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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 505 records · Page 28
All sourcesNASA NTRSDOE OSTI
DOE OSTI2013

Laser ablation and ionisation by laser plasma radiation in the atmospheric-pressure mass spectrometry of organic compounds

A new method was developed for the mass spectrometric analysis of organic and bioorganic compounds, which involves laser ablation with the ionisation of its products by laser-plasma radiation and enables analysing gaseous, liquid, and solid substances at atmospheric pressure without sample preparation. The capabilities of this method were demonstrated by the examples of fast pharmaceutical composition screening, real-time atmosphere composition analysis, and construction of the mass spectrometric images of organic compound distributions in biological materials. (interaction of laser radiation with matter)

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2015

In vacuo X-ray data collection from graphene-wrapped protein crystals

A method is reported for collecting room-temperature data from protein crystals under vacuum by protecting them with a thin graphene layer. The measurement of diffraction data from macromolecular crystal samples held in vacuo holds the promise of a very low X-ray background and zero absorption of incident and scattered beams, leading to better data and the potential for accessing very long X-ray wavelengths (>3 Å) for native sulfur phasing. Maintaining the hydration of protein crystals under vacuum is achieved by the use of liquid jets, as with serial data collection at free-electron lasers, or is side-stepped by cryocooling the samples, as implemented at new synchrotron beamlines. Graphene has been shown to protect crystals from dehydration by creating an extremely thin layer that is impermeable to any exchanges with the environment. Furthermore, owing to its hydrophobicity, most of the aqueous solution surrounding the crystal is excluded during sample preparation, thus eliminating most of the background caused by liquid. Here, it is shown that high-quality data can be recorded at room temperature from graphene-wrapped protein crystals in a rough vacuum. Furthermore, it was observed that graphene protects crystals exposed to different relative humidities and a chemically harsh environment.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2011

Quantifying Uranium Isotope Ratios Using Resonance Ionization Mass Spectrometry: The Influence of Laser Parameters on Relative Ionization Probability

Resonance Ionization Mass Spectrometry (RIMS) has been developed as a method to measure relative uranium isotope abundances. In this approach, RIMS is used as an element-selective ionization process to provide a distinction between uranium atoms and potential isobars without the aid of chemical purification and separation. We explore the laser parameters critical to the ionization process and their effects on the measured isotope ratio. Specifically, the use of broad bandwidth lasers with automated feedback control of wavelength was applied to the measurement of 235 U/ 238 U ratios to decrease laser-induced isotopic fractionation. By broadening the bandwidth of the first laser in a 3-color, 3-photon ionization process from a bandwidth of 1.8 GHz to about 10 GHz, the variation in sequential relative isotope abundance measurements decreased from >10% to less than 0.5%. This procedure was demonstrated for the direct interrogation of uranium oxide targets with essentially no sample preparation. A rate equation model for predicting the relative ionization probability has been developed to study the effect of variation in laser parameters on the measured isotope ratio. This work demonstrates that RIMS can be used for the robust measurement of uranium isotope ratios.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2016

Synthesis and characterization of α-NaYF{sub 4}: Yb, Er nanoparticles by reverse microemulsion method

A simple and cost effective reverse microemulsion system was newly designed to synthesis NaYF{sub 4}:20%Yb,2%Er upconverting luminescent nanoparticles. XRD results confirms the cubic structure of NaYF{sub 4} nanophosphor in the as prepared condition without any other impurity phases. The as-prepared sample itself having highly crystalline nanoparticle with well dispersed uniform morphology is the advantage of this reverse microemulsion process. HRTEM images of as prepared and calcined samples revealed spherical nanoclusters morphology with size of ~210 nm and ~245 nm respectively. The characteristic absorption wavelength that occurs at 980 nm due to transition of energy levels {sup 2}F{sub 5/2} to {sup 2}F{sub 7/2} for Yb{sup 3+} rare earth ion in as prepared and calcined upconversion nanoparticle confirms the presence of Yb{sup 3+} by UV-Visible spectroscopy which can act as a sensitizer for photonic upconversion. Therefore the absorption at NIR region and emission spectrum at visible region suggests that NaYF{sub 4}:20%Yb,2%Er is suitable for upcoversion process, due to its optical property and chemical stability this material also be useful for bio imaging applications.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2015

