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Zircon grains preserve records of crystallization, growth, and/or deformation that can be envisaged from their internal structures and through the U–Pb isotope analysis. Electron backscatter diffraction (EBSD) is a non-destructive method for visualizing undeformed domains to differentiate them from those that are plastically deformed. In this study, we report EBSD analyses conducted on zircon grains, in thin sections with available textural information, from Himalayan eclogites. The studied eclogite samples show no petrographic evidence of shearing or mylonitization. However, several zircon grains preserve plastically deformed domains. These deformed domains display several degrees of misorientation relative to the undeformed domain and yielded geologically reset ages when analysed for U–Pb isotope ratios using nanoscale secondary ion mass spectrometry (NanoSIMS), in contrast to most undeformed domains which retained the protolith age. The degree of resetting is positively correlated with the extent of misorientation. These pieces of evidence indicate that plastic deformation in zircon grains, equilibrated at higher pressure–temperature conditions, affected the primary geochemical and geochronological records. Based on these observations, we assume that not only regional shearing/mylonitization in metamorphic rocks affects the geochemical records, but also that zircon grains in apparently unsheared high-grade metamorphic rocks behave plastically. The micro-scale intra-grain plastically deformed domains can easily be identified through EBSD analysis in the form of crystallographic misorientations. To extract meaningful geochronological results, it is necessary to identify undisturbed domains in zircon grains before applying any destructive analytical method.

We report a comprehensive data set characterizing and quantifying the geometrically necessary dislocation (GND) density in the crystallographic frame (ραc) and disclination density (ρθ) in fine-grained polycrystalline olivine deformed in uniaxial compression or torsion, at 1000 and 1200 ∘C, under a confining pressure of 300 MPa. Finite strains range from 0.11 up to 8.6 %, and stresses reach up to 1073 MPa. The data set is a selection of 19 electron backscatter diffraction maps acquired with conventional angular resolution (0.5∘) but at high spatial resolution (step size ranging between 0.05 and 0.1 µm). Thanks to analytical improvement for data acquisition and treatment, notably with the use of ATEX (Analysis Tools for Electron and X-ray diffraction) software, we report the spatial distribution of both GND and disclination densities. Areas with the highest GND densities define sub-grain boundaries. The type of GND densities involved also indicates that most olivine sub-grain boundaries have a mixed character. Moreover, the strategy for visualization also permits identifying minor GND that is not well organized as sub-grain boundaries yet. A low-temperature and high-stress sample displays a higher but less organized GND density than in a sample deformed at high temperature for a similar finite strain, grain size, and identical strain rate, confirming the action of dislocation creep in these samples, even for micrometric grains (2 µm). Furthermore, disclination dipoles along grain boundaries are identified in every undeformed and deformed electron backscatter diffraction (EBSD) map, mostly at the junction of a grain boundary with a sub-grain but also along sub-grain boundaries and at sub-grain boundary tips. Nevertheless, for the range of experimental parameters investigated, there is no notable correlation of the disclination density with stress, strain, or temperature. However, a broad positive correlation between average disclination density and average GND density per grain is found, confirming their similar role as defects producing intragranular misorientation. Furthermore, a broad negative correlation between the disclination density and the grain size or perimeter is found, providing a first rule of thumb on the distribution of disclinations. Field dislocation and disclination mechanics (FDDM) of the elastic fields due to experimentally measured dislocations and disclinations (e.g., strains/rotations and stresses) provides further evidence of the interplay between both types of defects. At last, our results also support that disclinations act as a plastic deformation mechanism, by allowing rotation of a very small crystal volume.

