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At least 1,351 records · Page 75

Magnetic Properties of Co-doped Bismuth Oxide (δ-Bi{sub 2}O{sub 3}) at Low Temperature

The (Bi{sub 2}O{sub 3}){sub 1−x−y}(Gd{sub 2}O{sub 3}){sub x}(Lu{sub 2}O{sub 3}){sub y} material compounds were prepared by using the solid-state reaction technique under normal air conditions. The heat treatments of the ternary samples were performed firstly at 800 °C for 48 h and then at 750 °C for 100 h. The structural, morphological, and magnetic properties of the materials were characterized by X-ray powder diffraction (XRD), scanning electron microscope, and a Quantum Design PPMS-9T system, respectively. From the XRD results, it was found that the phases of all of the samples consisted of the fluorite-type face-centered cubic δ-Bi{sub 2}O{sub 3} phase. It was observed that the microstructure of the samples is uniformly distributed on the samples’ surface. The temperature dependence of magnetization (M–T) measurements showed that the magnetization rose sharply at the critical temperature. The calculated critical temperature values vary from 22.19 to 56.61 K for the samples. All of the samples displayed the paramagnetic behavior. The paramagnetic behavior started from 300 K to very low temperature which varied from 22.19 to 56.61 K. The coercive rise on the magnetization below 22.19 K or 56.61 K with decreasing temperature causes a phase transformation in the δ-Bi{sub 2}O{sub 3} system. This sudden increment was considered as a ferromagnetic or ferrimagnetic phase transition.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

High-Temperature Oxidation of Stellite 12 Hardfacings: Effect of Mo on Characteristics of Oxide Scale

This study aims to understand the oxide scale formation on the surfaces of commercial and Mo (10 wt.%)-modified Stellite 12 hardfacings deposited on 4140 steel. For this purpose, samples of the hardfacings were isothermally oxidized in air at various temperatures in between 500 and 900 °C for 30 h. As a result of changes in the microstructure upon Mo addition, about 50% higher mass gain at all oxidation temperatures was observed. The characteristics of the developed oxide scales were examined by utilizing Raman spectroscopy, scanning electron microscopy and x-ray diffraction analysis. The oxide scale formed over Stellite 12 consisted of CoO-, Co{sub 3}O{sub 4-} and Cr{sub 2}O{sub 3}-type oxides, while additionally CoMoO{sub 4}-type complex oxide was detected on Mo-modified hardfacing, more likely at the alloy–scale interface. On the basis of findings of isothermal oxidation tests, the formation mechanisms of this complex oxide imposing better wear resistance as reported in our previous studies were explained during high-temperature wear testing, i.e., dynamic oxidation conditions.

36 MATERIALS SCIENCE↗

The development of in situ fracture toughness evaluation techniques in hydrogen environment

Reliability of hydrogen pipelines and storage tanks is significantly influenced by the mechanical performance of the structural materials exposed in the hydrogen environment. Fracture behavior and fracture toughness are of specific interest since they are relevant to many catastrophic failures. However, many conventional fracture testing techniques are difficult to be realized under the presence of hydrogen. Thus it is desired to develop novel in situ techniques to study the fracture behavior of structural materials in hydrogen environments. In this study, special testing apparatus were designed to facilitate in situ fracture testing in H 2 . A torsional fixture was developed to utilize an emerging fracture testing technique, Spiral Notch Torsion Test (SNTT). The design concepts will be discussed. Preliminary in situ testing results indicated that the exposure to H 2 significantly reduces the fracture toughness of 4340 high strength steels by up to 50 percent. Furthermore, SNTT tests conducted in air demonstrated a significant fracture toughness reduction in samples subject to simulated welding heat treatment using Gleeble, which illustrated the effect of welding on the fracture toughness of this material.