The ReactorAFM: Non-contact atomic force microscope operating under high-pressure and high-temperature catalytic conditions

An Atomic Force Microscope (AFM) has been integrated in a miniature high-pressure flow reactor for in-situ observations of heterogeneous catalytic reactions under conditions similar to those of industrial processes. The AFM can image model catalysts such as those consisting of metal nanoparticles on flat oxide supports in a gas atmosphere up to 6 bar and at a temperature up to 600 K, while the catalytic activity can be measured using mass spectrometry. The high-pressure reactor is placed inside an Ultrahigh Vacuum (UHV) system to supplement it with standard UHV sample preparation and characterization techniques. To demonstrate that this instrument successfully bridges both the pressure gap and the materials gap, images have been recorded of supported palladium nanoparticles catalyzing the oxidation of carbon monoxide under high-pressure, high-temperature conditions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2017

Imaging the presence of silane coatings in concrete with micro X-ray fluorescence

Silane is a commonly used surface treatment to reduce fluid entry into the concrete matrix. This work uses micro X-ray fluorescence (μXRF) to image the presence of silane coatings in field samples and the changes made to the paste chemistry. There are many advantages that μXRF has over other imaging techniques due to the large spot size and the high energy levels. Because of this, μXRF can rapidly investigate large areas and requires minimal sample preparation. Quantitative measurements are made to show that there is a reduction in the amount of sulfur and an increase in potassium in the hydrophobic regions formed by silane coatings. These measurements provide important insights into modifications made to the concrete matrix when silane sealers are used. The mechanisms for the observed chemistry changes are discussed and a simple field or laboratory test method is presented that uses a dye to detect silane coatings.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Characterisation of metals in the electronic waste of complex mixtures of end-of-life ICT products for development of cleaner recovery technology

Highlights: • New characterisation methodology has been established to understand an industrially processed ICT waste. • Particle size distribution, composition, thermal–chemical behaviour and occurrence of metals were considered. • The characterisation provides direct guidelines for values recovery from the waste. - Abstract: Recycling of valuable metals from electronic waste, especially complex mixtures of end-of-life information and communication technology (ICT) products, is of great difficulty due to their complexity and heterogeneity. One of the important reasons is the lack of comprehensive characterisation on such materials, i.e. accurate compositions, physical/chemical properties. In the present research, we focus on developing methodologies for the characterisation of metals in an industrially processed ICT waste. The morphology, particle size distribution, compositional distribution, occurrence, liberation as well as the thermo-chemical properties of the ICT waste were investigated with various characterisation techniques, including X-ray Fluorescence Spectrometry (XRF), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM) with energy dispersed spectroscopy (EDS). Due to the high heterogeneity of the material, special sample preparation procedures were introduced to minimise the discrepancies during compositional analyses. As a result, a clearer overview of the ICT waste has been reached. This research provides better understanding of the extractability of each metal and improves the awareness of potential obstacles for extraction. It will lead to smarter decisions during further development of a clean and effective recovery process.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2015

Suppression of spin pumping between Ni{sub 80}Fe{sub 20} and Cu by a graphene interlayer

We compare ferromagnetic resonance measurements of Permalloy Ni{sub 80}Fe{sub 20} (Py) films sputtered onto Cu(111) films with and without a graphene (Gr) interlayer grown by chemical vapor deposition before Py deposition. A two-angle sputtering method ensured that neither Gr nor Py was degraded by the sample preparation process. We find the expected damping enhancement from spin pumping for the Py/Cu case and no detectable enhancement for the Py/Gr/Cu case. Since damping is sensitive to effects other than spin pumping, we used magnetometry to verify that differences in Py magnetostatic properties are not responsible for the difference in damping. We attribute the suppression of spin pumping in Py/Gr/Cu to the large contact resistance of the Gr/Cu interface.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2013