Earth's long-term cycling of carbon is regulated from mid-ocean ridges to convergent plate boundaries by mass transfers involving mantle rocks. Here we examine the conversion of peridotite to listvenite (magnesite + quartz rock) during CO2 metasomatism along the basal thrust of the Semail Ophiolite (Fanja, Sultanate of Oman). At the outcrop scale, this transformation defines reaction zones, from serpentinized peridotites to carbonated serpentinites and listvenites. Based on a detailed petrological and chemical study, we show that carbonation progressed through three main stages involving the development of replacive textures ascribed to early stages, whilst carbonate (± quartz) veining becomes predominant in the last stage. The pervasive replacement of serpentine by magnesite is characterized by the formation of spheroids, among which two types are identified based on the composition of their core regions: Fe-core and Mg-core spheroids. Fe zoning is a type feature of matrix and vein magnesite formed during the onset carbonation (Stage 1). While Fe-rich magnesite is predicted to form at low fluid XCO2 from a poorly to moderately oxidized protolith, our study evidences that the local non-redox destabilization of Fe oxides into Fe-rich magnesite is essential to the development of Fe-core spheroids. The formation of Fe-core spheroids is followed by the pervasive (over-)growth of Mg-rich spheroids and aggregates (Stage 2) at near-equilibrium conditions in response to increasing fluid XCO2. Furthermore, the compositions of carbonates indicate that most siderophile transition elements released by the dissolution of primary minerals are locally trapped in carbonate and oxides during matrix carbonation, while elements with a chalcophile affinity are the most likely to be leached out of reaction zones.

Abstract Amphibole‐rich rocks constitute significant components of the mid‐ to lower continental crust, particularly in active orogens characterized with thick and hot crusts. Nevertheless, experimental data on their viscosity remain scarce. We conducted axial compression deformation experiments on synthetic amphibolites under temperature and pressure conditions resembling deep sections of overthickened crust. A novel flow law for a calcic‐amphibole‐rich rock (80% amphibole +20% garnet) in the dislocation creep regime is derived from these experiments. Contrary to common assumptions, our results reveal that calcic‐amphibolite is 1‐2 orders of magnitude weaker than plagioclase‐rich amphibolite, granulite, or gabbro. A calcic‐amphibole‐rich, low viscosity deep crust may not only support the “channel flow” model proposed for the Tibetan Plateau but also explain the observed high crustal seismic anisotropy in the region.

Melt transport mechanisms have an important impact on the chemical composition of the percolated host rock and the migrating melts. Melt migration is usually assumed to occur at grain boundaries. However, microstructural studies revealed the occurrence of polyphase inclusions along dislocations, subgrain boundaries and microcracks in single mineral grains. The inclusions are interpreted as crystallized melt pockets suggesting that melts can migrate within deformed crystals. Intracrystalline melt migration and diffusive re-equilibration can lead to significant mineral trace element enrichments when associated with dissolution–precipitation reactions. In this contribution, we study a body of replacive troctolites associated with the Erro-Tobbio ophiolitic mantle peridotites (Ligurian Alps, Italy). The replacive formation of the olivine-rich troctolite involved extensive impregnation of a dunitic matrix, i.e. partial dissolution of olivine and concomitant crystallization of interstitial phases. The olivine matrix is characterized by two distinct olivine textures: (i) coarse deformed olivine, representing relicts of the pre-existing mantle dunite matrix (olivine1), and (ii) fine-grained undeformed olivine, a product of the melt–rock interaction process (olivine2). Previous studies documented a decoupling between olivine texture and trace element composition, namely enriched trace element compositions in olivine1 rather than in olivine2, as would be expected from the dissolution–precipitation process. Notably, the trace element enrichments in deformed olivines are correlated with the occurrence of elongated 10 µm size polyphase inclusions (clinopyroxene, Ti-pargasite, chromite) preferentially oriented along olivine crystallographic axes. These inclusions show irregular contacts and have no crystallographic preferred orientation with the host olivine, and the phases composing the inclusions show similar chemical compositions to the vermicular phases formed at the grain boundaries during late-stage reactive crystallization of the troctolite. This suggests that the investigated inclusions did not form as exsolutions of the host olivine but rather by input of metasomatic fluids percolating through the deformed olivine grains during closure of the magmatic system. We infer that strongly fractionated volatile-rich melts were incorporated in oriented microfractures within olivine1 and led to the crystallization of the polyphase inclusions. The presence of intracrystalline melt greatly enhanced diffusive re-equilibration between the evolved melt and the percolated olivine1, in turn acquiring the enriched character expected in neoformed olivine crystals. Intracrystalline melt percolation can have strong geochemical implications and can lead to efficient re-equilibration of percolated minerals and rocks.

