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A method for mapping submicron-scale crystallographic order/disorder applied to human tooth enamel
Tooth enamel, the outermost layer of human teeth, is a complex, hierarchically structured biocomposite. The details of this structure are important in multiple human health contexts, from understanding the progression of dental caries (tooth decay) to understanding the process of amelogenesis and related developmental defects. Enamel is composed primarily of long, nanoscale crystallites of hydroxyapatite that are bundled by the thousands to form micron-scale rods. Studies with transmission electron microscopy show the relationships between small groups of crystallites and X-ray diffraction characterize averages over many rods, but the direct measurement of variations in local crystallographic structure across and between enamel rods has been missing. Here, we describe a synchrotron X-ray-based experimental approach and a novel analysis method developed to address this gap in knowledge. A ~500-nm-wide beam of monochromatic X-rays in conjunction with a sample section only 1 μm in thickness enables 2D diffraction patterns to be collected from small well-separated volumes within the enamel microstructure but still probes enough crystallites (~300 per pattern) to extract population-level statistics on crystallographic features like lattice parameter, crystallite size, and orientation distributions. Furthermore, the development of a quantitative metric to characterize relative order and disorder based on the azimuthal autocorrelation of diffracted intensity enables these crystallographic measurements to be correlated with their location within the enamel microstructure (e.g., between rod and interrod regions). These methods represent a step forward in the characterization of human enamel and will elucidate the variation of the crystallographic structure across and between enamel rods for the first time.
Experimental evidence that halogen bonding catalyzes the heterogeneous chlorination of alkenes in submicron liquid droplets
The heterogeneous chlorination rate of an alkene is unexpectedly accelerated in the presence of spectator molecules containing oxygenated functional groups, which suggests weak halogen bonds can catalyze reactions at liquid surfaces.
Experimental phase diagram and its temporal evolution for submicron 2-methylglutaric acid and ammonium sulfate aerosol particles
The experimental phase diagram for liquid–liquid phase separation in submicrometer aerosol particles converges with theory as equilibration time is increased.
Quasi-deterministic localization of Er emitters in thin film TiO 2 through submicron-scale crystalline phase control
With their shielded 4f orbitals, rare-earth ions (REIs) offer optical and electron spin transitions with good coherence properties even when embedded in a host crystal matrix, highlighting their utility as promising quantum emitters and memories for quantum information processing. Among REIs, trivalent erbium (Er 3+ ) uniquely has an optical transition in the telecom C-band, ideal for transmission over optical fibers, making it well suited for applications in quantum communication. The deployment of Er 3+ emitters into a thin film TiO 2 platform has been a promising step toward scalable integration; however, like many solid-state systems, the deterministic spatial placement of quantum emitters remains an open challenge. Here, we investigate laser annealing as a means to locally tune the optical resonance of Er 3+ emitters in TiO 2 thin films on Si. Using both nanoscale x-ray diffraction measurements and cryogenic photoluminescence spectroscopy, we show that tightly focused below-gap laser annealing can induce anatase to rutile phase transitions in a nearly diffraction-limited area of the films and improve local crystallinity through grain growth. As a percentage of Er:TiO 2 is converted to rutile, the Er 3+ optical transition blueshifts by 13 nm. We explore the effects of changing laser annealing time and show that the amount of optically active Er:rutile increases linearly with laser power. We additionally demonstrate local phase conversion on microfabricated Si structures, which holds significance for quantum photonics.
Optimization of submicron Ni/Au/Ge contacts to an AlGaAs/GaAs two-dimensional electron gas
We report on fabrication and performance of sub-micrometer Ni/Au/Ge contacts to a two-dimensional electron gas in an AlGaAs/GaAs heterostructure. Utilizing scanning transmission electron microscopy, energy dispersive x-ray spectroscopy, and low temperature electrical measurements, we investigate the relationship between contact performance and the mechanical and chemical properties of the annealed metal stack. Contact geometry and crystallographic orientation significantly impact performance. Our results indicate that the spatial distribution of germanium in the annealed contact plays a central role in the creation of high transmission contacts. We characterize the transmission of our contacts at high magnetic fields in the quantum Hall regime. Our work establishes that contacts with an area of 0.5 μm2 and resistance less than 400 Ω can be fabricated with high yield.
