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At least 1,783 records · Page 99

Evidence of root zone hypoxia in Brassica rapa L. grown in microgravity

A series of experiments was conducted aboard the U.S. space shuttle and the Mir space station to evaluate microgravity-induced root zone hypoxia in rapid-cycling Brassica (Brassica rapa L.), using both root and foliar indicators of low-oxygen stress to the root zone. Root systems from two groups of plants 15 and 30 d after planting, grown in a phenolic foam nutrient delivery system on the shuttle (STS-87), were harvested and fixed for microscopy or frozen for enzyme assays immediately postflight or following a ground-based control. Activities of fermentative enzymes were measured as indicators of root zone hypoxia and metabolism. Following 16 d of microgravity, ADH (alcohol dehydrogenase) activity was increased in the spaceflight roots 47% and 475% in the 15-d-old and 30-d-old plants, respectively, relative to the ground control. Cytochemical localization showed ADH activity in only the root tips of the space-grown plants. Shoots from plants that were grown from seed in flight in a particulate medium on the Mir station were harvested at 13 d after planting and quick-frozen and stored in flight in a gaseous nitrogen freezer or chemically fixed in flight for subsequent microscopy. When compared to material from a high-fidelity ground control, concentrations of shoot sucrose and total soluble carbohydrate were significantly greater in the spaceflight treatment according to enzymatic carbohydrate analysis. Stereological analysis of micrographs of sections from leaf and cotyledon tissue fixed in flight and compared with ground controls indicated no changes in the volume of protoplast, cell wall, and intercellular space in parenchyma cells. Within the protoplasm, the volume occupied by starch was threefold higher in the spaceflight than in the ground control, with a concomitant decrease in vacuolar volume in the spaceflight treatment. Both induction of fermentative enzyme activity in roots and accumulation of carbohydrates in foliage have been repeatedly shown to occur in response to root zone oxygen deprivation. These results indicate that root zone hypoxia is a persistent challenge in spaceflight plant growth experiments and may be caused by microgravity-induced changes in fluid and gas distribution.

long duration↗

[Cyto-embryologic investigation of super dwarf wheat grown on board of the Mir orbital complex]

The cytoembryologic analysis of wet and dry samples of super dwarf wheat cultivated in greenhouse SVET aboard the MIR station over the whole cycle of vegetation was made with the use of light microscopy. Characteristic features of wheat development in space flight are plentiful early tillering, and formation and rapid growth of side shoots. Elementary spikelets in the composite head were more numerous but the top spikelets were rudimentary and, therefore, the ripe head contained less of these spikelets as compared with the ground controls (9-13 and 14, respectively). The number of florets in a spike was also higher reaching 14-16 vs. 7-8 in the control. Typically, no more than 4 to 5 florets vs. 3 in the control were fully differentiated while the others died off earlier in development. The fact that there were no caryopses found in the flight crop is explained by absolute male sterility appearing at different stages of staminal development: before archesporium formation, on the stage of differentiated archesporium, during meiosis, on the stage of microspores or uninucleate "pollen". The female generative system developed mainly without abnormalities. An assumption was made that elevated ethylene concentrations in the MIR atmosphere at the time of the wheat experiment were the cause for abnormal development of the male generative system which led to barrenness of the super dwarf wheat crop.

manned↗

Electron-Beam-Related Studies of Halide Perovskites: Challenges and Opportunities

Electron beam microscopy and related characterization techniques play an important role in revealing the microstructural, morphological, physical, and chemical information of halide perovskites and their impact on associated optoelectronic devices. However, electron beam irradiation usually causes damage to these beam-sensitive materials, negatively impacting their device performance, and complicating this interpretation. Here, the electron microscopy and spectroscopy techniques are reviewed that are crucial for the understanding of the crystallization and microstructure of halide perovskites. In addition, special attention is paid to assessing and mitigating the electron beam-induced damage caused by these techniques. Since the halide perovskites are fragile, a protocol involving delicate control of both electron beam dose and dose rate, coupled with careful data analysis, is key to enable the acquisition of reliable structural and compositional information such as atomic-resolution images, chemical elemental mapping and electron diffraction patterns. Limiting the electron beam dose is critical parameter enabling the characterization of various halide perovskites. Novel methods to unveil the mechanisms of device operation, including charge carrier generation, diffusion, and extraction are presented in scanning electron microscopy studies combined with electron-beam-induced current and cathodoluminescence mapping. Future opportunities for electron-beam-related characterizations of halide perovskites are also discussed.