Torsion experiments were performed in polycrystalline ice at high temperature (0.97 Tm) to reproduce the simple shear kinematics that are believed to dominate in ice streams and at the base of fast-flowing glaciers. As clearly documented more than 30 years ago, under simple shear ice develops a two-maxima c axis crystallographic preferred orientation (CPO), which evolves rapidly into a single cluster CPO with a c axis perpendicular to the shear plane. Dynamic recrystallization mechanisms that occur in both laboratory conditions and naturally deformed ice are likely candidates to explain the observed CPO evolution. In this study, we use electron backscatter diffraction (EBSD) and automatic ice texture analyzer (AITA) to characterize the mechanisms accommodating deformation, the stress and strain heterogeneities that form under torsion of an initially isotropic polycrystalline ice sample at high temperature, and the role of dynamic recrystallization in accommodating these heterogeneities. These analyses highlight an interlocking microstructure, which results from heterogeneity-driven serrated grain boundary migration, and sub-grain boundaries composed of dislocations with a [c]-component Burgers vector, indicating that strong local stress heterogeneity develops, in particular, close to grain boundaries, even at high temperature and high finite shear strain. Based on these observations, we propose that nucleation by bulging, assisted by sub-grain boundary formation and followed by grain growth, is a very likely candidate to explain the progressive disappearance of the c axis CPO cluster at low angle to the shear plane and the stability of the one normal to it. We therefore strongly support the development of new polycrystal plasticity models limiting dislocation slip on non-basal slip systems and allowing for efficient accommodation of strain incompatibilities by an association of bulging and formation of sub-grain boundaries with a significant [c] component.

During the last decade pulverized rocks have been described on outcrops along large active faults and attributed to damage related to a propagating seismic rupture front. Questions remain concerning the maximal lateral distance from the fault plane and maximal depth for dynamic damage to be imprinted in rocks. In order to document these questions, a representative core sample of granodiorite located 51.3 m from the Nojima fault (Japan) that was drilled after the Hyogo-ken Nanbu (Kobe) earthquake is studied by using electron backscattered diffraction (EBSD) and high-resolution X-ray Laue microdiffraction. Although located outside of the Nojima damage fault zone and macroscopically undeformed, the sample shows pervasive microfractures and local fragmentation. These features are attributed to the first stage of seismic activity along the Nojima fault characterized by laumontite as the main sealing mineral. EBSD mapping was used in order to characterize the crystallographic orientation and deformation microstructures in the sample, and X-ray microdiffraction was used to measure elastic strain and residual stresses on each point of the mapped quartz grain. Both methods give consistent results on the crystallographic orientation and show small and short wavelength misorientations associated with laumontite-sealed microfractures and alignments of tiny fluid inclusions. Deformation microstructures in quartz are symptomatic of the semi-brittle faulting regime, in which low-temperature brittle plastic deformation and stress-driven dissolution-deposition processes occur conjointly. This deformation occurred at a 3.7–11.1 km depth interval as indicated by the laumontite stability domain. Residual stresses are calculated from deviatoric elastic strain tensor measured using X-ray Laue microdiffraction using the Hooke's law. The modal value of the von Mises stress distribution is at 100 MPa and the mean at 141 MPa. Such stress values are comparable to the peak strength of a deformed granodiorite from the damage zone of the Nojima fault. This indicates that, although apparently and macroscopically undeformed, the sample is actually damaged. The homogeneously distributed microfracturing of quartz is the microscopically visible imprint of this damage and suggests that high stresses were stored in the whole sample and not only concentrated on some crystal defects. It is proposed that the high residual stresses are the sum of the stress fields associated with individual dislocations and dislocation microstructures. These stresses are interpreted to be originated from the dynamic damage related to the propagation of rupture fronts or seismic waves at a depth where confining pressure prevented pulverization. Actually, M6 to M7 earthquakes occurred during the Paleocene on the Nojima fault and are good candidates for inducing this dynamic damage. The high residual stresses and the deformation microstructures would have contributed to the widening of the damaged fault zone with additional large earthquakes occurring on the Nojima fault.

