41 research outputs found

    Atom probe microscopy of zinc isotopic enrichment in ZnO nanorods

    Get PDF
    We report on atomic probe microscopy (APM) of isotopically enriched ZnO nanorods that measures the spatial distribution of zinc isotopes in sections of ZnO nanorods for natural abundance natZnO and 64Zn and 66Zn enriched ZnO nanorods. The results demonstrate that APM can accurately quantify isotopic abundances within these nanoscale structures. Therefore the atom probe microscope is a useful tool for characterizing Zn isotopic heterostructures in ZnO. Isotopic heterostructures have been proposed for controlling thermal conductivity and also, combined with neutron transmutation doping, they could be key to a novel technology for producing p-n junctions in ZnO thin films and nanorods

    From ID-TIMS U-Pb dating of single monazite grain to APT-nanogeochronology: application to the UHT granulites of Andriamena (North-Central Madagascar)

    Get PDF
    The causes of U-Pb isotopic discordance documented by Paquette et al. (2004) in monazite grains from the ultra-high temperature (UHT) granulite of the Andriamena unit of Madagascar are re-evaluated in the light of nanoscale crystal-chemical characterization utilising Atom Probe Tomography (APT) and state-of-the-art Scanning Transmission Electron Microscopy (STEM). APT provides isotopic (208Pb/232Th) dating and information on the chemical segregation of trace elements (e.g., Pb) in monazite at nanoscale. Latest generation of STEM allows complementary high-resolution chemical and structural characterization at nanoscale. In situ isotopic U–Pb dating with Secondary Ion Mass Spectrometry (SIMS) on 25 monazite grains and Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) on zircon have been employed to refine the age spectra. Monazite and zircon grains located in quartz and garnet formed with the peak UHT metamorphic assemblage, which is partially overprinted by retrograde coronitic textures. Zircon grains hosted in garnet and in quartz yield concordant U–Pb ages at 2758 ± 28 Ma and 2609 ± 51 Ma, respectively whereas monazite grains hosted in quartz and garnet show a discordant Pb* loss trend on the Concordia diagram recording disturbance at 1053 ± 246 Ma that is not seen by the zircon, underlining the importance of combining the use of monazite and zircon to understand the history of polymetamorphic rocks. The Pb*-loss trend of monazite is related to petrographic position, with less Pb* lost from monazite hosted in quartz and garnet than monazite hosted in the coronitic reaction texture domains. STEM shows that the garnet- and quartz-hosted monazite grains contain more Pb-bearing nanophases than monazite grains located in the coronitic textures. An inverse correlation between the number of Pb-bearing nanophases and the percentage of Pb*-loss in monazite grains demonstrates that Pb* is retained in the grain in the form of nanophases. The formation of Pb-bearing nanophases limits Pb*-loss at the grain scale and therefore allows the preservation of early events. 208Pb/232Th ratios obtained with APT in monazite located in quartz and garnet and excluding Pb*-bearing nanophases indicate a mean age of 1059 ± 129 Ma corresponding to a disturbance event hitherto undetected in the geochronological record of the Andriamena unit. Thus, geochronology with APT allows access to information and the definition of events that may be blurred or obscured when examined at lower spatial resolution

    Atom scale element and isotopic investigation of 25Mg-rich stardust from a H-burning supernova

    Get PDF
    We have discovered a presolar olivine from ALH 77307 with the highest 25Mg isotopic composition measured in a silicate to date (ÎŽ25Mg = 3025.1‰ ± 38.3‰). Its isotopic compositions challenge current stellar models, with modeling of magnesium, silicon, and oxygen showing a closest match to formation in a supernova (SN) where hydrogen ingestion occurred in the pre-SN phase. Presolar grains within primitive astromaterials retain records of processes and environmental changes throughout stellar evolution. However, accessing these records has proved challenging due to the average grain size (∌150 nm) of presolar silicates, their sensitivity to extraction agents, and instrumental restrictions, limiting the range of isotopic and chemical signatures which can be studied per grain volume. Here, we present the first known detailed geochemical study of a presolar silicate from a hydrogen-burning SN, studied in 3D without contributions to the analysis volume and at unprecedented spatial resolutions (<1 nm), essential for constraining physical and chemical processes occurring within this recently proposed stellar environment. From our results, we infer either (i) condensation within an environment depleted of heavy elements compatible with the olivine lattice under the pressure and temperature conditions during condensation, or (ii) during periods of limited mixing either near the end of the pre-SN phase or from a collapse so rapid localized pockets of different gas compositions formed