08 HYDROGEN↗

Monolayer-crystal streptavidin support films provide an internal standard of cryo-EM image quality

Analysis of images of biotinylated Escherichia coli 70S ribosome particles, bound to streptavidin affinity grids, demonstrates that the image-quality of particles can be predicted by the image-quality of the monolayer crystalline support film. Also, the quality of the Thon rings is a good predictor of the image-quality of particles, but only when images of the streptavidin crystals extend to relatively high resolution. When the estimated resolution of streptavidin was 5 Å or worse, for example, the ribosomal density map obtained from 22,697 particles went to only 9.5 Å, while the resolution of the map reached 4.0 Å for the same number of particles, when the estimated resolution of streptavidin crystal was 4 Å or better. It thus is easy to tell which images in a data set ought to be retained for further work, based on the highest resolution seen for Bragg peaks in the computed Fourier transforms of the streptavidin component. The refined density map obtained from 57,826 particles obtained in this way extended to 3.6 Å, a marked improvement over the value of 3.9 Å obtained previously from a subset of 52,433 particles obtained from the same initial data set of 101,213 particles after 3-D classification. These results are consistent with the hypothesis that interaction with the air-water interface can damage particles when the sample becomes too thin. Finally, streptavidin monolayer crystals appear to provide a good indication of when that is the case.

59 BASIC BIOLOGICAL SCIENCES↗

Phase formation, crystal structures and magnetic properties of perovskite-type phases in the system La{sub 2}Co{sub 1+z}(Mg{sub x}Ti{sub 1-x}){sub 1-z}O{sub 6}

Perovskite-type cobaltates in the system La{sub 2}Co{sub 1+z}(Mg{sub x}Ti{sub 1-x}){sub 1-z}O{sub 6} were studied for z=0{<=}x{<=}0.6 and 0{<=}x<0.9, using X-ray and neutron powder diffraction, electron diffraction (ED), magnetic susceptibility measurements and X-ray absorption near-edge structure (XANES) spectroscopy. The samples were synthesised using the citrate route in air at 1350 {sup o}C. The space group symmetry of the structure changes from P2{sub 1}/n via Pbnm to R3-bar c with both increasing Mg content and increasing Co content. The La{sub 2}Co(Mg{sub x}Ti{sub 1-x})O{sub 6} (z=0) compounds show anti-ferromagnetic couplings of the magnetic moments for the Co below 15 K for x=0, 0.1 and 0.2. XANES spectra show for the compositions 0{<=}x{<=}0.5 a linear decrease in the L{sub 3}/(L{sub 3}+L{sub 2}) Co-L{sub 2,3} edge branching ratio with x, in agreement with a decrease of the average Co ion spin-state, from a high-spin to a lower-spin-state, with decreasing nominal Co{sup 2+} ion content. -- Graphical abstract: XRPD patterns for perovskite compounds along the lines La{sub 2}Co(Mg{sub x}Ti{sub 1-x})O{sub 6} and La{sub 2}Co{sub 1+z}(Mg{sub 0.5}Ti{sub 0.5}){sub 1-z}O{sub 6}. Display Omitted Research Highlights: {yields}Tuning of the oxidation state of Co in the perovskite system La{sub 2}Co{sub 1+z}(Mg{sub x}Ti{sub 1-x}){sub 1-z}O{sub 6}, z=0{<=}x{<=}0.6 and 0{<=}x<0.9. {yields}XANES study of the oxidation state of Co in the perovskite system La{sub 2}Co{sub 1+z}(Mg{sub x}Ti{sub 1-x}){sub 1-z}O{sub 6}, z=0{<=}x{<=}0.6 and 0{<=}x<0.9. {yields}Phase relations in the perovskite system La{sub 2}Co{sub 1+z}(Mg{sub x}Ti{sub 1-x}){sub 1-z}O{sub 6}, z=0{<=}x{<=}0.6 and 0{<=}x<0.9. {yields}Magnetic properties in the perovskite system La{sub 2}Co{sub 1+z}(Mg{sub x}Ti{sub 1-x}){sub 1-z}O{sub 6}, z=0{<=}x{<=}0.6 and 0{<=}x<0.9.

