > 950 ºC) at high-P should be accompanied by omphacite and garnet growth. However, a high monzodioritic proportion and inefficient metamorphism in the Breaksea Orthogneiss resulted in its positive buoyancy and preservation. Metamorphic inefficiency and compositional relationships in the 1.2 GPa Malaspina Pluton meant it was never likely to have developed densities sufficiently high to founder. These relationships suggest that the deep arc crust must have primarily involved significant igneous accumulation of garnet-clinopyroxene (in proportions >75%). Crustal dismemberment with or without the development of extensional shear zones is proposed to have induced foundering of excised cumulate material at P > 1.2 GPa.

One of the challenges in microstructure analysis nowadays resides in the reliable and accurate characterization of ultra-fine grained (UFG) and nanocrystalline materials. The traditional techniques associated with scanning electron microscopy (SEM), such as electron backscatter diffraction (EBSD), do not possess the required spatial resolution due to the large interaction volume between the electrons from the beam and the atoms of the material. Transmission electron microscopy (TEM) has the required spatial resolution. However, due to a lack of automation in the analysis system, the rate of data acquisition is slow which limits the area of the specimen that can be characterized. This paper presents a new characterization technique, Transmission Kikuchi Diffraction (TKD), which enables the analysis of the microstructure of UFG and nanocrystalline materials using an SEM equipped with a standard EBSD system. The spatial resolution of this technique can reach 2 nm. This technique can be applied to a large range of materials that would be difficult to analyze using traditional EBSD. After presenting the experimental set up and describing the different steps necessary to realize a TKD analysis, examples of its use on metal alloys and minerals are shown to illustrate the resolution of the technique and its flexibility in term of material to be characterized.

The application of atom probe tomography to the study of minerals is a rapidly growing area. Picosecond-pulsed, ultraviolet laser (UV-355 nm) assisted atom probe tomography has been used to analyze trace element mobility within dislocations and low-angle boundaries in plastically deformed specimens of the nonconductive mineral zircon (ZrSiO4), a key material to date the earth's geological events. Here we discuss important experimental aspects inherent in the atom probe tomography investigation of this important mineral, providing insights into the challenges in atom probe tomography characterization of minerals as a whole. We studied the influence of atom probe tomography analysis parameters on features of the mass spectra, such as the thermal tail, as well as the overall data quality. Three zircon samples with different uranium and lead content were analyzed, and particular attention was paid to ion identification in the mass spectra and detection limits of the key trace elements, lead and uranium. We also discuss the correlative use of electron backscattered diffraction in a scanning electron microscope to map the deformation in the zircon grains, and the combined use of transmission Kikuchi diffraction and focused ion beam sample preparation to assist preparation of the final atom probe tip.

Deformation microstructures are widely used for reconstructing tectono-metamorphic events recorded in rocks. In crustal settings deformation is often accompanied and/or succeeded by fluid infiltration and dissolution-precipitation reactions. However, the microstructural consequences of dissolution-precipitation in minerals have not been investigated experimentally. Here we conducted experiments where KBr crystals were reacted with a saturated KCl-H 2 O fluid. The results show that reaction products, formed in the absence of deformation, inherit the general crystallographic orientation from their parents, but also display a development of new microstructures that are typical in deformed minerals, such as apparent bending of crystal lattices and new subgrain domains, separated by low-angle and, in some cases, high-angle boundaries. Our work suggests that fluid-mediated dissolution-precipitation reactions can lead to a development of potentially misleading microstructures. We propose a set of criteria that may help in distinguishing such microstructures from the ones that are created by crystal-plastic deformation., Competing Interests: The authors declare no competing financial interests.

Geochemical signatures throughout the layered Earth require significant mass transfer through the lower crust, yet geological pathways are under-recognized. Elongate bodies of basic to ultrabasic rocks are ubiquitous in exposures of the lower crust. Ultrabasic hornblendite bodies hosted within granulite facies gabbroic gneiss of the Pembroke Valley, Fiordland, New Zealand, are typical occurrences usually reported as igneous cumulate hornblendite. Their igneous features contrast with the metamorphic character of their host gabbroic gneiss. Both rock types have a common parent; field relationships are consistent with modification of host gabbroic gneiss into hornblendite. This precludes any interpretation involving cumulate processes in forming the hornblendite; these bodies are imposter cumulates. Instead, replacement of the host gabbroic gneiss formed hornblendite as a result of channeled high melt flux through the lower crust. High melt/rock ratios and disequilibrium between the migrating magma (granodiorite) and its host gabbroic gneiss induced dissolution (grain-scale magmatic assimilation) of gneiss and crystallization of mainly hornblende from the migrating magma. The extent of this reaction-replacement mechanism indicates that such hornblendite bodies delineate significant melt conduits. Accordingly, many of the ubiquitous basic to ultrabasic elongate bodies of the lower crust likely map the 'missing' mass transfer zones.

