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Ancient metamorphic processes are recorded by the formation of metallic-Pb nanospheres in zircon, a product of internal Pb mobilisation and thermally driven concentration. Here, metallic-Pb nanospheres formed within an ore deposit are characterised for the first time using high-angle annular dark field scanning transmission electron microscopy and energy-dispersive X-ray spectroscopy element-distribution mapping. Exceptional examples from the migmatite-hosted Archean–Paleoproterozoic Challenger Au deposit (Central Gawler Craton, South Australia) support widespread metallic-Pb nanosphere formation in zircon from rocks experiencing granulite-facies metamorphism. We also report new trace-element associations found with metallic-Pb nanospheres and a new mode of occurrence, in which Sc ‘haloes’ form adjacent to metallic-Pb nanospheres within the crystalline zircon lattice. This differs to previously characterised examples of metallic-Pb nanospheres associated with amorphous Si-rich glasses and unidentified Al–Ti, or Fe-bearing phases. Multiple modes of metallic-Pb nanosphere occurrences and trace-element associations suggests multiple modes of formation, probably dependant on zircon composition and metamorphic conditions. Identification of metallic-Pb nanospheres in a growing range of geological settings further highlights the mobility of Pb in zircon and the importance of detailed, nanoscale mineral characterisation, in order to constrain accurate geochronological histories for rocks within high-temperature geological environments.
Preferential removal of W relative to other trace elements from zoned, W–Sn–U–Pb-bearing hematite coupled with disturbance of U–Pb isotope systematics is attributed to pseudomorphic replacement via coupled dissolution reprecipitation reaction (CDRR). This hematite has been studied down to the nanoscale to understand the mechanisms leading to compositional and U/Pb isotope heterogeneity at the grain scale. High-Angle Annular Dark Field Scanning Transmission Electron Microscopy (HAADF STEM) imaging of foils extracted in situ from three locations across the W-rich to W-depleted domains show lattice-scale defects and crystal structure modifications adjacent to twin planes. Secondary sets of twins and associated splays are common, but wider (up to ~100 nm) inclusion trails occur only at the boundary between the W-rich and W-depleted domains. STEM energy-dispersive X-ray mapping reveals W- and Pb-enrichment along 2–3 nm-wide features defining the twin planes; W-bearing nanoparticles occur along the splays. Tungsten and Pb are both present, albeit at low concentrations, within Na–K–Cl-bearing inclusions along the trails. HAADF STEM imaging of hematite reveals modifications relative to ideal crystal structure. A two-fold hematite superstructure (a = b = c = 10.85 Å; α = β = γ = 55.28°) involving oxygen vacancies was constructed and assessed by STEM simulations with a good match to data. This model can account for significant W release during interaction with fluids percolating through twin planes and secondary structures as CDRR progresses from the zoned domain, otherwise apparently undisturbed at the micrometre scale. Lead remobilisation is confirmed here at the nanoscale and is responsible for a disturbance of U/Pb ratios in hematite affected by CDRR. Twin planes can provide pathways for fluid percolation and metal entrapment during post-crystallisation overprinting. The presence of complex twinning can therefore predict potential disturbances of isotope systems in hematite that will affect its performance as a robust geochronometer.