36 MATERIALS SCIENCE↗

A study on tensile properties of Alloy 709 at various temperatures

In recent years, there have been several advancements in energy production from both fossil fuels and the alternate “clean” sources such as nuclear fission. These advancements are fueled by the need for more efficient systems that will optimize the use of the depleting fossil fuel reserves and shift the focus to cleaner sources of energy. The efficiency of any power generation cycle is dependent on the ability of the structural material to withstand increased peak operating temperatures. Advanced austenitic stainless steels have been in the focus as structural material for the next generation nuclear power plants, due to their strength, corrosion resistance, weldability and the wide range of temperatures at which the austenite phase is stable. Alloy 709, a recently developed advanced austenitic stainless steel, is being investigated in this paper. Here in this study, tensile tests were conducted on dog-bone samples of Alloy 709 in an in-situ scanning electron microscope (SEM) loading and heating stage, equipped with electron backscatter diffraction (EBSD), at various temperatures. The in-situ experiments indicated that the material primarily accommodated deformation by slip at lower temperatures. Void formation and coalescence at grain boundaries preceded slip at higher temperatures. Although crack initiation at all elevated temperatures was intergranular, the crack propagation through the material and the final fracture was transgranular ductile. Additionally, tensile tests were conducted on larger cylindrical samples at 550, 650 and 750 °C in air. The results of tests conducted in air and in-situ were found to be in agreement, at these temperatures.

36 MATERIALS SCIENCE↗

Molecular Selectivity of Brown Carbon Chromophores

Complementary methods of high-resolution mass spectrometry and micro-spectroscopy were utilized for molecular analysis of secondary organic aerosol (SOA) generated from ozonolysis of two structural monoterpene isomers: D-limonene (LSOA) and a-pinene (PSOA). Laboratory simulated aging of LSOA and PSOA, through conversion of carbonyls into imines mediated by NH3 vapors in humid air, resulted in selective browning of the LSOA sample, while the PSOA sample remained white. Comparative analysis of the reaction products in the aged LSOA and PSOA samples provided insights into chemistry relevant to formation of brown carbon chromophores. A significant fraction of carbonyl-imine conversion products with identical molecular formulas were detected in both samples. This reflects the high level of similarity in the molecular composition of these two closely related SOA materials. Several highly conjugated products were detected exclusively in the brown LSOA sample and were identified as potential chromophores responsible for the observed color change. The majority of the unique products in the aged LSOA sample with the highest number of double bonds contain two nitrogen atoms. We conclude that chromophores characteristic of the carbonyl- imine chemistry in LSOA are highly conjugated oligomers of secondary imines (Schiff bases) present at relatively low concentrations. Formation of this type of conjugated compounds in PSOA is hindered by the structural rigidity of the a-pinene oxidation products. Our results suggest that the overall light-absorbing properties of SOA may be determined by trace amounts of strong brown carbon chromophores.

Environmental Molecular Sciences Laboratory↗

Probing Terra Incognita of Ni–P Catalysts: Operando Explorations during Hydrogen Evolution Reaction

We have developed two Ni phosphide preparation methods allowing operando XAS surface-sensitive studies of well-defined bulk systems. For Ni K-edge XAS, a Ni 2 P phase-pure powder was sintered into a high-density pellet and polished for grazing incidence XAS. Ni sites were mildly affected by the acidic electrolyte prior to the HER, while the applied cathodic potential caused the reduction of Ni surface states beyond the states of as-prepared Ni 2 P. The computed fully H-covered Ni 2 P [0001] model describes the difference in the operando Ni K-edge GIXAS spectrum well. Upon turning the applied bias off, the Ni sites became immediately oxidized, forming NiO on the surface. Thus, the active phase during the HER is covalent Ni 0 close to that in the intermetallic phosphides, and Ni 2+ oxides formed after, and not during, the HER. For P K-edge XAS, Ni foam was phosphorized to form a thin Ni 3 P layer while preserving its high surface area. Upon immersion in the acidic electrolyte, the P sites underwent removal of P 5+ phosphates and formed new P coordination, possibly due to the adsorption of protons from the electrolyte. These new P surface states were not affected by turning the cathodic current on and off as soon as the sample was immersed in the acidic electrolyte. However, the removal of the sample from the electrochemical cell and drying in air resulted in substantial depletion and oxidation of surface P. Echoing the observed Ni site chemistry during HER, XAS and XPS suggest that the in situ active P sites are different from the oxidized P states observed under ex situ conditions.

