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Accessory minerals like zircon, rutile and monazite are routinely studied to inform about the timing and nature of geological processes. These studies are underpinned by our understanding of the transfer processes of trace elements and the assumption that the isotopic systems remain undisturbed. However, the presence of microstructures or Pb-bearing phases in minerals can lead to the alteration of the Pb isotopic composition. To gain insight into the relationship between Pb isotopic alterations from inclusions and microstructures, this study focused on inclusions from an ultra-high-temperature metamorphic rutile. The studied inclusions are submicrometer monazites, a common mineral rich in Pb but normally not present in rutile. The sample is sourced from Mt. Hardy, Napier Complex, East Antarctica, an ultra-high-temperature (UHT) metamorphic terrane. By applying correlative analytical techniques, including electron backscatter diffraction mapping, transmission electron microscopy (TEM), and atom probe tomography, it is shown that monazite inclusions are often in contact with low-angle boundaries and yield no preferred orientation. TEM analysis shows the monazite core has a mottled texture due to the presence of radiation damage and nanoclusters associated with the radiation damage defects that are rich in U, Pb, and Ca. Some monazites exhibit a core-rim structure. The rim yields clusters composed of Ca- and Li-phosphate that enclose Pb nanoclusters that are only present in small amounts compared to the core, with Pb likely diffused into the rutile-monazite interface. These textures are the result of two stages of Pb mobility. Initial Pb segregation was driven by volume diffusion during UHT metamorphism (2500 Ma). The second stage is a stress-induced recrystallization during exhumation, leading to recrystallization of the monazite rim and trace element transport. The isotopic signature of Pb trapped within the rutile-monazite interface constrains the timing of Pb mobility to ca. 550 Ma. [ABSTRACT FROM AUTHOR]

The mineral zircon is used widely to constrain the age of rocks and the processes that formed them. Although zircon is robust to a range of physical and chemical processes, it may show evidence for rapid re-equilibration that is generally considered to reflect interaction with hydrous fluids. Here, we show that zircon grains that crystallized from melt produced during the catastrophic meltdown of the Chernobyl nuclear reactor exhibit re-equilibration textures that occurred in an environment without free water. The process of re-equilibration involved a melt-mediated interface-coupled dissolutionreprecipitation that took place over a few days to produce textures that are commonly observed in igneous and anatectic systems. Thus, the composition of zircon can be modified even in the absence of hydrous fluids in a short time frame. Through this process, zircon crystals may track the timing of the last silicate melt they interacted with. [ABSTRACT FROM AUTHOR]

Xenotime (YPO4) is an accessory phase common in low to high‐temperature geological environments. Xenotime is an established geochronometer, though its small size, low modal abundance and textural complexity make it more difficult to analyse with traditional techniques but makes a prime candidate for nanoscale analysis. In this study, we develop an atom probe tomography (APT) protocol to determine the 206Pb/238U and 207Pb/206Pb ages of micro‐scale xenotime crystals with analytical volumes four to six orders of magnitude smaller than typical geochronology techniques. A linear correlation between the 206Pb/238U fractionation and 238UO22+/238UO2+ was used to correct for the atom probe instrument parameters variability between specimens. For 207Pb/206Pb ages, we employed two methods of background correction owing to the 206Pb2+ thermal tail contribution to the 207Pb2+ counts: A constant background correction for the younger (˜ 1000 Ma) Y1 reference material and a variable correction of background for Archaean age reference material xtc to correct for the thermal tail influence. This contribution also proposes strategies for optimisation of xenotime analysis using APT and permits us to explore the various geological problems in the nanoscale realm. This methodology potentially allows determining the age of small xenotime crystals in sedimentary rocks, low metamorphic grade settings and deformation microstructures. [ABSTRACT FROM AUTHOR]