    Assessing the mechanisms of common Pb incorporation into titanite

    Get PDF
    Common Pb, the portion of non-radiogenic Pb within a U bearing mineral, needs to be accurately accounted for in order to subtract its effect on U-Pb isotopic ratios so that meaningful ages can be calculated. The propensity to accommodate common Pb during crystallization, or later, is different across the range of U bearing minerals used for geochronology. Titanite frequently accommodates significant amounts of common Pb. However, the most appropriate method to correct for this requires knowledge on the mechanism and timing of common Pb incorporation; information that is commonly difficult to extract. In this study, the spatial and compositional distribution of trace elements (including Pb) in metamorphic titanites from a Greenland amphibolite is investigated on the grain- to nano-scale. Titanites have an isotopically similar signature for both common and radiogenic-Pb in all grains but significantly different quantities of the non-radiogenic component. Microstructural and compositional examination of these grains reveals undeformed, but high common Pb (F207%) titanites have homogeneous element distributions on the atomic scale suggesting common Pb is incorporated into titanite during its growth and not during later processes. In contrast, deformed titanite comprising low-angle boundaries, formed by subgrain rotation recrystallization, comprise networks of dislocations that are enriched in Mg, Al, K and Fe. Smaller cations may migrate due to elastic strain in the vicinity of the dislocation network, yet the larger K cations more likely reflect the mobility of externally-derived K along the orien tation interface. The absence of Pb enrichment along the boundary indicates that either Pb was too large to fit into migrating lattice dislocations or static low-angle boundaries and/or that there was no external Pb available to diffuse along the grain boundary. As the common Pb composition is distinctly different to regional Pb models, the metamorphic titanite grew in a homogeneous Pb reservoir dominated by the break-down of precursor U-bearing phases. The different quantity of common Pb in the titanite grains indicates a mineral-driven element partitioning in an isotopically homogeneous metamorphic reservoir, consistent with low U, low total REE and flat LREE signatures in high F207% analyses. These results have implications for the selection of appropriate common Pb corrections in titanite and other accessory phases

    Developing atom probe tomography of phyllosilicates in preparation for extra-terrestrial sample return

    Get PDF
    Hydrous phyllosilicate minerals, including the serpentine subgroup, are likely to be major constituents of material that will be bought back to Earth by missions to Mars and to primitive asteroids Ryugu and Bennu. Small quantities (< 60 g) of micrometre sized, internally heterogeneous material will be available for study, requiring minimally destructive techniques. Many conventional methods are unsuitable for phyllosilicates as they are typically finely crystalline and electron beam sensitive resulting in amorphisation and dehydration. New tools will be required for nanoscale characterisation of these precious extra‐terrestrial samples. Here we test the effectiveness of atom probe tomography (APT) for this purpose. Using lizardite from the Ronda peridotite, Spain, as a terrestrial analogue, we outline an effective analytical protocol to extract nanoscale chemical and structural measurements of phyllosilicates. The potential of APT is demonstrated by the unexpected finding that the Ronda lizardite contains SiO‐rich nanophases, consistent with opaline silica that formed as a by‐product of the serpentinisation of olivine. Our new APT approach unlocks previously unobservable nanominerals and nanostructures within phyllosilicates owing to resolution limitations of more established imaging techniques. APT will provide unique insights into the processes and products of water/rock interaction on Earth, Mars and primitive asteroids
    corecore