This study presents a unique database of 172 plagioclase Crystallographic Preferred Orientations (CPO) of variously deformed gabbroic rocks. The CPO characteristics as a function of the deformation regime (magmatic or crystal-plastic) are outlined and discussed. The studied samples are dominantly from slow- and fast-spread present-day ocean crust, as well as from the Oman ophiolite. Plagioclase is the dominant mineral phase in the studied samples. Plagioclase CPOs are grouped into three main categories: Axial-B, a strong point alignment of (010) with a girdle distribution of [100]; Axial-A, a strong point maximum concentration of [100] with parallel girdle distributions of (010) and (001); and P-type, point maxima of [100], (010), and (001). A majority of CPO patterns are Axial-B and P-type, in samples showing either magmatic or crystal-plastic deformation textures. Axial-A CPOs are less common; they represent 21% of the samples deformed by crystal-plastic flow. Although fabric strength (ODF J index) does not show any consistent variation as a function of the CPO patterns, there is a significant difference in the relationship between the ODF and pole figures J indices; the magmatic type microstructures have high (010) pole figures J indices, which increase linearly with ODF J index, whereas the high [100] pole figures J indices of plastically deformed samples vary in a more scattered manner with ODF J index. The multistage nature of plastic deformation superposed on a magmatic structure compared with magmatic flow, and the large number of possible slip-systems in plagioclase probably account for these differences. Calculated seismic properties (P wave and S wave velocities and anisotropies) of plagioclase aggregates show that anisotropy (up to 12% for P wave and 14% for S wave) tends to increase as a function of ODF J index. In comparison with the olivine 1998 CPO database, the magnitude of P wave anisotropy for a given J index is much less than olivine, whereas it is similar for S wave anisotropy. Despite a large variation of fabric patterns and geodynamic setting, seismic properties of plagioclase-rich rocks have similar magnitudes of anisotropy. There is a small difference in the aggregate elastic symmetry, with magmatic microstructures having higher orthorhombic and hexagonal components, whereas plastic deformation microstructures have a slightly higher monoclinic component, possibly correlated with predominant monoclinic simple shear flow in plastically deformed samples. Overall, plots for CPO strength (ODF J index), pole figure strength, CPO symmetry and seismic anisotropy show significant scattering. This could be related to sampling statistics, although our database is a factor of ten higher than the olivine database of 1998, or it could be related to the low symmetry (triclinic) structure of plagioclase resulting in the addition of degrees of freedom in the processes creating the CPOs.

No abstract available.

In this paper, we propose a novel approach to reason with spatial proximity. The approach is based on contextual information and uses a neurofuzzy classifier to handle the uncertainty aspect of proximity. Neurofuzzy systems are a combination of neural networks and fuzzy systems and incorporate the advantages of both techniques. Although fuzzy systems are focused on knowledge representation, they do not allow the estimation of membership functions. Conversely, neuronal networks use powerful learning techniques but they are not able to explain how results are obtained. Neurofuzzy systems benefit from both techniques by using training data to generate membership functions and by using fuzzy rules to represent expert knowledge. Moreover, contextual information is collected from a knowledge base. The complete solution that we propose is integrated in a GIS, enhancing it with proximity reasoning. From an application perspective, the proposed approach was used in the telecommunication domain and particularly in fiber optic monitoring systems. In such systems, a user needs to qualify the distance between a fiber break and the surrounding objects of the environment to optimize the assignment of emergency crews. The neurofuzzy classifier has been used to compute the membership function parameters of the contextual information inputs using a training data set and fuzzy rules.

