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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 649 records · Page 36
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

Information depth in backscattered electron microscopy of nanoparticles within a solid matrix

Highlights: • Backscattered electron microscopy was used for reliable determination of nanoparticle density and sizes within Al alloys • Backscattered electron information depth was determined as a function of nanoparticle size from Monte Carlo simulations • Unlike transmission electron microscopy, the method is non-destructive and allows analyzing large sample areas • Good agreement with transmission electron microscopy data shows that our method is suitable for nanocomposite materials - Abstract: Measuring the dimensions and number density of nanoparticles dispersed in a solid matrix is usually accomplished via transmission electron microscopy (TEM) which suffers from high cost, low throughput, and small analytical volume. In comparison, scanning backscattered electron microscopy is inexpensive, requires little sample preparation, and allows for the analysis of large sample areas. However, the information depth is usually not known precisely and depends on several factors such as the composition of the nanoparticles and the matrix as well as the size of the nanoparticles, hindering the reconstruction of the actual size distribution and three-dimensional number density. Here we present a method to estimate the information depth for spherical nanoparticles of different sizes in order to accurately determine size distribution and number density. The approach is based on Monte Carlo simulation of electron trajectories in the material and analysis of the obtained backscattered electron signal-to-noise-ratio. Our experimental results are compared to those obtained via TEM and good agreement is demonstrated; this shows that TEM can be replaced by scanning electron microscopy for studying nanocomposites in many cases.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
NASA NTRS2022

An Evaluation of the Liquid Cloud Droplet Effective Radius Derived from MODIS, Airborne Remote Sensing, and in Situ Measurements from CAMP2Ex

The cloud drop effective radius (Re) of the drop size distribution derived from passive satellite sensors is a key variable used in climate research. Validation of these satellite products has often taken place under stratiform cloud conditions that favor the assumption of cloud horizontal homogeneity used by the retrieval techniques. However, many studies have noted concerns with respect to significant biases in retrieved Re arising from cloud heterogeneity, for example, in cumulus cloud fields. Here, we examine data collected during the 2019 “Cloud, Aerosol and Monsoon Processes Philippines Experiment” (CAMP2Ex), which, in part, targeted the objective of providing the first detailed evaluation of Re retrieved across multiple platforms and techniques in a cumulus and congestus cloud region. Our evaluation consists of cross-comparisons of Re between the Moderate Resolution Imaging Spectroradiometer (MODIS) onboard the Terra satellite, the Research Scanning Polarimeter (RSP) onboard the NASA P-3 aircraft, and in situ measurements from both the NASA P-3 and Learjet aircraft that are all taken in close spatiotemporal proximity to the same cloud fields. A particular advantage of our approach lies in the capability of the RSP to retrieve Re using a bi-spectral MODIS approach and a polarimetric approach, which allows for the evaluation of bi-spectral and polarimetric Re retrievals from an airborne perspective using the same samples. Averaged over all P-3 flight segments examined here for warm clouds, the RSP polarimetric method, the in situ method, and the bias-adjusted MODIS method of Fu et al. (2019) show a comparable median (mean ± standard deviation) for the Re samples of 9.6 (10.2 ± 4.0) µm, 11.0 (13.6 ± 11.3) µm, and 10.4 (10.8 ± 3.8) µm, respectively. These values are far lower than the values of 15.1 (16.2 ± 5.5) µm and 17.2 (17.7 ± 5.7) µm from the bi-spectral retrievals of RSP and MODIS, respectively. Similar results are observed when Re is segregated by cloud-top height and in detailed case studies. The clouds sampled during CAMP2Ex consist of mostly small (mean transect length ∼ 1.4 km) and low clouds (mean cloud-top height ∼ 1 km), which had more numerous small clouds than the trade wind cumuli sampled in past field campaigns such as Rain in Shallow Cumulus over the Ocean (RICO) and the Indian Ocean Experiment (INDOEX). The overestimates of Re from the RSP bi-spectral technique compared with the polarimetric technique increased as cloud size and cloud optical depth decreased. Drizzle, cloud-top bumpiness, and solar zenith angle, however, are not closely correlated with the overestimate of bi-spectral Re. For shallow clouds that dominated the liquid cloud cover for the CAMP2Ex region and period, we show that 3-D radiative transfer and cloud heterogeneity, particularly for the optically thin and small clouds, appear to be the leading cause of the large positive biases in bi-spectral retrievals. Because this bias varies with the underlying structure of the cloud field, caution continues to be warranted in studies that use bi-spectral Re retrievals in cumulus cloud fields.