36 MATERIALS SCIENCE↗

Analysis of Phase Separation in Czochralski Grown Single Crystal Ilmenite

Ilmenite (FeTiOs) is a wide bandgap semiconductor with an energy gap of 2.58 eV. Ilmenite has properties suited for radiation tolerant applications, as well as a variety of other electronic applications. Single crystal ilmenite has been grown from the melt using the Czochralski method. Growth conditions have a profound effect on the microstructure of the samples. Here we present data from a variety of analytical techniques which indicate that some grown crystals exhibit distinct phase separation during growth. This phase separation is apparent for both post-growth annealed and unannealed samples. Under optical microscopy, there appear two distinct areas forming a matrix with an array of dots on order of 5 pm diameter. While appearing bright in the optical micrograph, atomic force microscope (AFM) shows the dots to be shallow pits on the surface. Magnetic force microscope (MFM) shows the dots to be magnetic. Phase identification via electron microprobe analysis (EMPA) indicates two major phases in the unannealed samples and four in the annealed samples, where the dots appear to be almost pure iron. This is consistent with micrographs taken with a scanning probe microscope used in the magnetic force mode. Samples that do not exhibit the phase separation have little or no discernible magnetic structure detectable by the MFM.

Wilkins, R.↗

Characterization of dissipative regions of a N-doped superconducting radio-frequency cavity

We report radio-frequency measurements of quality factors and temperature mapping of a nitrogen doped Nb superconducting RF cavity. Cavity cutouts of hot and cold spots were studied with low temperature scanning tunneling microscopy and spectroscopy, X-ray photoelectron spectroscopy and secondary electron microscopy. Temperature mapping revealed a substantial reduction of the residual resistance upon cooling the cavity with a greater temperature gradient and hysteretic losses at the quench location, pointing to trapped vortices as the dominant source of residual surface resistance. Analysis of the tunneling spectra in the framework of a proximity effect theory shows that hot spots have a reduced pair potential and a wider distribution of the contact resistance between the Nb and the top Nb oxide. Alone, these degraded superconducting properties account for a much weaker excess dissipation as compared with the vortex contribution. Based on the correlation between the quasiparticle density of states and temperature mapping, we suggest that degraded superconducting properties may facilitate vortex nucleation or settling of trapped flux during cooling the cavity through the critical temperature.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Tilted fluctuation electron microscopy

Fluctuation electron microscopy (FEM) is a scanning nanodiffraction-based method that offers a unique approach to characterizing nanometer-scale medium-range order (MRO) in disordered materials. In addition to determining the degree of MRO, careful analysis of scanning nanodiffraction data can also be used to determine strain in thin film amorphous samples. We applied FEM to characterize the strain and MRO of magnetron sputtered amorphous tantalum (a-Ta) thin films over a range of tilt angles from 0° to 45° in order to measure any deviations between the in-plane and out-of-plane strain and MRO. We validate our approach using electron diffraction simulations of FEM experiments for a-Ta. We measure anisotropic strain in the simulated a-Ta diffraction patterns and find that the experimental a-Ta is isotropically strained within the accuracy of our method. Our approach provides a workflow for acquiring tilted scanning nanodiffraction data, determining the relative strain and ordering as a function of in- A nd out-of-plane directions, and removing any artifacts induced in FEM data due to strain. We also describe some limitations of the tilted FEM method when applied to thin films with very low strains.

36 MATERIALS SCIENCE↗

Thermal cycling-driven microstructural changes of eutectic Al–Si phase change materials in SS304 containers revealed by multi-modal imaging

Aluminum-based Al–Si alloys are widely used as phase change materials (PCMs) in thermal energy storage (TES) systems owing to their high volumetric latent heat and superior thermal conductivity. However, their long-term reliability is limited by degradation processes that remain insufficiently understood. In this work, we employ a multimodal, correlative characterization framework to systematically resolve the degradation behavior of eutectic Al–Si PCMs in contact with SS304 containers under repeated thermal cycling. By integrating high-resolution electron microscopy, three-dimensional X-ray fluorescence (3D XRF) imaging, and differential scanning calorimetry (DSC), we directly link spatially resolved compositional and microstructural evolution to changes in thermophysical properties. The correlative analysis reveals that elemental leaching of Fe, Cr, and Ni from the stainless-steel container into the PCM drives the formation of intermetallic compounds (IMCs) both at the interface and within the bulk PCM, leading to pronounced compositional heterogeneity. These interfacial reactions and diffusion-induced transformations progressively destabilize the Al–Si eutectic, reducing the effective phase-transforming fraction. Consistent with these observations, DSC measurements show a decrease in melting temperature and latent heat of fusion with thermal cycling. These results underscore the critical influence of interfacial reactions and material compatibility on the stability, durability, and overall performance of Al–Si-based TES systems.