Kong, Seongyoung [Iowa State Univ., Ames, IA (Unit↗

Mechanical Properties of Laser Heat Treated 6 mm Thick UHSS-Steel

In this work abrasion resistant (AR) steel with a sheet thickness of 6 mm was heat treated by a 4 kW Nd:YAG and a 4 kW Yb:Yag-laser, followed by self-quenching. In the delivered condition, test material blank (B27S) is water quenched from 920 deg. C. In this condition, fully martensitic microstructure provides excellent hardness of over 500 HB. The test material is referred to AR500 from now onwards. Laser heat treatment was carried out only on top surface of the AR500 sheet: the achieved maximum temperature in the cross-section varies as a function of the depth. Consequently, the microstructure and mechanical properties differ between the surfaces and the centre of the cross-section (layered microstructure). For better understanding, all layers were tested in tensile tests. For a wide heat treatment track, the laser beam was moved by scanning. Temperatures were measured using thermographic camera and thermocouples. Laser heat treated AR500 samples were tested in hardness tests and by air bending using a press brake machine. Microstructures were studied using a light microscope and FE-SEM/SEM-EBSD. At least three kind of microstructure layers were observed: 1) Dual-Phase ferritic/martensitic (T = A{sub C1}-A{sub C3}), 2) ferritic (T{approx}A{sub C3}) and 3) bainitic/martensitic (T>A{sub C3}).

36 MATERIALS SCIENCE↗

Effect of TiO{sub 2} additives to the sintering of Y{sub 2}O{sub 3}

The effect of sintering additive on the microstructure development of yttrium oxide was investigated. Different combinations of yttrium oxide with TiO{sub 2} were used as x-ray diffraction, differential thermal analysis (DTA) were sintering additive. The investigated and microstructure of resulting compacts were characterized by, using scanning electron microscopy, porosity and sintering density for all compacting samples sintered at different sintering temperature under static air.

36 MATERIALS SCIENCE↗

Magnetic studies of CuFe{sub 2}O{sub 4} nanoparticles prepared by co-precipitation method

Cu-ferrite nanoparticles were synthesized by co-precipitation method and were annealed at different temperatures ranging from 400 to l000°C in air for 4 hours. The as-prepared sample and the sample annealed at 400°C showed small peaks of cubic Cu-ferrite in X-ray diffraction studies. For the intermediate temperature 600°C, some additional peaks of α-Fe{sub 2}O{sub 3} were observed. As the annealing temperature increased further only tetragonal Cu-ferrite peaks were observed. In all the samples some traces of CuO was noted. Grain size was increased from 2lnm for the as prepared sample to 42nm for the sample annealed at l000°C. Spontaneous magnetization value was found to be very small for the as prepared sample and it was increased monotonically with the increase in annealing temperature. Maximum magnetization of 29.7emu/g was observed at 300K for the sample annealed at l000°C. The remanent magnetization was increased with the increase in annealing temperature up to 900°C and then decreased whereas for the coercivity a peak was observed for the sample annealed at 800°C. The highest coercivity of l402 Oe was observed at 300K for the sample annealed at 800°C. As the measurement temperature decreased from 300K to 60K, magnetization and coercivity values were increased. The observed magnetic behaviour may be understood on the basis of phase transformation, grain growth with the increase in annealing temperature and reduced thermal energy at low measurement temperature.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

A high bandwidth microelectromechanical system-based nanopositioner for scanning tunneling microscopy

Limited Z-axis bandwidth of piezotube scanners used in conventional Scanning Tunneling Microscopes (STMs) has been a major limiting factor in achieving high scan speeds in STM applications. Slow Z-axis dynamics of typical piezotube scanners combined with the weight of the STM tip/tip holder assembly, that the scanner has to carry, substantially limit the achievable Z-axis bandwidth in both imaging and lithography modes. To tackle this issue, we introduce a high bandwidth microelectromechanical-system-based nanopositioner to be integrated into an existing STM scanner. The device is designed to replace the STM tip and fine Z-positioning mechanisms in the conventional STM setup, while providing an order of magnitude higher bandwidth in Z axis. The device is microfabricated using double silicon-on-isolator technology, and standard cleanroom processes. Experiments show that tunneling current between the device tip and a highly ordered pyrolytic graphite sample can be successfully established and maintained in air using the proposed device in a feedback loop. Results suggest that the proposed device uniquely combines a very high resolution and a large stroke with a substantially larger Z-axis bandwidth compared to that of conventional STM piezotube scanners, enabling higher scanning speeds in STM operations.