Cloud microphysics↗
NASA NTRS1977

The application of LANDSAT-1 imagery for monitoring strip mines in the new river watershed in northeast Tennessee, part 2

The author has identified the following significant results. LANDSAT imagery and supplementary aircraft photography of the New River drainage basin were subjected to a multilevel analysis using conventional photointerpretation methods, densitometric techniques, multispectral analysis, and statistical tests to determine the accuracy of LANDSAT-1 imagery for measuring strip mines of common size. The LANDSAT areas were compared with low altitude measurements. The average accuracy over all the mined land sample areas mapped from LANDSAT-1 was 90%. The discrimination of strip mine subcategories is somewhat limited on LANDSAT imagery. A mine site, whether active or inactive, can be inferred by lack of vegetation, by shape, or image texture. Mine ponds are difficult or impossible to detect because of their small size and turbidity. Unless bordered and contrasted with vegetation, haulage roads are impossible to delineate. Preparation plants and refuge areas are not detectable. Density slicing of LANDSAT band 7 proved most useful in the detection of reclamation progress within the mined areas. For most state requirements for year-round monitoring of surface mined land, LANDSAT is of limited value. However, for periodic updating of regional surface maps, LANDSAT may provide sufficient accuracies for some users.

Shahrokhi, F.↗
NASA NTRS2017

Field Exploration and Life Detection Sampling Through Planetary Analogue Sampling (FELDSPAR).

Exploration missions to Mars rely on rovers to perform analyses over small sampling areas; however, landing sites for these missions are selected based on large-scale, low-resolution remote data. The use of Earth analogue environments to estimate the multi-scale spatial distributions of key signatures of habitability can help ensure mission science goals are met. A main goal of FELDSPAR is to conduct field operations analogous to Mars sample return in its science, operations, and technology from landing site selection, to in-field sampling location selection, remote or stand-off analysis, in situ analysis, and home laboratory analysis. Lava fields and volcanic regions are relevant analogues to Martian landscapes due to desiccation, low nutrient availability, and temperature extremes. Operationally, many Icelandic lava fields are remote enough to require that field expeditions address several sampling constraints that are experienced in robotic exploration, including in situ and sample return missions. The Fimmvruhls lava field was formed by a basaltic effusive eruption associated with the 2010 Eyjafjallajkull eruption. Mlifellssandur is a recently deglaciated plain to the north of the Myrdalsjkull glacier. Holuhraun was formed by a 2014 fissure eruptions just north of the large Vatnajkull glacier. Dyngjusandur is an alluvial plain apparently kept barren by repeated mechanical weathering. Informed by our 2013 expedition, we collected samples in nested triangular grids every decade from the 10 cm scale to the 1 km scale (as permitted by the size of the site). Satellite imagery is available for older sites, and for Mlifellssandur, Holuhraun, and Dyngjusandur we obtained overhead imagery at 1 m to 200 m elevation. PanCam-style photographs were taken in the field by sampling personnel. In-field reflectance spectroscopy was also obtained with an ASD spectrometer in Dyngjusandur. All sites chosen were 'homogeneous' in apparent color, morphology, moisture, grain size, and reflectance spectra at all scales greater than 10 cm. Field lab assays were conducted to monitor microbial habitation, including ATP quantification, qPCR for fungal, bacterial, and archaeal DNA, and direct cell imaging using fluorescence microscopy. Home laboratory analyses include Raman spectroscopy and community sequencing. ATP appeared to be significantly more sensitive to small changes in sampling location than qPCR or fluorescence microscopy. Bacterial and archaeal DNA content were more consistent at the smaller scales, but similarly variable across more distant sites. Conversely, cell counts and fungal DNA content have significant local variation but appear relatively homogeneous over scales of 1 km. ATP, bacterial DNA, and archaeal DNA content were relatively well correlated at many spatial scales. While we have observed spatial variation at various scales and are beginning to observe how that variation fluctuates over time as biodiversity recovers after an eruption, we do not yet fully understand what parameters lead to the observed spatial variation. Home laboratory analyses will help us further understand the elemental and structural composition of the basaltic matrices, but further field analyses are vital for the understanding how temperature, moisture, incident radiation, and so forth influence the habitability of a microclimate.