Iodine doping effects on the lattice thermal conductivity of oxidized polyacetylene nanofibers

Thermal transport in oxidized polyacetylene (PA) nanofibers with diameters in the range between 74 and 126 nm is measured with the use of a suspended micro heater device. With the error due to both radiation and contact thermal resistance corrected via a differential measurement procedure, the obtained thermal conductivity of oxidized PA nanofibers varies in the range between 0.84 and 1.24 W m{sup −1} K{sup −1} near room temperature, and decreases by 40%–70% after iodine doping. It is also found that the thermal conductivity of oxidized PA nanofibers increases with temperature between 100 and 350 K. Because of exposure to oxygen during sample preparation, the PA nanofibers are oxidized to be electrically insulating before and after iodine doping. The measurement results reveal that iodine doping can result in enhanced lattice disorder and reduced lattice thermal conductivity of PA nanofibers. If the oxidation issue can be addressed via further research to increase the electrical conductivity via doping, the observed suppressed lattice thermal conductivity in doped polymer nanofibers can be useful for the development of such conducting polymer nanostructures for thermoelectric energy conversion.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Characterization of encapsulated quantum dots via electron channeling contrast imaging

A method for characterization of encapsulated epitaxial quantum dots (QD) in plan-view geometry using electron channeling contrast imaging (ECCI) is presented. The efficacy of the method, which requires minimal sample preparation, is demonstrated with proof-of-concept data from encapsulated (sub-surface) epitaxial InAs QDs within a GaAs matrix. Imaging of the QDs under multiple diffraction conditions is presented, establishing that ECCI can provide effectively identical visualization capabilities as conventional two-beam transmission electron microscopy. This method facilitates rapid, non-destructive characterization of sub-surface QDs giving immediate access to valuable nanostructural information.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2015

The effect of an excess of components on the electrical properties of indium-antimonide films

The causes of anomalous behavior of the Hall mobility of charge carriers as a result of a decrease in the measurement temperature from 300 K in indium-antimonide films obtained by the method of three temperatures are studied. It is shown experimentally that there exist drops in the “admissible” temperatures of evaporators of components and the substrate within which continuous conducting films are obtained. The optimal conditions for sample preparation for which the values of the mobility remain practically constant in the temperature range of 150–350 K are determined. On the basis of the comparison with optical-transmission spectra, it is concluded that there is a high concentration of defects in the films; these defects are related to deviation of the composition from stoichiometry and act as donor and acceptor centers. The presence of such defects makes it possible to explain the decrease in mobility in the films as the temperature is lowered.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Development and testing of a prototype modular tritium and carbon-14 gas environmental monitoring system

Increasing quantities of radioactive waste are being placed into storage facilities. Many of the waste products contain organic materials which may undergo degradation leading to the release of tritium and carbon-14 species into waste containers and potentially into the environment. Monitoring for radioactive gas releases are required for environmental regulatory compliance and for radiation protection of facility workers. Research is currently being undertaken at the National Physical Laboratory (NPL) as part of a European Metrology Research Programme (EMRP) project MetroRWM to adapt and automate existing environmental sampling techniques for tritium and carbon-14 species. An innovative modular system is being developed which will lead to the introduction of an on-site small scale system capable of gas collection, liquid scintillation sample preparation and measurement. This paper outlines the evaluation of a liquid scintillation system that has been performed to date using active solutions of spiked trapping medium of similar activity concentrations to those anticipated in a waste repository. This system will operate using pre-set conditions for quench and luminescence derived from these and subsequent trials, unlike most other counters for which corrections for these phenomena are applied post measurement. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2015

Specific features of the optical and photoelectric properties of nanocrystalline indium oxide