25 ENERGY STORAGE↗

Electronic structure orientation as a map of in-plane antiferroelectricity in β'-In 2 Se 3

Antiferroelectric (AFE) materials are excellent candidates for sensors, capacitors, and data storage due to their electrical switchability and high-energy storage capacity. However, imaging the nanoscale landscape of AFE domains is notoriously inaccessible, which has hindered development and intentional tuning of AFE materials. Here, we demonstrate that polarization-dependent photoemission electron microscopy can resolve the arrangement and orientation of in-plane AFE domains on the nanoscale, despite the absence of a net lattice polarization. Through direct determination of electronic transition orientations and analysis of domain boundary constraints, we establish that antiferroelectricity in β'-In 2 Se 3 is a robust property from the scale of tens of nanometers to tens of micrometers. Ultimately, the method for imaging AFE domain organization presented here opens the door to investigations of the influence of domain formation and orientation on charge transport and dynamics.

36 MATERIALS SCIENCE↗

Nanocolumnar Pt:Ni Alloy Thin Films by High Pressure Sputtering for Oxygen Reduction Reaction

Self-supported nanocolumnar Pt:Ni thin films (TFs) with varying Pt:Ni atomic ratios and Pt mass loadings were produced on a microporous layer (MPL)-like surface composed of carbon particles by high pressure sputtering and examined as oxygen reduction reaction (ORR) electrocatalysts for polymer electrolyte membrane fuel cells. Cauliflower-like microstructures were observed from scanning electron microscopy imaging. Various Pt:Ni atomic ratios were obtained by simply changing the relative deposition power between Pt and Ni source and investigated by X-ray diffraction and quartz crystal microbalance analysis. Additionally, electrochemical characterization of the Pt:Ni-TF/MPL-like-layer/glassy-carbon samples was conducted through benchtop cyclic voltammetry and rotating disk electrode measurements. The electrochemically active surface area (ECSA) was found to be between 22–42 m 2 g -1 for different Pt:Ni atomic ratios. Lower Pt mass loadings exhibited a higher ECSA and the catalytic activity of all Pt:Ni ratios increased with the increase in Pt mass loading. The ORR activity of the Pt:Ni-TFs increased in the order of 3:1 < 1:1 < 1:3 with exhibiting a specific activity of 1781 μA cm -2 and mass activity of 0.66 A mg -1 for the Ni-rich film with 1:3 ratio. The catalytic performance of Pt:Ni-TFs were higher than traditional high surface area carbon supported Pt nanoparticles, elemental Pt nanorods, and Pt-Ni nanorods.

08 HYDROGEN↗

Impact- and Thermal-Resistant Epoxy Resin Toughened with Acacia Honey

High performance polymers with bio-based modifiers are promising materials in terms of applications and environmental impact. In this work, raw acacia honey was used as a bio-modifier for epoxy resin, as a rich source of functional groups. The addition of honey resulted in the formation of highly stable structures that were observed in scanning electron microscopy images as separate phases at the fracture surface, which were involved in the toughening of the resin. Structural changes were investigated, revealing the formation of a new aldehyde carbonyl group. Thermal analysis confirmed the formation of products that were stable up to 600 °C, with a glass transition temperature of 228 °C. An energy-controlled impact test was performed to compare the absorbed impact energy of bio-modified epoxy containing different amounts of honey with unmodified epoxy resin. The results showed that bio-modified epoxy resin with 3 wt% of acacia honey could withstand several impacts with full recovery, while unmodified epoxy resin broke at first impact. The absorbed energy at first impact was 2.5 times higher for bio-modified epoxy resin than it was for unmodified epoxy resin. In this manner, by using simple preparation and a raw material that is abundant in nature, a novel epoxy with high thermal and impact resistance was obtained, opening a path for further research in this field.