Automated segmentation of soft X-ray tomography: Native cellular structure with submicron resolution at high-throughput for whole-cell quantitative imaging in yeast
Soft X-ray tomography (SXT) is an invaluable tool for quantitatively analyzing cellular structures at suboptical isotropic resolution. However, it has traditionally depended on manual segmentation, limiting its scalability for large datasets. Here, we leverage a deep learning-based autosegmentation pipeline to segment and label cellular structures in hundreds of cells across three Saccharomyces cerevisiae strains. This task-based pipeline uses manual iterative refinement to improve segmentation accuracy for key structures, including the cell body, nucleus, vacuole, and lipid droplets, enabling high-throughput and precise phenotypic analysis. Using this approach, we quantitatively compared the three-dimensional (3D) whole-cell morphometric characteristics of wild-type, VPH1-GFP, and vac14 strains, uncovering detailed strain-specific cell and organelle size and shape variations. We show the utility of SXT data for precise 3D curvature analysis of entire organelles and cells and detection of fine morphological features using surface meshes. Our approach facilitates comparative analyses with high spatial precision and statistical throughput, uncovering subtle morphological features at the single-cell and population level. This workflow significantly enhances our ability to characterize cell anatomy and supports scalable studies on the mesoscale, with applications in investigating cellular architecture, organelle biology, and genetic research across diverse biological contexts.
Searching for new interactions at submicron scale using the Mössbauer effect
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Submicron Thickness Characterization of Poly-Si Thin Films on Textured Surfaces by X-Ray Diffraction for Minimizing Parasitic Absorption in Poly-Si/SiO2 Passivating Contact Cells
Poly-Si/SiO2 passivating contacts have shown great potential for industry-relevant next-generation solar cells. Previous work has demonstrated an improved Jsc from dry reactive ion etching in an SF6 environment, using front metal grids as a self-aligned mask. Here, we show an effective method to measure the front poly-Si thickness on an alkaline textured surface using X-ray diffraction. The calculated thicknesses are compared with cross-section SEM analysis and Quokka simulation. We show that by thinning the front poly-Si from 200 nm to 60 nm, Jsc increases by 2.4 mA/cm2, leading to an absolute efficiency gain of 1.73%. Finally, we discuss possible reasons for the premature loss of passivation before the removal of all poly-Si.
Submicron focusing of high-energy X-rays with silicon saw-tooth refractive lenses: fabrication and aberrations
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Submicron focusing of high-energy X-rays with silicon saw-tooth refractive lenses – fabrication and aberrations: errata
Three (3) items of errata are submitted for our recently published paper [ Opt. Express 28 , 36505 ( 2020 ) 10.1364/OE.405566 ]. One is a clarifying extension to the Fig. 3 caption. Two are typographical corrections. The scientific results and conclusions are unaffected.
The sources and diurnal variations of submicron aerosols in a coastal–rural environment near Houston, US
Aerosol properties were characterized at a rural site southwest of Houston from May to September 2022 during the intensive operation periods (IOPs) of the Tracking Aerosol Convection Interactions ExpeRiment (TRACER). Backward trajectory analysis reveals three major air mass types: marine air mass from the Gulf, urban air mass influenced by urban emissions, and regional air mass. Marine aerosols typically show a bimodal size distribution and have the lowest particle number and mass concentrations of PM 1 (particulate matter with an aerodynamic diameter of less than 1 µm), while aerosols from air masses strongly influenced by urban emissions exhibit the highest concentrations. Organic aerosol (OA) accounts for more than 50 % of PM 1 for urban and regional air masses, whereas sulfate is comparable to OA in marine air masses. Positive matrix factorization (PMF) analysis of aerosol mass spectra identifies 6 OA factors: hydrocarbon-like OA (HOA), OA from the oxidation of monoterpenes (MT-SOA), OA from the reactive uptake of isoprene epoxydiols by acidic sulfate particles (isoprene-SOA), oxygenated OA arising from shipping emissions (shipping-OOA), and two oxygenated OA factors with high O : C ratios (OOA1 and OOA2). OOA2 has the highest O : C ratio and exhibits elevated mass concentration in the afternoon. Similar diurnal variation of highly oxidized OA factors was commonly observed in the Houston area during previous studies and attributed to the SOA formation by photochemistry and mixing from aloft. Here, using air mass backward trajectories and a 1-D box model, we show the diurnal trend of OOA2 mass concentration is instead driven by changes in air mass arriving at the rural site. The air mass changes are likely caused by the shift between land breezes and sea/bay breezes. Within the same air mass type (e.g., either urban or marine air mass), OOA2 mass concentration is largely independent of wind direction and shows essentially no diurnal variation, suggesting OOA2 is related to aged OA with minimal influence by local emissions. This study helps identify the major sources of OA in the Houston region and highlights the impacts of both atmospheric chemistry and meteorology on aerosol properties in the coastal–rural environment.
Dynamic submicron particulate behavior in turbulent media, STL-008-20, Year 2 of 3
Presentation to be presented during the Site-Directed Research and Development (SDRD) program FY 2021 review meeting (Webex), September 22–23, 2021.
Dynamic submicron particulate behavior in turbulent media, STL-008-20, Year 2 of 3
Presentation to be presented during the Site-Directed Research and Development (SDRD) program FY 2021 review meeting (Webex), September 22–23, 2021.