Field↗
DOE OSTI2018

Development of Hot-Isostatic Pressing for Treatment of UK ILW Radioactive Wastes - 18280

Hot-Isostatic Pressing (HIPing) has been proposed as an improved method for the treatment of radioactive wastes in the UK. Sludges and slurries housed on the Sellafield site are a prime candidate for HIP treatment due to their large volumes and issues associated with the use of the baseline cementation strategy. Options have been developed by GeoRoc Ltd to co-process these wastes, including a detailed conceptual plant design. This paper will describe research and development aimed at demonstrating the viability of the concept presented in this design. This paper summarizes two studies performed to address the knowledge gaps identified for treatment of these wastes using HIP technology. The first study related to the poorly characterized nature of the wastes, which requires any treatment option to be flexible in terms of the chemical and physical properties of the waste feed. The second study involved demonstrating that HIPing can be effectively utilized at a scale applicable to treat a waste inventory estimated to be in excess of 5,000 m{sup 3}. The first section of this paper presents a summary of research carried out to determine where variation in the waste stream composition may affect the processing and wasteform produced when HIPing Magnox sludges. This study aimed to qualify where restrictions on the process envelope may exist due to poorly defined waste-stream characteristics. A baseline wasteform was selected with the aim of achieving significant waste volume reduction, while producing a physically and chemically stable wasteform. A glass-bonded magnesium-titanate/magnesium-silicate wasteform was selected as the preferred option for the Magnox sludge wastes. A series of studies investigated the densification and phase formation of waste-forms by altering key variables in the Magnox sludge simulant. To test the extremes of the processable waste loading, samples were produced and characterized at 100 wt% waste-loading for Magnox sludge, Site-Ion Exchange Plant (SIXEP) sand/clinoptilolite and a 50:50 mix of the two waste-streams. Further studies involved a) altering the waste loading to additive mass ratio (to simulate changes in the waste loading/sludge solids content), b) varying the particle size distribution from the datum to include only small or large particulates in the sludge feed; and c) introducing up to 20 wt% metallic Magnox alloy, organic species or carbonate materials (to determine how their inclusion may affect the processing and densification of the materials). A U{sub 3}O{sub 8} loaded sample was also produced using the baseline Magnox sludge formulation. All the tests performed were shown to produce monolithic, well densified waste-forms with substantial volume reductions. Minimal variations from the baseline were noted but the waste-forms produced with these deviations was determined to be of comparable quality to of the baseline product. U{sub 3}O{sub 8} was shown to behave in a similar fashion to the ZrO{sub 2} surrogate used to simulate it in the process envelope studies and was encapsulated in the magnesium titanate/magnesium silicate matrix. This work demonstrates that HIP technology can successfully produce waste-forms across the broad process envelope expected in the Magnox sludge inventory. It is also possible to produce monolithic waste-forms at 100 wt% waste loading from Magnox sludges, SIXEP sand clinoptilolite slurries or a co-processed mixture of the two. The second part of this paper summarizes a commercially relevant demonstration of HIP technology for the treatment of sludge and slurry wastes housed at the Sellafield site (UK). This study culminated in production of the largest HIPed wasteform successfully produced to date. This study was performed in a series of stages. Investigations into formulation and properties of waste-forms were performed at a lab scale to evaluate suitable wasteform systems and identify suitable combinations of additives and waste loadings. Scale up demonstrations were then performed in stages with custom-designed HIP canisters. Scale-up and characterization of key wasteform properties were successfully performed with initial canister volumes of 50 ml, 400 ml and 8 L. Suitable front-end unit operations to produce a granular, free-flowing calcined simulant were demonstrated at an engineering scale. The demonstration was successful in processing a HIP canister with an initial starting volume in excess of 100 L. A 75 % volume reduction from the raw sludge was achieved at scale while demonstrating that HIP is applicable at suitably large scale for immobilization of ILW waste. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2014

