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  1. Do We Really Need All That Data: From Data to Agency in Automated Microscopy

    Microscopy is entering an era of automated laboratories and AI-enabled instruments, often justified by a simple narrative of automating experiments to collect more data and train better models. Here we argue that, for microscopy, this framing is incomplete and can be counterproductive.
  2. Characterizing microscale signatures in uranium ore concentrates using electron probe microanalyzer

    Impurities in uranium ore concentrates (UOCs) serve as forensic signatures of processing history and origin. Here, this study utilizes Electron Probe Microanalyzer (EPMA) to characterize microscale compositional and textural features in individual UOC particles from both commercial and bench-scale production. At the particle scale, multiple internal phases with distinct morphologies, chemical signatures, and stoichiometries are documented. Our data shows that chemical impurities are heterogeneously distributed within single particles and among particles within a sample. These microscale heterogeneities correlate with known processing histories, indicating that microscale signatures of early fuel cycle materials can provide valuable information for nuclear forensic material analysis.
  3. Deconstruction by C. thermocellum—from microbe mediated to dynamic redistribution of cellulosomes

    Clostridium thermocellum is one of the most efficient microorganisms for the deconstruction of cellulosic biomass. To achieve this high level of cellulolytic activity, C. thermocellum uses large multienzyme complexes known as cellulosomes to break down complex polysaccharides, notably cellulose, found in plant cell walls. The attachment of bacterial cells to the nearby substrate via the cellulosome has been hypothesized to be the reason for this high efficiency. The region lying between the cell and the substrate has shown great variation and dynamics that are affected by the growth stage of cells and the substrate used for growth. Here, we usedmore » both super-resolution imaging and machine-learning approaches to study the distribution of C. thermocellum cellulosomes at different stages of growth. We show that C. thermocellum initially retains its cellulosomes primarily on the cell surface but then relocates large cellulosome clusters to the interface with biomass, therefore depleting its cell surface of cellulosomes. These results indicate dynamic redistribution of cellulosomes during growth, with a functional shift toward substrate-associated degradation later during growth on biomass.« less
  4. Scanning transmission election microscopy observations of twisted epitaxial gold nanodiscs in twisted molybdenum disulfide bilayers

    Atomic scale, scanning transmission electron microscopy (STEM) analysis of the moiré structures in twisted epitaxial gold nanodiscs encapsulated in twisted bilayer molybdenum disulfide is presented. High angle annular dark field STEM imaging reveals that the period of the moiré patterns between gold and molybdenum disulfide varies with different twist angles of the bilayer molybdenum disulfide, ranging from 1.80 nm (epitaxial alignment of gold) to 1.53 nm (twisted epitaxial alignment of gold). Additionally, bright field STEM imaging reveals a faint, larger "moiré of moiré" structure in cases where the bilayer molybdenum disulfide twist angle is small (~6°), arising from the overlappingmore » three-layers, which is not visible in conventional transmission electron microscopy images. In conclusion, our experiments indicate that scanning transmission electron microscopy as a suitable tool for moiré analysis of twisted multilayer planar heterostructures, complementary to information provided by conventional transmission electron microscopy and diffraction.« less
  5. Fabrication and characterization of boron-terminated tetravacancies in monolayer hBN using STEM, EELS and electron ptychography

    Tetravacancies in monolayer hexagonal boron nitride (hBN) with consistent edge termination (boron or nitrogen) form triangular nanopores with electrostatic potentials that can be leveraged for applications such as selective ion transport and neuromorphic computing. In order to quantitatively predict the properties of these structures, an atomic-level understanding of their local electronic and chemical environments is required. Moreover, robust methods for their precision manufacture are needed. Here we use electron irradiation in a scanning transmission electron microscope (STEM) at a high dose rate to drive the formation of boron-terminated tetravacancies in monolayer hBN. Characterization of the defects is achieved using aberration-correctedmore » STEM, monochromated electron energy-loss spectroscopy (EELS), and electron ptychography. Z-contrast in STEM and chemical fingerprinting by core-loss EELS enable identification of the edge terminations, while electron ptychography gives insight into structural relaxation of the tetravacancies and provides evidence of enhanced electron density around the defect perimeters indicative of bonding effects.« less
  6. Facet-Dependent Doping and Dopant-Dependent Faceting in Si-doped GaAsSb Nanowires