Diamonds and their inclusions are unique probes into the deep Earth, tracking the deep carbon cycle to >800 km. Understanding the mechanisms of carbon mobilization and freezing is a prerequisite for quantifying the fluxes of carbon in the deep Earth. Here we show direct evidence for the formation of diamond by redox reactions involving FeNi sulfides. Transmission Kikuchi Diffraction identifies an arrested redox reaction from pyrrhotite to magnetite included in diamond. The magnetite corona shows coherent epitaxy with relict pyrrhotite and diamond, indicating that diamond nucleated on magnetite. Furthermore, structures inherited from h-Fe3O4 define a phase transformation at depths of 320-330 km, the base of the Kaapvaal lithosphere. The oxidation of pyrrhotite to magnetite is an important trigger of diamond precipitation in the upper mantle, explaining the presence of these phases in diamonds.

Trace elements diffuse negligible distances through the pristine crystal lattice in minerals: this is a fundamental assumption when using them to decipher geological processes. For example, the reliable use of the mineral zircon (ZrSiO4) as a U-Th-Pb geochronometer and trace element monitor requires minimal radiogenic isotope and trace element mobility. Here, using atom probe tomography, we document the effects of crystal-plastic deformation on atomic-scale elemental distributions in zircon revealing sub-micrometre-scale mechanisms of trace element mobility. Dislocations that move through the lattice accumulate U and other trace elements. Pipe diffusion along dislocation arrays connected to a chemical or structural sink results in continuous removal of selected elements (for example, Pb), even after deformation has ceased. However, in disconnected dislocations, trace elements remain locked. Our findings have important implications for the use of zircon as a geochronometer, and highlight the importance of deformation on trace element redistribution in minerals and engineering materials.

Investigations of the Mantle Transition Zone (MTZ; 410-660 km deep) by deformation experiments and geophysical methods suggest that the MTZ has distinct rheological properties, but their exact cause is still unclear due to the lack of natural samples. Here we present the first direct evidence for crystal-plastic deformation by dislocation creep in the MTZ using a chromitite from the Luobusa peridotite (E. Tibet). Chromite grains show exsolution of diopside and SiO2, suggesting previous equilibration in the MTZ. Electron backscattered diffraction (EBSD) analysis reveals that olivine grains co-existing with exsolved phases inside chromite grains and occurring on chromite grain boundaries have a single pronounced crystallographic preferred orientation (CPO). This suggests that olivine preserves the CPO of a high-pressure polymorph (wadsleyite) before the high-pressure polymorph of chromite began to invert and exsolve. Chromite also shows a significant CPO. Thus, the fine-grained high-pressure phases were deformed by dislocation creep in the MTZ. Grain growth in inverted chromite produced an equilibrated microstructure during exhumation to the surface, masking at first sight its MTZ deformation history. These unique observations provide a window into the deep Earth, and constraints for interpreting geophysical signals and their geodynamic implications in a geologically robust context.

Electron backscatter diffraction (EBSD) on ice is a decade old. We have built upon previous work to select and develop methods of sample preparation and analysis that give >90% success rate in obtaining high-quality EBSD maps, for the whole surface area (potentially) of low porosity (<15%) water ice samples, including very fine-grained (<10 μm) and very large (up to 70 mm by 30 mm) samples. We present and explain two new methods of removing frost and providing a damage-free surface for EBSD: pressure cycle sublimation and 'ironing'. In general, the pressure cycle sublimation method is preferred as it is easier, faster and does not generate significant artefacts. We measure the thermal effects of sample preparation, transfer and storage procedures and model the likelihood of these modifying sample microstructures. We show results from laboratory ice samples, with a wide range of microstructures, to illustrate effectiveness and limitations of EBSD on ice and its potential applications. The methods we present can be implemented, with a modest investment, on any scanning electron microscope system with EBSD, a cryostage and a variable pressure capability., (© 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.)