Synthesis of Fe/SiO{sub 2} and iron oxides/SiO{sub 2} nanocomposites by long-term ball milling

Graphical abstract: - Highlights: • Iron–iron oxides/silica composites are synthesized by long term dry ball-milling. • Bcc iron and α-quartz powders are used as precursors. • Surface effects enhance coercivity in iron/silica nanocomposites. • In spite of their small size, about 10 nm, iron particles are ferromagnetic. • Ferro and superparamagnetic particles are found in maghemite/silica composites. - Abstract: Iron oxide/SiO{sub 2} nanocomposites are synthesized by dry ball-milling a mixture of bcc Fe and α-quartz powders for prolonged times. A sequence of nanocomposites is obtained, with small magnetic particles dispersed in a non magnetic, amorphous matrix. The powders are characterized by X-ray diffraction and transmission electron microscopy. The magnetic hysteresis properties are investigated in the range 50–300 K. After 120 h milling, deformed, non-spherical, α-Fe nanocrystallites of about 10 nm in size and very few small (<10 nm) maghemite particles are found. At room temperature, iron particles are ferromagnetic and a large effective magnetic anisotropy is estimated, which is mainly attributed to surface effects. Between 160 and 200 h milling, maghemite nanoparticles are observed while after 220 h grinding, hematite phase appears; after 340 h milling, the sample consists of ferromagnetic hematite particles with a broad size distribution (5–50 nm) embedded in an amorphous matrix.

36 MATERIALS SCIENCE↗
NASA NTRS2014

Coordinated Microanalyses of Seven Particles of Probable Interstellar Origin from the Stardust Mission

Stardust, a NASA Discovery-class mission, was the first sample-return mission to return solid samples from beyond the Moon. Stardust was effectively two missions in one spacecraft: it returned the first materials from a known primitive solar system body, the Jupiter-family comet Wild 2; Stardust also returned a collector that was exposed to the contemporary interstellar dust stream for 200 days during the interplanetary cruise. Both collections present severe technical challenges in sample preparation and in analysis. By far the largest collection is the cometary one: approximately 300 micro g of material was returned from Wild 2, mostly consisting of approx. 1 ng particles embedded in aerogel or captured as residues in craters on aluminum foils. Because of their relatively large size, identification of the impacts of cometary particles in the collection media is straightforward. Reliable techniques have been developed for the extraction of these particles from aerogel. Coordinated analyses are also relatively straightforward, often beginning with synchrotron-based x-ray fluorescence (S-XRF), X-ray Absorption Near-Edge Spectoscopy (XANES) and x-ray diffraction (S-XRD) analyses of particles while still embedded in small extracted wedges of aerogel called ``keystones'', followed by ultramicrotomy and TEM, Scanning Transmission X-ray Microscopy (STXM) and ion microprobe analyses (e.g., Ogliore et al., 2010). Impacts in foils can be readily analyzed by SEM-EDX, and TEM analysis after FIB liftout sample preparation. In contrast, the interstellar dust collection is vastly more challenging. The sample size is approximately six orders of magnitude smaller in total mass. The largest particles are only a few pg in mass, of which there may be only approx.10 in the entire collection. The technical challenges, however, are matched by the scientific importance of the collection. We formed a consortium carry out the Stardust Interstellar Preliminary Examination (ISPE) to carry out an assessment of this collection, partly in order to characterize the collection in sufficient detail so that future investigators could make well-informed sample requests. The ISPE is the sixth PE on extraterrestrial collections carried out with NASA support. Some of the basic questions that we asked were: how many impacts are there in the collector, and what fraction of them have characteristics consistent with extraterrestrial materials? What is the elemental composition of the rock-forming elements? Is there crystalline material? Are there organics? Here we present coordinated microanalyses of particles captured in aerogel, using S-FTIR, S-XRF, STXM, S-XRD; and coordinated microanalyses of residues in aluminum foil, using SEMEDX, Auger spectroscopy, STEM, and ion microprobe. We discuss a novel approach that we employed for identification of tracks in aerogel, and new sample preparation techniques developed during the ISPE. We have identified seven particles - three in aerogel and four in foils - that are most consistent with an interstellar origin. The seven particles exhibit a large diversity in elemental composition. Dynamical evidence, supported supported by laboratory simulations of interstellar dust impacts in aerogel and foils, and numerical modeling of interstellar dust propagation in the heliosphere, suggests that at least some of the particles have high optical cross-section, perhaps due to an aggregate structure. However, the observations are most consistent with a variety of morphologies