42 ENGINEERING↗

Dynamic optical spectroscopy and pyrometry of static targets under optical and x-ray laser heating at the European XFEL

Experiments accessing extreme conditions at x-ray free electron lasers (XFELs) involve rapidly evolving conditions of temperature. Here, we report time-resolved, direct measurements of temperature using spectral streaked optical pyrometry of x-ray and optical laser-heated states at the High Energy Density instrument of the European XFEL. This collection of typical experiments, coupled with numerical models, outlines the reliability, precision, and meaning of time dependent temperature measurements using optical emission at XFEL sources. Dynamic temperatures above 1500 K are measured continuously from spectrally- and temporally-resolved thermal emission at 450–850 nm, with time resolution down to 10–100 ns for 1–200 μs streak camera windows, using single shot and integrated modes. Targets include zero-pressure foils free-standing in air and in vacuo, and high-pressure samples compressed in diamond anvil cell multi-layer targets. Radiation sources used are 20-fs hard x-ray laser pulses at 17.8 keV, in single pulses or 2.26 MHz pulse trains of up to 30 pulses, and 250-ns infrared laser single pulses. A range of further possibilities for optical measurements of visible light in x-ray laser experiments using streak optical spectroscopy are also explored, including for the study of x-ray induced optical fluorescence, which often appears as background in thermal radiation measurements. We establish several scenarios where combined emissions from multiple sources are observed and discuss their interpretation. Challenges posed by using x-ray lasers as non-invasive probes of the sample state are addressed.

47 OTHER INSTRUMENTATION↗

Phylogenetic Molecular Ecological Network of Soil Microbial Communities in Response to Elevated CO 2

Understanding the interactions among different species and their responses to environmental changes, such as elevated atmospheric concentrations of CO 2 , is a central goal in ecology but is poorly understood in microbial ecology. Here we describe a novel random matrix theory (RMT)-based conceptual framework to discern phylogenetic molecular ecological networks using metagenomic sequencing data of 16S rRNA genes from grassland soil microbial communities, which were sampled from a long-term free-air CO 2 enrichment experimental facility at the Cedar Creek Ecosystem Science Reserve in Minnesota. Our experimental results demonstrated that an RMT-based network approach is very useful in delineating phylogenetic molecular ecological networks of microbial communities based on high-throughput metagenomic sequencing data. The structure of the identified networks under ambient and elevated CO 2 levels was substantially different in terms of overall network topology, network composition, node overlap, module preservation, module-based higher-order organization, topological roles of individual nodes, and network hubs, suggesting that the network interactions among different phylogenetic groups/populations were markedly changed. Also, the changes in network structure were significantly correlated with soil carbon and nitrogen contents, indicating the potential importance of network interactions in ecosystem functioning. In addition, based on network topology, microbial populations potentially most important to community structure and ecosystem functioning can be discerned. The novel approach described in this study is important not only for research on biodiversity, microbial ecology, and systems microbiology but also for microbial community studies in human health, global change, and environmental management.

59 BASIC BIOLOGICAL SCIENCES↗

EMP - Environmental Radiological Air Monitoring Plan: PNNL Operations in Washington

The Environmental Radiological Air Monitoring Plan (EMP) for Pacific Northwest National Laboratory (PNNL) describes systems/processes/practices related to radiological operations in Richland and Sequim, Washington, that are associated with environmental radiological air monitoring and surveillance activities. The activities described support the lab’s responsibility to maintain safe operations and minimize negative impacts to both onsite and offsite persons and environment. Dose assessments required by regulations and DOE Orders for the public and biota are described. PNNL conducts environmental air surveillance monitoring as part of the PNNL Site Radioactive Air Emissions License (RAEL)-005 for Richland Campus, issued in 2010 with its most recent renewal effective in January 2021. The radioactive air emissions license for the PNNL-Sequim campus (RAEL-014) was issued to the U.S. Department of Energy in 2012 with its most recent renewal effective in January 2023. The EMP is a compilation of the following four documents: - Environmental Radiological Air Monitoring Plan (this main document) (PNNL-20919) - Sampling and Analysis Plan (Attachment 1) (PNNL-20919-1) - Data Management Plan (Attachment 2) (PNNL-20919-2) - Dose Assessment Guidance (Attachment 3) (PNNL-20919-3).

