Atom probe tomography characterisation of a laser diode structure grown by molecular beam epitaxy

Atom probe tomography (APT) has been used to achieve three-dimensional characterization of a III-nitride laser diode (LD) structure grown by molecular beam epitaxy (MBE). Four APT data sets have been obtained, with fields of view up to 400 nm in depth and 120 nm in diameter. These data sets contain material from the InGaN quantum well (QW) active region, as well as the surrounding p- and n-doped waveguide and cladding layers, enabling comprehensive study of the structure and composition of the LD structure. Two regions of the same sample, with different average indium contents (18% and 16%) in the QW region, were studied. The APT data are shown to provide easy access to the p-type dopant levels, and the composition of a thin AlGaN barrier layer. Next, the distribution of indium within the InGaN QW was analyzed, to assess any possible inhomogeneity of the distribution of indium (“indium clustering”). No evidence for a statistically significant deviation from a random distribution was found, indicating that these MBE-grown InGaN QWs do not require indium clusters for carrier localization. However, the APT data show steps in the QW interfaces, leading to well-width fluctuations, which may act to localize carriers. Additionally, the unexpected presence of a small amount (x = 0.005) of indium in a layer grown intentionally as GaN was revealed. Finally, the same statistical method applied to the QW was used to show that the indium distribution within a thick InGaN waveguide layer in the n-doped region did not show any deviation from randomness

Atomic worlds: Current state and future of atom probe tomography in geoscience

Atom Probe Tomography (APT) is rapidly finding new applications within the geosciences. Historically connected with materials science and semiconductor device applications, recent years have seen APT established as a useful tool for nanoscale geochemistry, offering unique capabilities when compared with conventional geoanalytical techniques. The ability to characterize 3D nanoscale chemistry with isotopic sensitivity has uncovered intricate details of complex trace element distributions within a variety of minerals. Already these advances are having an impact on long-standing questions within geochronology, planetary science and other fields. Future developments are likely to bring significant expansion in this research space

Lunar samples record an impact 4.2 billion years ago that may have formed the Serenitatis Basin

Impact cratering on the Moon and the derived size-frequency distribution functions of lunar impact craters are used to determine the ages of unsampled planetary surfaces across the Solar System. Radiometric dating of lunar samples provides an absolute age baseline, however, crater-chronology functions for the Moon remain poorly constrained for ages beyond 3.9 billion years. Here we present U–Pb geochronology of phosphate minerals within shocked lunar norites of a boulder from the Apollo 17 Station 8. These minerals record an older impact event around 4.2 billion years ago, and a younger disturbance at around 0.5 billion years ago. Based on nanoscale observations using atom probe tomography, lunar cratering records, and impact simulations, we ascribe the older event to the formation of the large Serenitatis Basin and the younger possibly to that of the Dawes crater. This suggests the Serenitatis Basin formed unrelated to or in the early stages of a protracted Late Heavy Bombardment

Trace-element heterogeneity in rutile linked to dislocation structures: Implications for Zr-in-rutile geothermometry

The trace-element composition of rutile is commonly used to constrain P-T-t-conditions for a wide range of metamorphic systems. However, recent studies have demonstrated the redistribution of trace elements in rutile via high-diffusivity pathways and dislocation-impurity associations related to the formation and evolution of microstructures. Here we investigate trace-element migration in low-angle boundaries formed by dislocation creep in rutile within an omphacite vein of the Lago di Cignana unit (Western Alps, Italy). Zr-in-rutile thermometry and inclusions of quartz in rutile and of coesite in omphacite constrain the conditions of rutile deformation to around the prograde boundary from high pressure to ultra-high pressure (~2.7 GPa) at temperatures of 500–565 °C. These results constrain the conditions of deformation of rutile and its effects on composition. Crystal-plastic deformation of a large rutile grain results in low-angle boundaries that generate a total misorientation of ~25°. Dislocations constituting one of these low-angle boundaries are enriched in common and uncommon trace elements, including Fe and Ca, providing evidence for diffusion and trapping of trace elements along the dislocation cores. The role of dislocation microstructures as fast-diffusion pathways must be evaluated when applying high-resolution analytical procedures as compositional disturbances might lead to erroneous interpretations for Ca and Fe. In contrast, our results indicate a trapping mechanism for Zr

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

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