Westphal, Andrew J.↗
DOE OSTI2016

Graphene addition to MgB{sub 2} superconductor obtained by ex-situ spark plasma sintering technique

Highlights: • Graphene-added dense MgB{sub 2} was prepared by ex-situ spark plasma sintering. • There is a limited interaction between graphene and MgB{sub 2}. • Addition of graphene (G) shows a small enhancement of J{sub c} and μ{sub 0}H{sub irr}. • G is one of the least effective C-containing additions. - Abstract: Graphene nanopowder (G) with average thickness particle size of about 6–8 nm was added to MgB{sub 2} commercial powder. Starting composition was (MgB{sub 2}){sub (1−x)}(G){sub x}, x = 0.0125, 0.025, 0.05. Processing was performed by Spark Plasma Sintering (SPS) technique. All added samples have high density (above 95%). The critical temperature (T{sub c}) and the lattice parameter a (c-axis lattice parameter is constant) show a small variation suggesting that carbon substitution for boron is low. TEM observations show the presence of un-reacted graphene plates supporting the T{sub c} and structural results. It also indicates that G-addition does not modify the MgB{sub 2} microstructure. Despite this, there is an optimum doped sample (MgB{sub 2}){sub 0.9875}(G){sub 0.0125} for which the critical current density at temperatures below 25 K is slightly higher at high magnetic fields than for the pristine sample. The addition of G is found as one of the least effective C-source additions enhancing J{sub c}. We discuss results as being strongly related to variation of the residual stress.

36 MATERIALS SCIENCE↗
DOE OSTI2019

SANS coupled with fluid invasion approaches for characterization of overall nanopore structure and mesopore connectivity of organic-rich marine shales in China

The pore structure of shales, including pore morphology, connectivity, pore volume, specific surface area (SSA), and pore size distribution (PSD), is a significant factor in controlling gas storage and transport and the migration mechanisms of hydrocarbons. However, the lack of comprehensive characterization for both accessible and inaccessible pore structure increases the difficulty of gas-in-place estimation and gas exploration. In order to investigate the nanoscale pore system, integration of high-pressure mercury intrusion porosimetry (MIP), low-pressure N 2 /CO 2 adsorption (LNA/LCA), and small-angle neutron scattering (SANS) were employed to obtain a multi-scale quantitative characterization of the nanopore structure of organic-rich marine shale samples from the Longmaxi and Niutitang Formations in China. In this work, PSDs obtained from the combined techniques appropriately cover an overall nanopore size range of shale (0.35–15,000 nm) and overcome the limits of the individual method. Uni-, bi, and multi-modal PSDs were observed, but the sizes of a significant portion of the nanopores observed in these shales range from 0.35 to 100 nm. Pore volumes and surface areas of micropores (<2 nm), mesopores (2–50 nm), and macropores (>50 nm) were characterized based on the best performance window of each technique: LCA for micropores; LNA and SANS for mesopores; and MIP for macropores. It was found that micropores are the major contributor to the total SSA for both the Longmaxi and Niutitang shales. With respect to pore volume, however, the contribution to the total pore volume has a trend of micropore < mesopore < macropore for the Longmaxi shale samples, but micro-/mesopore volumes are greater than macropore volumes for samples of the Niutitang shale. Strong correlations were also observed between total organic carbon (TOC) content and micropore volume and surface area, which implies that organic matter is a controlling factor in the micropore system of organic-rich shales. In addition, strong correlations between methane adsorption capacity and both micro-/mesopore volumes and SSAs indicate that micro-/mesopores are governing factors for methane storage. Furthermore, the fractions of accessible mesopore volume and surface area were quantitatively estimated by SANS and LNA. Correlation analyses suggest that the accessibility of the mesopore surface area could be an indicator for gas transport and storage in mesopores in organic matter. Thus, a shale with higher connectivity could have higher gas diffusion capability but lower gas adsorption capacity, and vice versa.