Monazite U‐Th‐Pb geochronology is widely used for dating geological processes, but current analytical techniques are limited to grains greater than 5 μm in diameter. This limitation precludes the analysis of both micrometre‐scale discrete monazite grains and fine textures within monazite crystals that are commonly found in geological specimens. Here, we analyse reference materials by atom probe tomography and develop a protocol for 208Pb/232Th dating of nanoscale domains of monazite (0.0007 μm3 analytical volume). The results indicate that the 208Pb2+/232ThO2+ ratios are higher than the true values. Such fractionation can be corrected using a linear regression between 208Pb2+/232ThO2+ and the M/ΔM10 peak shape parameter, where M is the position of the O2+ peak and ΔM10 the full‐width‐at‐tenth‐maximum for the same peak. This correction results in 15–20% analytical uncertainty on the corrected 208Pb/232Th age. Nonetheless, this approach opens the possibility of obtaining 208Pb/232Th ages with sufficient precision to address geological questions on an unprecedented small scale. To illustrate the approach, atom probe geochronology of a small monazite grain from the contact aureole of the Fanad pluton (Ireland) yielded a 208Pb/232Th atom probe age of 420 ± 60 Ma (2s) and is consistent with the known metamorphism in the region. [ABSTRACT FROM AUTHOR]

Atom probe tomography (APT) is an analytical technique that provides quantitative three‐dimensional elemental and isotopic analyses at sub‐nanometre resolution across the whole periodic table. Although developed and mostly used in the materials science and semiconductor fields, recent years have seen increasing development and application in the geoscience and planetary science disciplines. Atom probe studies demonstrate compositional complexity at the nanoscale and provide fundamental new insights into the atom‐scale mechanisms taking place in minerals over geological time. Here, we provide an overview of APT, including the historical development and technical aspects of the instrumentation, and the fundamentals of data acquisition, data processing and data reconstruction. We also review previous studies and highlight the potential future applications of nanoscale geochemical studies of natural materials. [ABSTRACT FROM AUTHOR]

The Western Gneiss Region, western Norway, consists of Paleoproterozoic crust of Baltica ancestry (Baltican Basement), partly subducted to high- and ultrahigh-pressure (HP-UHP) conditions during the Scandian Orogeny between 415 and 395 Ma. The dominant felsic gneisses carry little evidence for the HP-UHP history but were affected by amphibolite-facies reworking during exhumation. Laser ablation-ICP-MS and secondary ion mass spectrometry (SIMS) zircon U-Pb data collected in augen gneiss samples constrain the magmatic and metamorphic geochronology in this crust. Five samples from the eclogite-bearing HP-UHP basement near Molde yield intrusion ages ranging from 1644±6 to 1594±10 Ma. Two samples of the structurally underlying eclogite-free basement yield ages of 1685± 18 and 1644±13 Ma, and a sample from the infolded Middle Allochthon Risberget Nappe yields an equivalent age of 1676±18 Ma. Two samples of the eclogite-bearing basement contain low Th/U neocrystallized zircon with an age of 950±26 Ma. This zircon provides the northernmost direct evidence for at least amphibolite-facies Sveconorwegian metamorphism in unquestionable Baltica crust, close to the known "Sveconorwegian boundary" in the Western Gneiss Region. The Western Gneiss Region (1686-1594 Ma magmatism), the Eastern Segment of the Sveconorwegian Orogen (1795-1640 Ma magmatism), and the Idefjorden terrane hosting the type Gothian active margin magmatism (1659-1520 Ma) probably represent three distinct Proterozoic growth zones of Baltica into which Sveconorwegian reworking propagated. Samples of the eclogite-bearing basement lack Scandian neocrystallized zircon but do show partial recrystallization of zircon. Paired cathodoluminescence and electron backscatter diffraction images indicate that zircon crystals underwent crystal-plastic deformation during the Scandian subduction-exhumation cycle. They illustrate a relationship between crystal-plastic deformation by dislocation creep, fading of oscillatory growth zoning, and loss of radiogenic lead. [ABSTRACT FROM AUTHOR]

Abstract: Geochemical and geochronological studies of zircon are commonly supplemented by cathodoluminescence (CL) imaging because it provides a means of recognizing different generations of zircon growth at high-spatial resolution. Crystal-plastic deformation of zircon can have significant effects on zircon geochemistry. Detailed analyses from electron backscatter diffraction mapping combined with panchromatic CL imaging and hyperspectral CL mapping of several crystal-plastically deformed grains from different geological settings are used to establish the relationships between crystal-plastic deformation and CL in zircon. Results show a strong spatial association between deformation microstructures and CL response that lead to modification of CL that commonly cross-cuts primary zoning. Variable contributions from two fundamental deformation-related processes result in a variety of CL characteristics: A defect control on panchromatic CL intensity, particularly at low-angle (subgrain) boundaries; and changes in spectral CL response due to deformation-related modification of CL-active REE geochemistry. A framework is provided for the recognition of deformation-related microstructures using CL and the usefulness of CL imaging in the discrimination of these microstructures is critically evaluated. [Copyright &y& Elsevier]