Contact and multiple cyclic twins of cassiterite commonly form in SnO 2 -based ceramics when SnO 2 is sintered with small additions of cobalt and niobium oxides (dual doping). In this work, it is shown that the formation of twins is a two-stage process that starts with epitaxial growth of SnO 2 on CoNb 2 O 6 and Co 4 Nb 2 O 9 seeds (twin nucleation stage) and continues with the fast growth of (101) twin contacts (twin growth stage). Both secondary phases form below the temperature of enhanced densification and SnO 2 grain growth; CoNb 2 O 6 forms at ∼700°C and Co 4 Nb 2 O 9 at ∼900°C. They are structurally related to the rutile-type cassiterite and can thus trigger oriented (epitaxial) growth (local recrystallization) of SnO 2 domains in different orientations on a single seed particle. While oriented growth of cassiterite on columbite-type CoNb 2 O 6 grains can only result in the formation of contact twins, the Co 4 Nb 2 O 9 grains with a structure comparable with that of corundum represent suitable sites for the nucleation of contact and multiple cyclic twins with coplanar or alternating morphology. The twin nucleation stage is followed by fast densification accompanied by significant SnO 2 grain growth above 1300°C. The twin nuclei coarsen to large twinned grains as a result of the preferential and fast growth of the low-energy (101) twin contacts. The solid-state diffusion processes during densification and SnO 2 grain growth are controlled by the formation of point defects and result in the dissolution of the twin nuclei and the incorporation of Nb 5+ and Co 2+ ions into the SnO 2 matrix in the form of a solid solution. In this process, the twin nuclei are erased and their role in the formation of twins is shown only by irregular segregation of Co and Nb to the twin boundaries and inside the cassiterite grains, and Co,Nb-enrichment in the cyclic twin cores., (open access.)

Freeze-drying is a process of choice to texture hydrogel scaffolds with pores formed by an ice-templating mechanism. Using state-of-the-art microscopies (cryo-EBSD, μCT, CLSM), this work evidences and quantifies the effect of crosslinking and ice nucleation temperature on the porous structure of thin hydrogel scaffolds freeze-dried at a low cooling rate. We focused on a polysaccharide-based hydrogel and developed specific protocols to monitor or trigger ice nucleation for this study. At a fixed number of intermolecular crosslinks per primary molecule (p = 5), the mean pore size in the dry state decreases linearly from 240 to 170 μm, when ice nucleation temperature decreases from -6 °C to -18 °C. When ice nucleation temperature is fixed at -10 °C, the mean pore size decreases from 250 to 150 μm, as the crosslinking degree increases from p = 3 to p = 7. Scaffold infiltration ability was quantified with synthetic microspheres. The seeding efficiency was assessed with MC3T3-E1 individual cells and HepaRG™ spheroids. These data collapse into a single master curve that exhibits a sharp transition from 100 % to 0 %-efficiency as the entity diameter approaches the mean pore size in the dry state. Altogether, we can thus precisely tune the porosity of these 3D materials of interest for 3D cell culture and cGMP production for tissue engineering., (Copyright © 2022 Elsevier B.V. All rights reserved.)

Electron backscatter diffraction (EBSD) was used for the analysis of multiple cyclic twins in cassiterite (SnO 2 ), which form during sintering of SnO 2 with small additions of CoO and Nb 2 O 5 . Grain misorientation analysis has shown that about one third of all grains contain {101} twin boundaries (TBs). The majority of these grains are contact twins, whereas a small fraction of grains are multiple, mainly cyclic twins. A procedure was developed in MTEX [Bachmann, Hielscher & Schaeben (2010). Solid State Phenom. 160, 63-88] for automated identification of crystallographically different types of cyclic twins and found two main types: coplanar twins composed of three or four domains with a common [010] axis and alternating twins composed of three to seven domains oriented along the [111] axis. Both types of cyclic twins have a characteristic common origin (nucleus) of all TBs, which is positioned eccentric relative to the grain section and the cycle is closed with a shorter non-crystallographic contact between the first and the last twin domain. The morphology of cyclic twins suggests that they form by nucleation in the initial stages of grain growth. The average size of twinned grains increases with the number of twin domains indicating the influence of TBs formation on the growth of composite grains., (open access.)