58 GEOSCIENCES↗
DOE OSTI2015

Simple correction for the sample shape and radial offset effects on SQUID magnetometers: Magnetic measurements on Ln{sub 2}O{sub 3} (Ln=Gd, Dy, Er) standards

An increased focus on magnetic measurements of oriented single crystals, thin films, and magnetically dilute systems has led to a demand for the measurement of weak magnetic moments. This level of sensitivity and precision can be achieved on SQUID magnetometers by decreasing the size of the detection coils. However, the smaller detection coils can amplify two errors in the magnitude of the measured moment, the sample shape and radial offset effects, which were small and typically unaccounted for on previous magnetometers. We report a simple method to determine the radial offset of a sample by taking advantage of the two basic scan modes, DC and lock-in, typically used on magnetometers. This technique allows for the correction of the sample shape and radial offset effects in order to obtain the true moment of a sample. To show the efficacy of this technique, we report the magnetic properties of Ln{sub 2}O{sub 3} (Ln=Gd, Dy, Er). - Graphical abstract: Correction for the sample shape and radial offset effects on SQUID magnetometers using a combination of DC and VSM scan data. - Highlights: • Sample shape and radial offset effects alter the moment measured by magnetometers. • We present a simple method to correct for these sample effects on magnetometers. • We measure magnetic susceptibilities of Ln{sub 2}O{sub 3} to show the efficacy of this method.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2018

Effects of the annealing process on the structure and valence state of vanadium oxide thin films

Highlights: • TGA-DSC was used to determine the annealing temperature generally. • Pure VO{sub 2} (M) film was obtained with some annealing process. • The film surface transits from layer to grains as the annealing temperature increases. • Spans of O1s and V2p{sub 3/2} core level of V{sup 5+}, V{sup 4+}, V{sup 3+} were 12.75, 14.0 and 14.7 eV. • The Tc of pure VO{sub 2} (M) was 64.3 °C, its hysteresis loop width was 12.1 °C. - Abstract: V{sub 2}O{sub 5} was used to prepare vanadium oxide films via the sol-gel method. The “n” in V{sub 2}O{sub 5}∙nH{sub 2}O was determined to be approximately 1.67. After annealing at 390 °C for 4 h, a pure VO{sub 2} (M) phase was obtained and denoted sample Ⅴ. The crystallite sizes of VO{sub 2} (M) in samples Ⅱ, Ⅲ, Ⅳ and Ⅴ were 42, 41, 35 and 24 nm, respectively. The surface morphology of sample Ⅰ was flat; however, many small, dense particles covered the surface of sample Ⅴ. Sample Ⅱ had a layered structure, and samples Ⅲ and Ⅳ consisted of compact grains. The binding energy (BE) differences between the O1s and the V{sup 5+}2p{sub 3/2}, V{sup 4+}2p{sub 3/2}, and V{sup 3+}2p{sub 3/2} core levels were 12.75, 14.0 and 14.7 eV, respectively. For the sample Ⅴ film, the maximum transmittance change at 2500 nm was 39%, the phase transition temperature (Tc) was 64.3 °C, and the hysteresis loop width was 12.1 °C.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Embedding PbS Quantum Dots (QDs) in Pb-Halide Perovskite Matrices: QD Surface Chemistry and Antisolvent Effects on QD Dispersion and Confinement Properties