The spectral dependences of the absorption coefficient and steady-state photoconductivity and the relaxation of photoconductivity (after illumination switch off) in nanocrystalline indium oxide (In{sub 2}O{sub 3}) films synthesized by the sol–gel method are investigated. The mean nanocrystal size varies from 7–8 to 39–41 nm, depending on the sample-preparation conditions. The optical band gap of nanocrystalline In{sub 2}O{sub 3} is determined as a result of combined analysis of the optical absorption spectra and the spectral dependence of the photoconductivity. The optical band gap in nanocrystalline In{sub 2}O{sub 3} is found to be much narrower than the optical band gap in In{sub 2}O{sub 3} single crystals. The photoconductivity decay kinetics in nanocrystalline In{sub 2}O{sub 3} in air, vacuum, and argon at room temperature are studied. A model explaining the observed photoconductivity decay is proposed.

36 MATERIALS SCIENCE↗
DOE OSTI2011

I-NERI-2007-004-K, Development and Characterization of New High-Level Waste Forms for Achieving Waste Minimization from Pyroprocessing

Work describe in this report represents the final year activities for the 3-year International Nuclear Energy Research Initiative (I-NERI) project: Development and Characterization of New High-Level Waste Forms for Achieving Waste Minimization from Pyroprocessing. Used electrorefiner salt that contained actinide chlorides and was highly loaded with surrogate fission products was processed into three candidate waste forms. The first waste form, a high-loaded ceramic waste form is a variant to the CWF produced during the treatment of Experimental Breeder Reactor-II used fuel at the Idaho National Laboratory (INL). The two other waste forms were developed by researchers at the Korean Atomic Energy Research Institute (KAERI). These materials are based on a silica-alumina-phosphate matrix and a zinc/titanium oxide matrix. The proposed waste forms, and the processes to fabricate them, were designed to immobilize spent electrorefiner chloride salts containing alkali, alkaline earth, lanthanide, and halide fission products that accumulate in the salt during the processing of used nuclear fuel. This aspect of the I-NERI project was to demonstrate 'hot cell' fabrication and characterization of the proposed waste forms. The outline of the report includes the processing of the spent electrorefiner salt and the fabrication of each of the three waste forms. Also described is the characterization of the waste forms, and chemical durability testing of the material. While waste form fabrication and sample preparation for characterization must be accomplished in a radiological hot cell facility due to hazardous radioactivity levels, smaller quantities of each waste form were removed from the hot cell to perform various analyses. Characterization included density measurement, elemental analysis, x-ray diffraction, scanning electron microscopy and the Product Consistency Test, which is a leaching method to measure chemical durability. Favorable results from this demonstration project will provide additional options for fission product immobilization and waste management associated the electrochemical/pyrometallurgical processing of used nuclear fuel.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2014

The ReactorSTM: Atomically resolved scanning tunneling microscopy under high-pressure, high-temperature catalytic reaction conditions

To enable atomic-scale observations of model catalysts under conditions approaching those used by the chemical industry, we have developed a second generation, high-pressure, high-temperature scanning tunneling microscope (STM): the ReactorSTM. It consists of a compact STM scanner, of which the tip extends into a 0.5 ml reactor flow-cell, that is housed in a ultra-high vacuum (UHV) system. The STM can be operated from UHV to 6 bars and from room temperature up to 600 K. A gas mixing and analysis system optimized for fast response times allows us to directly correlate the surface structure observed by STM with reactivity measurements from a mass spectrometer. The in situ STM experiments can be combined with ex situ UHV sample preparation and analysis techniques, including ion bombardment, thin film deposition, low-energy electron diffraction and x-ray photoelectron spectroscopy. The performance of the instrument is demonstrated by atomically resolved images of Au(111) and atom-row resolution on Pt(110), both under high-pressure and high-temperature conditions.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2020

Multivariate Linear Models for In Situ Monitoring of Low-Activity Nuclear Waste Using Infrared and Raman Spectroscopy - 20218