36 MATERIALS SCIENCE↗

Results of analyses performed on basalt adjacent to penetrators emplaced into volcanic rock at Amboy, California, April 1976

The physical and chemical modifications found in the basalt after impact of four penetrators were studied. Laboratory analyses show that mineralogical and elemental changes are produced in the powdered and crushed basalt immediately surrounding the penetrator. Optical microscopy studies of material next to the skin of the penetrator revealed a layer, 0-2 mm thick, of glass and abraded iron alloy mixed with fractured mineral grains of basalt. Elemental analysis of the 0-2 mm layer revealed increased concentrations of Fe, Cr, Ni, No, and Mn, and reduced concentrations of Mg, Al, Si, and Ca. The Fe, Cr, Ni, and Mo were in fragments abraded from the penetrator. Mineralogical changes occurring in the basalt sediment next to the penetrator include the introduction of micron-size grains of alpha-iron, magnetite, and hematite. The newly formed silicate minerals include metastable phases of silica (tridymite and cristobalite). An increased concentration of Fe, Cr, Ni, and Mo occurred in the 2-mm to 1-cm layer of penetrator no. 1, which impacted at the highest velocity. No elemental concentration increase was noted for penetrators nos. 2 and 3 in the 2-mm to 1-cm layer. Contaminants introduced by the penetrator occur up to 1 cm away from the penetrator's skin. Although volatile elements do migrate and new minerals are formed during the destruction of host minerals in the crushed rock, no changes were observed beyond the 1-cm distance.

Blanchard, M.↗

Kinetics of crystal nucleation and growth in Pd(40)Ni(40)P(20) glass

Samples of Pd(40)Ni(40)P(20) glass, produced by cooling the melt at 1 or 800 K/s, are heated in a differential scanning calorimeter to determine the crystallization kinetics. Optical microscopy shows that eutectic crystallization proceeds both by growth from the surface of the samples and by the growth of spherical regions around preexisting nuclei in the interior. A modified Kissinger (1957) analysis is used to obtain the activation energy for crystal growth (3.49 eV). The steady state homogeneous nucleation frequency at 590 K is about 10 million/cu m per sec. This is estimated to be the maximum nucleation frequency: it is too low to account for the observed population of quenched-in nuclei, which are therefore presumed to be heterogeneous. The major practical obstacle to glass formation in this system is heterogeneous nucleation.

Drehman, A. J.↗

Microstructural, Chemical and Mechanical Characterization of Polymer-Derived Hi-Nicalon Fibers with Surface Coatings

Room temperature tensile strengths of as-received Hi-Nicalon fibers and those having BN/SiC, p-BN/SiC, and p-B(Si)N/SiC surface coatings, deposited by chemical vapor deposition, were measured using an average fiber diameter of 13.5 microns. The Weibull statistical parameters were determined for each fiber. The average tensile strength of uncoated Hi-Nicalon on was 3.19 +/- 0.73 GPa with a Weibull modulus of 5.41. Strength of fibers coated with BN/SiC did not change. However, coat with p-BN/SiC and p-B(Si)N/SiC surface layers showed strength loss of approx. 10 and 35 percent, respectively, compared with as-received fibers. The elemental compositions of the fibers and the coatings were analyzed using scanning Auger microprobe and energy dispersive x-ray spectroscopy. The BN coating was contaminated with a large concentration of carbon and some oxygen. In contrast, p-BN, p-B(Si)N, and SiC coatings did not show any contamination. Microstructural analyses of the fibers and the coatings were done by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected area electron diffraction. Hi-Nicalon fiber consists of the P-SIC nanocrystals ranging in size from 1 to 30 nm embedded in an amorphous matrix. TEM analysis of the BN coating revealed four distinct layers with turbostatic structure. The p-BN layer was turbostratic and showed considerable preferred orientation. The p-B(Si)N was glassy and the silicon and boron were uniformly distributed. The silicon carbide coating was polycrystalline with a columnar structure along the growth direction. The p-B(Si)N/SiC coatings were more uniform, less defective and of better quality than the BN/SiC or the p-BN/SiC coatings.

Bansal, Narottam P.↗

Sintering effects on NpO 2 grain size and morphology: The role of precursor Np phase

Neptunium dioxide (NpO 2 ) is a key phase in nuclear material processing as a target material for the production of plutonium-238 ( 238 Pu) and has been historically synthesized via the calcination of a Np oxalate precursor. Alternative synthesis methods for NpO 2 are now more prevalent, necessitating their study and comparison with the more common oxalate route. The purpose of this work was to investigate the microstructural properties of NpO 2 synthesized from a nitrate-based Np precursor phase via the assessment of NpO 2 particle size and morphology as a function of calcination temperature and time. Scanning electron microscopy (SEM) was used to probe the primary grain size and morphology of NpO 2 after calcination at temperatures ranging from 700 to 1100 °C and hold times ranging from 1 to 10 h. Post-image analysis using ImageJ software enabled the quantification of mean particle diameter. This analysis indicated that particle diameter increases with both increasing calcination temperature and hold time. Primary particles were shown to be clumped in irregular patterns into the overall rough, blocky aggregates, but this macroscopic morphology was not affected by calcination time or temperature. Although trends in primary grain size of NpO 2 were consistent with available literature from other Np precursor phases, the macroscopic morphology of the NpO 2 aggregates was quite different than reported for other precursors. Through comparison with historical literature on Np oxalate, this work emphasizes the importance of Np precursor on the physical properties of NpO 2 .