Hybrid materials of metal chalcogenide colloidal quantum dots (QDs) embedded in metal halide perovskites (MHPs) have led to composites with synergistic properties. Here, we investigate how QD size, surface chemistry, and MHP film formation methods affect the resulting optoelectronic properties of QD/MHP “dot-in-matrix” systems. We monitor the QD absorption and photoluminescence throughout synthesis, ligand exchange, and transfer into the MHP ink, and we characterize the final QD/MHP films via electron microscopy and transient absorption. In addition, we are the first to globally map how PbS QDs are distributed on the micrometer scale within these dot-in-matrix systems, using three-dimensional (3D) tomography time-of-flight secondary ion mass spectrometry. The surface chemistry imparted during synthesis directly affects the optical properties of the dot-in-matrix composites. Pb-halide passivation leads to QD/MHP dot-in-matrix samples with optical properties that are well-described by a theoretical model, based on a Type I finite-barrier heterostructure between the PbS QD and the MHP matrix. Samples without Pb-halide passivation show complicated size-dependent behavior, indicating a transition from a Type I heterostructure between the PbS QD wells and MHP barriers for small-sized QDs to PbS QDs that are electronically decoupled from the MHP matrix for larger QDs. Furthermore, the choice in perovskite antisolvent crystallization method leads to a difference in the spatial QD distribution within the perovskite matrix, differences in carrier lifetime, and photoluminescence shifts of up to 180 meV for PbS in methylammonium lead iodide. This work establishes an understanding of such emerging synergistic systems relevant for technologies such as photovoltaics, infrared emitters and detectors, and other unexplored technological applications.

92 SC - Basic Energy Sciences (BES) (SC-22)↗
DOE OSTI2013

Reactive triblock polymers from tandem ring-opening polymerization for nanostructured vinyl thermosets

Multiply functional hydroxyl telechelic poly(cyclooctene-s-5-norbornene-2-methylene methacrylate) was synthesized by ring opening metathesis (co)polymerization of cis-cyclooctene and 5-norbornene-2-methylene methacrylate using the second generation Grubbs catalyst in combination with a symmetric chain transfer agent bearing hydroxyl functionality. The resulting hydroxyl-telechelic polymer was used as a macroinitiator for the ring opening transesterification polymerization of d,l-lactide to form reactive poly(lactide)-b-poly(cyclooctene-s-5-norbornene-2-methylene methacrylate)-b-poly(lactide) triblock polymers. Subsequently, the triblocks were crosslinked by free radical copolymerization with several vinyl monomers including styrene, divinylbenzene, methyl methacrylate, and ethyleneglycol dimethacrylate. Certain conditions led to optically transparent thermosets with mesoscale phase separation as evidenced by small angle X-ray scattering, differential scanning calorimetry and transmission electron microscopy. Disordered, bicontinuous structures with nanoscopic domains were generated in several cases, rendering the samples attractive for size-selective membrane applications.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Direct observation of the kinetics of gas–solid reactions using in situ kinetic and spectroscopic techniques

Developing fundamental insight for reactions between gas phase H 2 S and solid phase CuO has the potential to lead to improved materials and processes for natural gas purification. However, this insight requires detailed knowledge of the atomistic characteristics of the solid and how these characteristics influence the reaction mechanism and kinetics. Herein, we use fixed bed reactors, X-ray absorption spectroscopy, and transmission X-ray microscopy to simultaneously probe the fundamental kinetics of the reaction of CuO with H 2 S to form CuS, and thereby probe spatial-temporal chemical and structural changes of copper during this reaction. H 2 S removal reaction kinetics show similar trends in fixed bed reactors as in 10-20 µm sized particles. However, reaction fronts proceed through the entire diameter of particles heterogeneously, indicating the presence of pore diffusion resistance even at very small length scales. In addition, CuO sorbent samples with similar characteristics exhibit 3 times different sulfidation conversion with reaction rate constants that differ by a factor of 1.5. Furthermore, these differences in reaction kinetics and conversion indicate the critical impact of possible atomic scale differences and the formation of different copper sulfide products.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