40 CFR 61 Subpart H↗

HSQC spectra of lignin isolated from poplar stems

Here we present a curated dataset of two-dimensional heteronuclear single quantum coherence (HSQC) nuclear magnetic resonance (NMR) spectra of lignin isolated from stems of genetically engineered poplar through auxin signaling gene modification. The plants were grown in greenhouse with temperatures between 21 and 23 °C. Plants were harvested and the aboveground stems were cut off an approximately five-inch-long segment from the bottom end of the plant stem, debarked and air-dried for three weeks. The dried stem samples were Wiley milled (mesh size 20), Soxhlet-extracted with toluene/ethanol for 24 h to remove extractives. The extracted biomass was ball-milled in a Retsch PM100 planetary ball mill using a porcelain jar with ceramic balls at 600 rpm for 2 h (in 5 min on and 5 min off cycles to avoid excessive sample heating). The ball-milled materials were then subjected to enzymatic hydrolysis for 48 h followed by centrifugation and washing with deionized water. The solid residue was freeze-dried to recover the lignin. The dry stem lignin samples were dissolved in deuterated dimethyl sulfoxide (d6) and transferred into a 5 mm tube. 13C–1H HSQC experiments were performed in a Bruker Avance III HD 500 MHz NMR spectrometer operating at a frequency of 125.12 MHz for the 13C nucleus using a standard Bruker pulse sequence on a Prodigy platform cryoprobe. The NMR spectra were acquired under the following acquisition conditions: 230 ppm spectral width in F1 (13C) dimension with 256 data points and 12 ppm spectral width in F2 (1H) dimension with 2048 data points, a 90° pulse, a one bond C–H coupling constant of 145 Hz, a 1.0 s pulse delay, and 64 scans. Spectra were processed using the Bruker TopSpin 3.6 software. Additional meta data is embedded in the raw spectra figures.

HSQC, lignin, poplar, stems, CBI↗

Radiocarbon in Ecosystem Respiration and Soil Pore-Space CO2 with Surface Gas Flux, Air Temperature, and Soil Temperature and Moisture, Utqiagvik (Barrow), Alaska, 2012-2014

Dataset includes Delta14C measurements made from CO2 that was collected and purified in 2012-2014 from surface soil chambers, soil pore space, and background atmosphere. In addition to 14CO2 data, dataset includes co-located measurements of CO2 and CH4 flux, soil and air temperature, and soil moisture. Measurements and field samples were taken from intensive study site 1 areas A, B, and C, and the site 0 and AB transects, from specified positions in high-centered, flat-centered, and low centered polygons. The column "sample_size" was added to "radiocarbon_field_Barrow_2012_2013_2014.csv" September 2018 with no changes to other data. This dataset contains one pdf and four csv files.The Next-Generation Ecosystem Experiments: Arctic (NGEE Arctic), was a research effort to reduce uncertainty in Earth System Models by developing a predictive understanding of carbon-rich Arctic ecosystems and feedbacks to climate. NGEE Arctic was supported by the Department of Energy's Office of Biological and Environmental Research.The NGEE Arctic project had two field research sites: 1) located within the Arctic polygonal tundra coastal region on the Barrow Environmental Observatory (BEO) and the North Slope near Utqiagvik (Barrow), Alaska and 2) multiple areas on the discontinuous permafrost region of the Seward Peninsula north of Nome, Alaska.Through observations, experiments, and synthesis with existing datasets, NGEE Arctic provided an enhanced knowledge base for multi-scale modeling and contributed to improved process representation at global pan-Arctic scales within the Department of Energy's Earth system Model (the Energy Exascale Earth System Model, or E3SM), and specifically within the E3SM Land Model component (ELM).

54 ENVIRONMENTAL SCIENCES↗