Correlating planar microstructures in shocked zircon from the Vredefort Dome at multiple scales: Crystallographic modeling, external and internal imaging, and EBSD structural analysis
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Microstructural and geochronological analysis of shocked zircon has greatly advanced understanding the formation and evolution of impact structures. However, fundamental aspects of shock-produced planar microstructures in zircon remain poorly known, such as their deformation mechanisms, crystallographic orientations, and how planar microstructures visible at the grain scale by scanning electron microscopy correlate to microstructures visible at sub-micrometer scales by transmission electron microscopy and electron backscatter diffraction (EBSD). To unify observations of planar microstructures in zircon made at different scales into a consistent framework, we integrate the results of: (1) three-dimensional crystallographic modeling of planar microstructure orientations, with (2) 360° external prism backscattered electron imaging at the grain scale, and (3) polished section cathodoluminescence and EBSD analysis at the sub-micrometer scale for a suite of detrital shocked zircons eroded from the Vredefort Dome in South Africa. Our combined approach resulted in the documentation of seven planar microstructure orientations that can be correlated from grain to sub-micrometer scales of observation: (010), (100), (112), (11̄2), (1̄12), (1̄1̄2), and (011). All orientations of planar microstructures exhibit minor variations in style, however all are considered to be fractures; no amorphous ZrSiO4 lamellae were identified. We therefore favor the usage of "planar fracture" (PF) over "planar deformation feature" (PDF) for describing the observed planar microstructures in zircon based broadly on the nomenclature developed for shocked quartz. Some {112} PFs visible at the grain scale contain impact microtwins detectable by EBSD, and are the first report of polysynthetic twinning in zircon. The microtwins consist of parallel sets of thin lamellae of zircon oriented 65° about <110> and occur in multiple crosscutting {112} orientations within single grains. Curviplanar fractures and injected melt are additional impact-related microstructures associated with PF formation. Crosscutting relations of shock microstructures reveal the following chronology: (1) Early development of c-axis parallel PFs in (010) and (100) orientations; (2) the development of up to four {112} PFs, including some with microtwins; (3) the development of curviplanar fractures and the injection of impact derived melt; (4) the development of (011) PFs associated with compressional deformation; and (5) grain-scale non-discrete crystal plastic deformation. Experimental constraints for the onset of PFs, together with the absence of reidite, suggest formation conditions from 20 to 40 GPa for all of the planar microstructures described here.Keywords:
Cathodoluminescence
Complex microstructures of zircon recrystallisation have been discovered in igneous and metamorphic zircons from the Jack Hills Metasedimentary Belt in Western Australia, and the granitic injection complex of Harris in north-west Scotland. Cathodoluminescence (CL), electron backscatter diffraction (EBSD) and wavelength dispersive spectroscopy (WDS) analysis reveal that recrystallisation in the studied zircons is often characterised by (1) translation, bending and fading of the oscillatory zoning; (2) structural recovery of the zircon; (3) an enrichment in Hf and depletion in Y in recrystallised zircon; and (4) the formation of a recrystallisation interface with a minor (<2°) misorientation. A new, composite recrystallisation model in which trace element and dislocation migration occurs shortly after crystallisation during magmatic cooling and pipe diffusion along dislocation arrays formed by the accumulation of dislocations allows enhanced diffusion to enrich Hf and leach U, Pb and Y. After the recrystallisation event, subsequent metamictization of primary zircon (typically with oscillatory zoning) creates zones that can structurally recover through a diffusion-reaction re-equilibration mechanism, resulting in further trace-element mobility. These mechanisms can create complex microstructures in zircons, suggesting that a detailed understanding of the crystallisation and recrystallisation history of a zircon may be required to accurately interpret its U-Pb ages.
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ABSTRACT Finite deformation patterns of accessory phases can indicate the tectonic regime and deformation history of the host rocks and geological units. In this study, tectonically deformed, seismically deformed, and shocked zircon grains from a granite sample from the core of the Vredefort impact structure were analyzed in situ, using a combination of Raman spectroscopy, backscatter electron (BSE) imaging, electron backscattered diffraction (EBSD) mapping, electron probe microanalyses (EPMA), energy-dispersive X-ray spectroscopy (EDS) qualitative chemical mapping, and cathodoluminescence (CL) imaging. We aimed to reveal the effects of marginal grain-size reduction, planar deformation bands (PDBs), and shock microtwins on the crystal structure and microchemistry of zircon. Deformation patterns such as PDBs, microtwins, and subgrains did not show any significant effect on zircon crystallinity/metamictization degree or on the CL signature. However, the ratio of Raman band intensities B1g (1008 cm–1) to Eg (356 cm–1) slightly decreased within domains with low misorientation. The ratio values were affected in shocked grains, particularly in twinned domains with high misorientation. B1g/Eg ratio mapping combined with metamictization degree mapping (full width at half maximum of B1g peak) suggest the presence of shock deformation features in zircon; however, due to the lower spatial resolution of the method, they must be used in combination with the EBSD technique. Additionally, we discovered anatase, quartz, goethite, calcite, and hematite micro-inclusions in the studied zircon grains, with quartz and anatase specifically being associated with strongly deformed domains of shocked zircon crystals.