SURVEY SIMULATIONS OF A NEW NEAR-EARTH ASTEROID DETECTION SYSTEM

We have carried out simulations to predict the performance of a new space-based telescopic survey operating at thermal infrared wavelengths that seeks to discover and characterize a large fraction of the potentially hazardous near-Earth asteroid (NEA) population. Two potential architectures for the survey were considered: one located at the Earth–Sun L1 Lagrange point, and one in a Venus-trailing orbit. A sample cadence was formulated and tested, allowing for the self-follow-up necessary for objects discovered in the daytime sky on Earth. Synthetic populations of NEAs with sizes as small as 140 m in effective spherical diameter were simulated using recent determinations of their physical and orbital properties. Estimates of the instrumental sensitivity, integration times, and slew speeds were included for both architectures assuming the properties of newly developed large-format 10 μm HgCdTe detector arrays capable of operating at ∼35 K. Our simulation included the creation of a preliminary version of a moving object processing pipeline suitable for operating on the trial cadence. We tested this pipeline on a simulated sky populated with astrophysical sources such as stars and galaxies extrapolated from Spitzer Space Telescope and Wide-field Infrared Explorer data, the catalog of known minor planets (including Main Belt asteroids, comets, Jovian Trojans, planets, etc.), and the synthetic NEA model. Trial orbits were computed for simulated position-time pairs extracted from the synthetic surveys to verify that the tested cadence would result in orbits suitable for recovering objects at a later time. Our results indicate that the Earth–Sun L1 and Venus-trailing surveys achieve similar levels of integral completeness for potentially hazardous asteroids larger than 140 m; placing the telescope in an interior orbit does not yield an improvement in discovery rates. This work serves as a necessary first step for the detailed planning of a next-generation NEA survey.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2017

Neutron Imaging of Laser Melted SS316 Test Objects with Spatially Resolved Small Angle Neutron Scattering

A novel neutron far field interferometer is explored for sub-micron porosity detection in laser sintered stainless steel alloy 316 (SS316) test objects. The results shown are images and volumes of the first quantitative neutron dark-field tomography at various autocorrelation lengths, ξ . In this preliminary work, the beam defining slits were adjusted to an uncalibrated opening of 0.5 mm horizontal and 5 cm vertical; the images are blurred along the vertical direction. In spite of the blurred attenuation images, the dark-field images reveal structural information at the micron-scale. The topics explored include: the accessible size range of defects, potentially 338 nm to 4.5 μ m, that can be imaged with the small angle scattering images; the spatial resolution of the attenuation image; the maximum sample dimensions compatible with interferometry optics and neutron attenuation; the procedure for reduction of the raw interferogram images into attenuation, differential phase contrast, and small angle scattering (dark-field) images; and the role of neutron far field interferometry in additive manufacturing to assess sub-micron porosity.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Towards large-cohort comparative studies to define the factors influencing the gut microbial community structure of ASD patients

Differences in the gut microbiota have been reported between individuals with autism spectrum disorders (ASD) and neurotypical controls, although direct evidence that changes in the microbiome contribute to causing ASD has been scarce to date. Here we summarize some considerations of experimental design that can help untangle causality in this complex system. In particular, large cross-sectional studies that can factor out important variables such as diet, prospective longitudinal studies that remove some of the influence of interpersonal variation in the microbiome (which is generally high, especially in children), and studies transferring microbial communities into germ-free mice may be especially useful. Controlling for the effects of technical variables, which have complicated efforts to combine existing studies, is critical when biological effect sizes are small. Large citizen-science studies with thousands of participants such as the American Gut Project have been effective at uncovering subtle microbiome effects in self-collected samples and with self-reported diet and behavior data, and may provide a useful complement to other types of traditionally funded and conducted studies in the case of ASD, especially in the hypothesis generation phase.

59 BASIC BIOLOGICAL SCIENCES↗
NASA NTRS1984

Case study of sample spacing in planar near-field measurement of high gain antennas

Far field antenna patterns can be reconstructed from planar near field measurements acquired at a sample spacing of lambda/2 or less. For electrically large antennas, sampling at the Nyquist rate may result in errors due to system electronic drift over long acquisition times. The computer capacity may limit the largest size of the near field data set. The requirement to sample at the Nyquist rate is relaxed for high gain antennas which concentrate most of the radiated energy into a small angular region of the far field. The criteria for sample spacing at greater than lambda/e through the use of a priori information of the antenna radiation characteristics are presented. Far field patterns of a 30 GHz dual offset reflector system with a 2.7 m parabolic main reflector are computed from near field data obtained at sample spacings ranging from 0.1 lambda to 10 lambda. The effects of sampling interval and spectrum cutoff on the far field patterns are discussed.

Acosta, R. J.↗