    In this work, we correlate the spatial distributions of Si, Sb, and rotational twins in Si-doped GaAs1 xSbx nanowires. GaAs1-xSbx nanowires were grown epitaxially on Si(111) substrates by tuning process conditions to achieve repeated nucleation of rotational twins and growth along the [111]B direction; dilute Sb and Si fluxes were chosen to create a sufficient twin density to achieve high yield while avoiding growth of the wurtzite phase. While the impact of Si and Sb on twin density and nanowire growth rate has been previously reported, the facet-dependent incorporation of these species has not been established. Scanning transmission electron microscopymore » was used to confirm that Sb incorporates preferentially on the (111)B facets relative to {1 ̅1 ̅0} facets prior to nucleation of a rotational twin. With periodic twinning, this facet dependence leads to alternating regions of enriched and depleted Sb concentration attributed to a growth rate-dependent Sb-As-exchange mechanism. Atom probe tomography measurements establish that while Si doping is not perturbed by twinning on (111)B facets, Si and Sb concentrations are anti-correlated for growth on non-(111)B facets. Density functional theory calculations underpin a thermodynamic model that explains the observed anisotropies in dopant incorporation.« less
  7. Stimulated Raman Scattering Microscopy: Real-Time In-Situ Physical and Chemical Characterization of Reverse Osmosis Desalination Membrane Scaling

    We introduce a stimulated Raman scattering (SRS) methodology designed for rapid, real-time, and in situ monitoring of RO membrane scaling adapted for bench-scale desalination flow cells. The methodology can provide new insights into membrane scaling dynamics by offering time-resolved reflection imaging of inorganic crystal growth, coupled with chemical identification from Raman spectral data. These capabilities allow for direct local measurement of the membrane surface area covered by different scalants as well as an approximation of the scalant volume using three-dimensional, integrated Raman intensity. The 2D and 3D SRS results obtained from CaSO4 scaling experiments are compared to and are inmore » reasonable agreement with those provided by confocal microscopy. The real-time physical and chemical characterization capabilities presented here could be extended to study combinations of inorganic, organic, and biological fouling. Overall, the SRS methodology represents an advancement in real-time sensing of membrane fouling that offers the potential for improved operation, lower cost, and more resilient RO membrane systems for sustainable water management.« less
  8. A collection of archaeal 16S rRNA Clone-FISH cultures for probe validation in fluorescence in situ hybridization experiments

    We present a collection of 30 Escherichia coli cultures (Clone-FISH cultures), each carrying a plasmid for the heterologous expression of a (near) full-length 16S rRNA gene from 1 of 30 lineages of archaea, including 17 yet uncultured ones. We make these clones available for use as controls in fluorescence in situ hybridization experiments.
  9. Nanoscale Tracking of the High-Temperature Spin-State Transition in LaCoO3

    The high-temperature spin and electronic transitions in LaCoO3 have recently been leveraged to create neuromorphic (brain-inspired) devices. While these devices have shown the potential for impactful functionality in next-generation computing systems, the nanoscale dynamics of the spin and electronic transitions that underlie their operation are not well understood. Inhomogeneities related to interfaces, electrode contacts, strain, and crystal defects can all affect device performance, making nanoscale characterization of the transitions essential for producing consistent and reliable devices. Here, we demonstrate the first nanoscale in situ measurement of the spin transition in LaCoO3 at device-relevant temperatures (25–325 °C) over length scales ofmore » tens of nanometers using STEM-EELS. This measurement is enabled by an Al2O3 coating, which prevents unwanted reduction of the LaCoO3 specimen at high temperature and vacuum. The detailed understanding of LaCoO3 transition dynamics enabled by such measurements will be crucial for optimizing LaCoO3-based neuromorphic devices and increasing reliability for real-world application.« less
  10. Beyond Optimization: Exploring Novelty Discovery in Autonomous Experiments

    Autonomous experiments (AEs) are transforming how scientific research is conducted by integrating artificial intelligence with automated experimental platforms. Current AEs primarily focus on the optimization of a predefined target; while accelerating this goal, such an approach limits the discovery of unexpected or unknown physical phenomena. Here, we introduce a novel framework, INS2ANE (Integrated Novelty Score−Strategic Autonomous Non-Smooth Exploration), to enhance the discovery of novel phenomena in autonomous microscopy experimentation. Our method integrates two key components: (1) a novelty scoring system that evaluates the uniqueness of experimental results and (2) a strategic sampling mechanism that promotes exploration of under-sampled regions evenmore » if they appear less promising by conventional criteria. We validate this approach on a preacquired data set with a known ground truth comprising of image−spectral pairs. We further implement the process on autonomous scanning probe microscopy experiments. INS2ANE significantly increases the diversity of explored phenomena in comparison to conventional optimization routines, enhancing the likelihood of discovering previously unobserved phenomena. These results demonstrate the potential for autonomous microscopy experiments to enhance the scientific discovery by navigating complex experimental spaces to uncover novel phenomena.« less
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aberration corrected scanning transmission electron microscopy AC STEM

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