Whereas freeze-drying is a widely used method to produce porous hydrogel scaffolds, the mechanisms of pore formation involved in this process remained poorly characterized. To explore this, we focused on a cross-linked polysaccharide-based hydrogel developed for bone tissue engineering. Scaffolds were first swollen in 0.025% NaCl then freeze-dried at low cooling rate, i.e. -0.1 °C min -1 , and finally swollen in aqueous solvents of increasing ionic strength. We found that scaffold's porous structure is strongly conditioned by the nucleation of ice. Electron cryo-microscopy of frozen scaffolds demonstrates that each pore results from the growth of one to a few ice grains. Most crystals were formed by secondary nucleation since very few nucleating sites were initially present in each scaffold (0.1 nuclei cm -3  °C -1 ). The polymer chains are rejected in the intergranular space and form a macro-network. Its characteristic length scale coincides with the ice grain size (160 μm) and is several orders of magnitude greater than the mesh size (90 nm) of the cross-linked network. After sublimation, the ice grains are replaced by macro-pores of 280 μm mean size and the resulting dry structure is highly porous, i.e. 93%, as measured by high-resolution X-ray tomography. In the swollen state, the scaffold mean pore size decreases in aqueous solvent of increasing ionic strength (120 µm in 0.025% NaCl and 54 µm in DBPS) but the porosity remains the same, i.e. 29% regardless of the solvent. Finally, cell seeding of dried scaffolds demonstrates that the pores are adequately interconnected to allow homogenous cell distribution. STATEMENT OF SIGNIFICANCE: The fabrication of hydrogel scaffolds is an important research area in tissue engineering. Hydrogels are textured to provide a 3D-framework that is favorable for cell proliferation and/or differentiation. Optimum hydrogel pore size depends on its biological application. Producing porous hydrogels is commonly achieved through freeze-drying. However, the mechanisms of pore formation remain to be fully understood. We carefully analyzed scaffolds of a cross-linked polysaccharide-based hydrogel developed for bone tissue engineering, using state-of-the-art microscopic techniques. Our experimental results evidenced the shaping of hydrogel during the freezing step, through a specific ice-templating mechanism. These findings will guide the strategies for controlling the porous structure of hydrogel scaffolds., (Copyright © 2019 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.)

Nucleation mechanisms occurring during dynamic recrystallization play a crucial role in the evolution of microstructures and textures during high temperature deformation. In polycrystalline ice, the strong viscoplastic anisotropy induces high strain heterogeneities between grains which control the recrystallization mechanisms. Here, we study the nucleation mechanisms occurring during creep tests performed on polycrystalline columnar ice at high temperature and stress (T=-5°C;σ=0.5 MPa) by post-mortem analyses of deformation microstructures using cryogenic electron backscatter diffraction. The columnar geometry of the samples enables discrimination of the nuclei from the initial grains. Various nucleation mechanisms are deduced from the analysis of the nuclei relations with the dislocation sub-structures within grains and at grain boundaries. Tilt sub-grain boundaries and kink bands are the main structures responsible for development of polygonization and mosaic sub-structures. Nucleation by bulging at serrated grain boundaries is also an efficient nucleation mechanism near the grain boundaries where strain incompatibilities are high. Observation of nuclei with orientations not related to the 'parent' ones suggests the possibility of 'spontaneous' nucleation driven by the relaxation of the dislocation-related internal stress field. The complexity of the nucleation mechanisms observed here emphasizes the impact of stress and strain heterogeneities on dynamic recrystallization mechanisms.This article is part of the themed issue 'Microdynamics of ice'., (© 2016 The Author(s).)

Mantle flow involves large strains of polymineral aggregates. The strongly anisotropic plastic response of each individual grain in the aggregate results from the interactions between neighbouring grains and the continuity of material displacement across the grain boundaries. Orthorhombic olivine, which is the dominant mineral phase of the Earth's upper mantle, does not exhibit enough slip systems to accommodate a general deformation state by intracrystalline slip without inducing damage. Here we show that a more general description of the deformation process that includes the motion of rotational defects referred to as disclinations can solve the olivine deformation paradox. We use high-resolution electron backscattering diffraction (EBSD) maps of deformed olivine aggregates to resolve the disclinations. The disclinations are found to decorate grain boundaries in olivine samples deformed experimentally and in nature. We present a disclination-based model of a high-angle tilt boundary in olivine, which demonstrates that an applied shear induces grain-boundary migration through disclination motion. This new approach clarifies grain-boundary-mediated plasticity in polycrystalline aggregates. By providing the missing mechanism for describing plastic flow in olivine, this work will permit multiscale modelling of the rheology of the upper mantle, from the atomic scale to the scale of the flow.