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

Biomolecular Analysis Capability for Cellular and Omics Research on the International Space Station

International Space Station (ISS) assembly complete ushered a new era focused on utilization of this state-of-the-art orbiting laboratory to advance science and technology research in a wide array of disciplines, with benefits to Earth and space exploration. ISS enabling capability for research in cellular and molecular biology includes equipment for in situ, on-orbit analysis of biomolecules. Applications of this growing capability range from biomedicine and biotechnology to the emerging field of Omics. For example, Biomolecule Sequencer is a space-based miniature DNA sequencer that provides nucleotide sequence data for entire samples, which may be used for purposes such as microorganism identification and astrobiology. It complements the use of WetLab-2 SmartCycler"TradeMark", which extracts RNA and provides real-time quantitative gene expression data analysis from biospecimens sampled or cultured onboard the ISS, for downlink to ground investigators, with applications ranging from clinical tissue evaluation to multigenerational assessment of organismal alterations. And the Genes in Space-1 investigation, aimed at examining epigenetic changes, employs polymerase chain reaction to detect immune system alterations. In addition, an increasing assortment of tools to visualize the subcellular distribution of tagged macromolecules is becoming available onboard the ISS. For instance, the NASA LMM (Light Microscopy Module) is a flexible light microscopy imaging facility that enables imaging of physical and biological microscopic phenomena in microgravity. Another light microscopy system modified for use in space to image life sciences payloads is initially used by the Heart Cells investigation ("Effects of Microgravity on Stem Cell-Derived Cardiomyocytes for Human Cardiovascular Disease Modeling and Drug Discovery"). Also, the JAXA Microscope system can perform remotely controllable light, phase-contrast, and fluorescent observations. And upcoming confocal microscopy capability will allow for optical sectioning of biological tissues to determine microanatomical localization of biomarkers. Furthermore, NASA's geneLAB effort addresses integration of genomic, epigenomic, transcriptomic, proteomic and metabolomic datasets, by applying an innovative open source science platform for multi-investigator high throughput utilization of the ISS. In sum, the expanding ISS capability for analysis of biomolecules is enabling innovative research in a broad spectrum of areas such as cellular and molecular biology, biotechnology, tissue engineering, biomedicine, and Omics, providing manifold benefits for humanity.

Guinart-Ramirez, Y.↗

Mechanisms of Polyethylene Terephthalate Pellet Fragmentation into Nanoplastics and Assimilable Carbons by Wastewater Comamonas

Comamonadaceae bacteria are enriched on poly(ethylene terephthalate) (PET) microplastics in wastewaters and urban rivers, but the PET-degrading mechanisms remain unclear. Here, we investigated these mechanisms with Comamonas testosteroniKF-1, a wastewater isolate, by combining microscopy, spectroscopy, proteomics, protein modeling, and genetic engineering. Compared to minor dents on PET films, scanning electron microscopy revealed significant fragmentation of PET pellets, resulting in a 3.5-fold increase in the abundance of small nanoparticles (<100 nm) during 30-day cultivation. Infrared spectroscopy captured primarily hydrolytic cleavage in the fragmented pellet particles. Solution analysis further demonstrated double hydrolysis of a PET oligomer, bis(2-hydroxyethyl) terephthalate, to the bioavailable monomer terephthalate. Supplementation with acetate, a common wastewater co-substrate, promoted cell growth and PET fragmentation. Of the multiple hydrolases encoded in the genome, intracellular proteomics detected only one, which was found in both acetate-only and PET-only conditions. Homology modeling of this hydrolase structure illustrated substrate binding analogous to reported PET hydrolases, despite dissimilar sequences. Mutants lacking this hydrolase gene were incapable of PET oligomer hydrolysis and had a 21% decrease in PET fragmentation; re-insertion of the gene restored both functions. Thus, we have identified constitutive production of a key PET-degrading hydrolase in wastewater Comamonas, which could be exploited for plastic bioconversion.

54 ENVIRONMENTAL SCIENCES↗