In-situ rock suites that preserve assemblages consistent with metamorphism to eclogite-facies conditions are absent from the Archaean. Their Palaeoproterozoic appearance is one of the markers of the onset of tectonic processes similar to those seen in the Phanerozoic Earth. We report new U–Pb Secondary Ion Mass Spectrometry (SIMS) zircon data from the oldest known eclogites (the ∼2.0 Ga Usagaran eclogites, Tanzania) that constrain the timing of high-grade metamorphism, deformation and exhumation of these eclogites and constrain the speed of these processes at this critical period in Earth history.Direct dating of metamorphic zircon from mafic eclogites, and isostructurally recrystallised zircon rims from pelites and felsic gneisses indicates that high-grade metamorphism occurred at 1999.1±1.1 Ma. The rocks were quickly cooled and exhumed at rates of ∼25 °C/Ma and 0.06–0.22 GPa/Ma, respectively, at least in part, by amphibolite-facies sinistral transpression constrained by a 1991±2 Ma pegmatite dyke that crosscuts foliation. Detrital zircons in metasedimentary gneiss protoliths were dominantly derived from two sources: (1) the Tanzanian craton, and (2) a 2400–2640 Ma source region that is compatible with a belt of reworked Archaean and Palaeoproterozoic rocks that lie in the East African Orogen. [Copyright &y& Elsevier]

Extensional episodes in Precambrian orogens are often difficult to decipher because of subsequent orogenesis and intracontinental reworking. Here, we use geochemical and geochronological constraints of a suite of preserved mafic–ultramafic rocks in the Paleoproterozoic Capricorn Orogen of Western Australia to reveal ophiolites, continental ribbons and aborted rifts. The Capricorn Orogen separates the Archean Yilgarn and Pilbara cratons and includes mafic–ultramafic rocks of the fault-bounded Trillbar Complex and Bryah Sub-basin. The Trillbar Complex is situated within a fault wedge between the Yilgarn Craton and a reworked portion of the craton to the north (Yarlarweelor Gneiss Complex), and has been variously interpreted as an obducted ophiolite, oceanic plateau or continental rift-related magmatic suite. In this study, a new U–Pb zircon age of 2069 ± 9 Ma from the Trillbar Complex indicates that it is at least 40 Myr older than the mafic and ultramafic rocks of the Bryah Sub-basin, with which it has previously been linked. The Trillbar Complex is characterised by E-MORB-like signatures, hydrous crystallization and a lack of crustal contamination, and probably formed in a mid-ocean ridge or, alternatively, an oceanic intraplate setting. Conversely, the 2030–1990 Ma mafic and ultramafic rocks in the Bryah Sub-basin show evidence of crustal contamination and are interpreted to have formed in a continental rift setting. Moreover, there is no evidence for boninites in the Bryah Sub-basin and, therefore, no justification for invoking a fore-arc setting. Thus, these pieces of evidence reveal a different tectonic and geodynamic origin for the Trillbar Complex compared to the Bryah Sub-basin rocks. The tectonic setting for the Trillbar Complex requires oceanic crust to have existed between the Yilgarn Craton and the Yarlarweelor Gneiss Complex. However, almost identical Archean histories of these crustal blocks support a proximal origin for the Yarlarweelor Gneiss Complex and a likely origin as a microcontinental ribbon. Farther east (in present-day coordinates), the Bryah Sub-basin and other sedimentary basins record punctuated rifting that never led to the formation of oceanic crust. Therefore, rigorous evaluation of high quality geochemical data coupled to geochronology from mafic–ultramafic rocks is able to provide valuable constraints on extensional episodes, where other evidence has since been erased from the rock record. [ABSTRACT FROM AUTHOR]