An Instrumental Platform for Identifying, Collecting, and Analyzing Particles with Micron and Submicron Dimensions
Explore the source record for details and available documents.
Dynamics of Liquid–Liquid Phase Separation in Submicrometer Aerosol
Nanoscale materials, when compared to their bulk components, possess unique properties. In particular, shifts in phase transitions can occur for submicron particles. For instance, small particles do not undergo the process of liquid-liquid phase separation (LLPS). LLPS has applications in emulsions such as Janus particles, controllable morphology to create drug-rich phases during drug delivery, and is often observed in atmospheric aqueous aerosol particles. In atmospheric particles, LLPS is tracked as a function of particle water activity, which is equivalent to the relative humidity (RH) at equilibrium. We probed three organic/inorganic aerosol systems in the range of RH over which phase separation occurs (SRH). Our findings indicate that SRH for submicron aerosol particles is lower than for micron-sized droplets. These findings show that it may be necessary to update the representation of phase transitions in aerosol particles in climate models. The vast majority of organic/inorganic aerosol particles have submicron diameters, and a decrease in SRH for submicron particles indicates that the current estimation of phase separated aerosols may be overestimated. Furthermore, understanding the properties of LLPS at the nanoscale can provide key parameters to describe these systems and may lead to better control of phase separation in submicron particles.
High Semi-Volatile Organic Aerosol Contributions Associated with Ammonium Nitrate in the Coastal Urban Environment
Organic components often contribute 50% or more of the submicron aerosol mass in coastal urban environments, but their partitioning between the gas and particle phases is controlled by a complex mixture of unidentified organic compounds that are poorly constrained by observations. This study compares daily filter organic functional groups (OFG) with online organic mass fragments from La Jolla, California, as part of the Eastern Pacific Cloud Aerosol Precipitation Experiment (EPCAPE), quantifying the contributions of four types of non-volatile (NV) organic emission sources to the submicron composition. Daily filters retained only 0.79–0.98 µg/m3 NV submicron organic mass concentration, even though 1.8–1.9 µg/m3 non-refractory (NR) submicron organic mass concentration was measured online. The 62–64% of measured NR submicron organic mass concentration that exceeded what remained on the filters after 23-hr sampling is interpreted as semi-volatile, consistent with the moderate correlation of the NR NV difference to NR ammonium, NR nitrate, and biomass burning-related NV and NR organic factors. The association between semi-volatile organic components and ammonium nitrate likely results from both co-emission and co-evaporation. Size-resolved filter analysis showed that NV organic mass concentration accounts for 68% of NR organic mass concentration for 0.5–1 µm dry diameter but account for 9.0% for 0.18–0.5 µm dry diameter showing the differences in volatility between particle modes. Importantly, volatility of organic components was size-dependent Information Classification: General and associated with ammonium nitrate and biomass burning, providing guidance for constraining atmospheric aerosol properties in global models.
Colloid-Facilitated Actinide Transport in a Cementitious-Impacted SRS Groundwater
The objective of this report is to provide a literature review relevant to the question of whether colloid facilitated transport of plutonium is enhanced in a cementitious groundwater system on the Savannah River Site (SRS). Contaminant transport is commonly described as taking place in a system with a mobile aqueous phase and an immobile solid phase. There has been an increasing awareness of a third phase, a mobile solid phase, also referred to as a mobile colloidal phase. Mobile colloids consist of organic and/or inorganic submicron-particles that move with groundwater flow. When radionuclides are associated with the mobile colloids, the net effect is that radionuclides can move faster through the subsurface system than would be predicted by transport models that do not include mobile colloids. It is important to distinguish between subsurface colloids and subsurface mobile colloids. The subsurface environment includes an enormous reservoir of colloids, but only a tiny fraction, if any, are mobile. Mobile colloid formation is commonly described as involving a three-step process: genesis, stabilization, and transport. It was concluded that there is a strong likelihood that submicron colloids of plutonium exist near the source term, (i.e., the genesis step is likely completed). While such particles have not been directly detected, it is highly likely that plutonium could either attach to submicron particles in the sediment or that submicron plutonium fragments exist at the source. However, the tendency for these plutonium colloids to move in the SRS subsurface is extremely low, especially in engineered cementitious environments where the ionic strength of the solution and the elevated concentrations of divalent cations greatly curtails colloid suspension stability (i.e., the stabilization step is likely not completed). Together these data strongly indicate that plutonium-bearing colloids would likely exist in the near field of a tank closure facility, but the colloids would be unlikely to be mobile, thereby providing a vector for enhanced transport. Under cementitious leachate impacted groundwater conditions, it is reasonable to assume plutonium transport occurs primarily as a two-phase system, a mobile aqueous phase and an immobile solid phase.