Nanoscale characterization (TEM on FIB-SEM-prepared foils) was undertaken on feldspars undergoing transformation from early post-magmatic (deuteric) to hydrothermal stages in granites hosting the Olympic Dam Cu-U-Au-Ag deposit, and from the Cu-Au skarn at Hillside within the same iron-oxide copper-gold (IOCG) province, South Australia. These include complex perthitic textures, anomalously Ba-, Fe-, or REE-rich compositions, and REE-flourocarbonate + molybdenite assemblages which pseudomorph pre-existing feldspars. Epitaxial orientations between cryptoperthite (magmatic), patch perthite (dueteric) and replacive albite (hydrothermal) within vein perthite support interface-mediated reactions between pre-existing alkali-feldspars and pervading fluid, irrespective of micro-scale crystal morphology. Such observations are consistent with a coupled dissolution-reprecipitation reaction mechanism, which assists in grain-scale element remobilization via the generation of transient interconnected microporosity. Micro-scale aggregates of hydrothermal hyalophane (Ba-rich K-feldspar), crystallizing within previously albitized areas of andesine, reveal a complex assemblage of calc-silicate, As-bearing fluorapatite and Fe oxides along reaction boundaries in the enclosing albite-sericite assemblage typical of deuteric alteration. Such inclusions are good REE repositories and their presence supports REE remobilization at the grain-scale during early hydrothermal alteration. Iron-metasomatism is recognized by nanoscale maghemite inclusions within ‘red-stained’ orthoclase, as well as by hematite in REE-fluorocarbonates, which reflect broader-scale zonation patterns typical for IOCG systems. Potassium-feldspar from the contact between alkali-granite and skarn at Hillside is characterized by 100–1000 ppm REE, attributable to pervasive nanoscale inclusions of calc-silicates, concentrated along microfractures, or pore-attached. Feldspar replacement by REE-fluorcarbonates at Olympic Dam and nanoscale calc-silicate inclusions in feldspar at Hillside are both strong evidence for the role of feldspars in concentrating REE during intense metasomatism. Differences in mineralogical expression are due to the availability of associated elements. Lattice-scale intergrowths of assemblages indicative of Fe-metasomatism, REE-enrichment and sulfide deposition at Olympic Dam are evidence for a spatial and temporal relationship between these processes.
The Olympic Dam iron-oxide copper-gold-silver-uranium deposit, South Australia, contains three dominant U minerals: uraninite; coffinite; and brannerite. Microanalytical and petrographic observations provide evidence for an interpretation in which brannerite and coffinite essentially represent the products of U mineralizing events after initial deposit formation at 1.6 Ga. Marked compositional and textural differences between the various types of brannerite and coffinite highlight the role of multiple stages of U dissolution and reprecipitation.
On the basis of petrography (size, habit, textures and mineral associations) and compositional variation, brannerites are divided into four distinct groups (brannerite-A, -B, -C and -D), and coffinite into three groups (coffinite-A, -B and -C). Brannerite-A ranges in composition from what is effectively uraniferous rutile to stoichiometric brannerite, and has elevated (Mg +Mn + Na + K) and (Fe + Al) compared to other brannerite types. It displays the most diverse range of morphologies, including complex irregular-shaped aggregates, replacement bands, and discrete elongate seams. The internal structure of brannerite-A consists of randomly-oriented hair-like needles and blades. Brannerite-B (>5 μm in size) is generally prismatic and typically associated with baryte and REY minerals (REE+Y= REY). Brannerite-C and -D are both associated with Cu-(Fe)-sulfides and are typically composed of irregular masses and blebs (10–50 μm in size) with a more uniform or massive internal structure. Brannerite-D is distinct from -C and always contains inclusions of galena. Brannerite-B to -D all contain elevated ΣREY, with brannerite-B and -C having elevated As, and brannerite-D having elevated Nb.
All coffinite is typically globular (each globule is 2–10 μm in size) to collomorphic in appearance. Coffinite-A ranges from discrete globules to collomorphic bands completely encompassing quartz. Coffinite-B is always found with uraninite, and includes collomorph coffinite enveloped by massive uraninite, as well as aureoles of coffinite on the margins of uraninite crystals. Coffinite-C is associated with brannerite and REY minerals. The majority of coffinite is heterogeneous.
Brannerite and coffinite have probably precipitated as part of a late-stage hydrothermal U-event, which might have involved the dissolution and/or reprecipitation of earlier precipitated uraninite, or could represent the products of a later U mineralizing event. Evidence which supports formation of late-stage coffinite and brannerite includes: (1) low-Pb contents of both minerals; (2) coffinite is commonly found on the edges of uraninite, implying later deposition; and (3) coffinite is often found on the edge of brannerite aggregates, suggestive of brannerite precipitation occurred before coffinite. Moreover, there are many features (e.g. banding, scalloped edges, alteration rinds, variable compositions etc.) indicative of hydrothermal alteration processes.
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