This paper presents the use of in situ monitoring tools for molecular analysis of non-radioactive species found in the supernatant liquid and dissolvable salt cake of nuclear waste at Hanford. We have selected two in situ spectroscopic techniques that do not require any sample preparation or consumables: infrared (in the form of attenuated total reflectance Fourier transform infrared or ATR-FTIR) and Raman spectroscopy. This work aims to evaluate their performance for liquid waste simulants representative of the Hanford DFLAW (Direct Feed Low-Activity Waste) feed. In addition, we have evaluated the performance of four multivariate linear models that extract concentrations from spectral measurements for a data set that was designed to include key molecular species found in liquid low-activity waste. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2013

An in-cell NMR study of monitoring stress-induced increase of cytosolic Ca{sup 2+} concentration in HeLa cells

Highlights: •We performed time-resolved NMR observations of calbindin D{sub 9k} in HeLa cells. •Stress-induced increase of cytosolic Ca{sup 2+} concentration was observed by in-cell NMR. •Calbindin D{sub 9k} showed the state-transition from Mg{sup 2+}- to Ca{sup 2+}-bound state in cells. •We provide a useful tool for in situ monitoring of the healthiness of the cells. -- Abstract: Recent developments in in-cell NMR techniques have allowed us to study proteins in detail inside living eukaryotic cells. The lifetime of in-cell NMR samples is however much shorter than that in culture media, presumably because of various stresses as well as the nutrient depletion in the anaerobic environment within the NMR tube. It is well known that Ca{sup 2+}-bursts occur in HeLa cells under various stresses, hence the cytosolic Ca{sup 2+} concentration can be regarded as a good indicator of the healthiness of cells in NMR tubes. In this study, aiming at monitoring the states of proteins resulting from the change of cytosolic Ca{sup 2+} concentration during experiments, human calbindin D{sub 9k} (P47M + C80) was used as the model protein and cultured HeLa cells as host cells. Time-resolved measurements of 2D {sup 1}H–{sup 15}N SOFAST–HMQC experiments of calbindin D{sub 9k} (P47M + C80) in HeLa cells showed time-dependent changes in the cross-peak patterns in the spectra. Comparison with in vitro assignments revealed that calbindin D{sub 9k} (P47M + C80) is initially in the Mg{sup 2+}-bound state, and then gradually converted to the Ca{sup 2+}-bound state. This conversion process initiates after NMR sample preparation. These results showed, for the first time, that cells inside the NMR tube were stressed, presumably because of cell precipitation, the lack of oxygen and nutrients, etc., thereby releasing Ca{sup 2+} into cytosol during the measurements. The results demonstrated that in-cell NMR can monitor the state transitions of stimulated cells through the observation of proteins involved in the intracellular signalling systems. Our method provides a very useful tool for in situ monitoring of the “healthiness” of the cells in various in-cell NMR studies.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2016

Process dependent thermoelectric properties of EDTA assisted bismuth telluride

Comparison between the structure and thermoelectric properties of EDTA (Ethylene-diamine-tetra-acetic acid) assisted bismuth telluride prepared by electrochemical deposition and hydrothermal route is reported in the present work. The prepared samples have been structurally characterized by high resolution X-ray diffraction spectra (HRXRD), field emission scanning electron microscopy (FESEM) and high resolution transmission electron microscopic images (HRTEM). Crystallite size and strain have been determined from Williamson-Hall plot of XRD which is in conformity with TEM images. Measurement of transport properties show sample in the pellet form (S{sub 1}) prepared via hydrothermal route has higher value of thermoelectric power (S) than the electrodeposited film (S{sub 2}). But due to a substantial increase in the electrical conductivity (σ) of the film (S{sub 2}) over the pellet (S{sub 1}), the power factor and the figure of merit is higher for sample S{sub 2} than the sample S{sub 1} at room temperature.

36 MATERIALS SCIENCE↗