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Misorientation
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Pseudotachylytes resulted from frictional melts associated with ultramylonites in high-grade metapelitic rocks from the Ivrea-Verbano zone in the Southern Alps (Northern Italy) were studied with focus on the deformation microstructures in zircon. The aims were to investigate the characteristics of zircon deformation in seismic zones, and to recognize specific microstructures generated in zircon during earthquakes, which could be useful for mineral dating of paleo-seismic events; helps to understand how seismic energy is released at depth and interacts with metamorphic processes. The interior of polished zircon grains ranging from 30 to 150 μm in length were investigated with optical microscope and scanning electron microscope (SEM) techniques, including secondary electron (SE), backscattered electron (BSE), forward scattered electron (FSE), cathodoluminescence (CL) imaging, and crystallographic orientation mapping by electron backscatter diffraction analysis (EBSD). Grains were studied in situ and as separated fractions embedded in epoxy disks. Among different cataclastic and crystal-plastic deformation microstructures in zircon we identified characteristic planar deformation bands (PDBs), planar fractures (PFs), and curviplanar fractures (CFs). Planar deformation bands in zircon are crystallographically controlled planar lattice volumes with misorientation from the host grain, which varies from 0.4° to 2.7°. PDBs are usually parallel to {100} crystallographic planes, have width from 0.3 to 1 μm and average spacing of 5 μm in 2D sections. Planar deformation bands appear as contrast lamellae in orientation contrast images and in EBSD maps, and in rare cases can be observed with the optical microscope. PDBs form in specifically oriented grains due to high differential stresses, high temperatures, and high strain rates generated in seismically active environment and/or due to shearing in the vicinity of frictional melts. Discovered structures represent a result of crystal-plastic deformation of zircon grains with operating dislocations having {010} glide system and misorientation axis, therefore, they can be classified as a new type 4 lattice distortion pattern, according to the existing classification for zircon (Piazolo et al. 2012; Kovaleva et al. 2014). We have demonstrated that formation of planar fractures in zircon takes place not only during impacts, but also in seismically active zones. We observe at least two cases of formation of PFs with {100} orientation: (1) as a result of evolution of PDBs and (2) as micro-cleavage. This study demonstrates that planar microstructures in terrestrial zircon do not exclusively form during impact events, but also as a result of seismic events at depth due to unusually high differential stress, strain rate, and temperature. According to the new findings, PDBs in zircon from the deep-crust are supposed to represent newly recognized evidence of seismicity.
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The effects of crystal-plasticity on the U-Th-Pb system in zircon is studied by quantitative microstructural and microchemical analysis of a large zircon grain collected from pyroxenite of the Lewisian Complex, Scotland. Electron backscatter diffraction (EBSD) mapping reveals a c.18 degree variation in crystallographic orientation that comprises both a gradual change in orientation and a series of discrete low-angle (<4 degrees) boundaries. These microstructural data are consistent with crystal-plastic deformation of zircon associated with the formation and migration of dislocations. A heterogeneous pattern of dark cathodoluminescence, with the darkest domains coinciding with low-angle boundaries, mimics the deformation microstructure identified by EBSD. Geochemical data collected using the Sensitive High Resolution Ion MicroProbe (SHRIMP) shows a positive correlation between concentrations of the elements U, Th and Pb (ranging from 20-60 ppm, 30-110 ppm, and 14-36 ppm, respectively) and Th/U ratio (1.13-1.8) with the deformation microstructure. The highest measured concentrations and Th/U coincide with low-angle boundaries. This enrichment is interpreted to reflect enhanced bulk diffusion of U and Th due to the formation and migration of high-diffusivity dislocations. 207Pb/206Pb ages for individual analyses show no significant variation across the grain, and define a concordant, combined mean age of 2451 +/- 14 Ma. This indicates that the grain was deformed shortly after initial crystallization, most probably during retrograde Inverian metamorphism at amphibolite facies conditions. The elevated Th over U and consistent 207Pb/206Pb ages indicates that deformation most likely occurred in the presence of a late-stage magmatic fluid that drove an increase in the Th/U during deformation. The relative enrichment of Th over U implies that Th/U ratio may not always be a robust indicator of crystallization environment. This study provides the first evidence of deformation-related modification of the U-Th system in zircon and has fundamental implications for the application and interpretation of zircon trace element data.
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Fission track dating
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He<sup>+</sup> ion implantation at 4.0 MeV, equivalent to energy of α particles from natural radioactive nuclei <sup>238</sup>U and <sup>232</sup>Th, has been conducted for undoped synthetic zircon. The cathodoluminescence (CL) of implanted samples was measured to clarify the radiation-induced effects. Unimplanted synthetic zircon shows pronounced and multiple blue emission bands between 310 nm and 380 nm, whereas the implanted samples have an intense yellow band at ~550 nm. The blue emission bands can be assigned to intrinsic defect centers formed during crystal growth. The yellow band should be derived from induced-defect centers by He<sup>+</sup> ion implantation, which might be related to the metamicitization originated from a self-induced radiation in natural zircon. The yellow band may be separated into two emission components at 1.96 eV and 2.16 eV. The emission component at 2.16 eV is recognized in both unimplanted and implanted samples, and its intensity increases with an increase in the implantation dose. The CL of zircon can be used as the geodosimeter.
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