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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 145 records · Page 8
All sourcesNASA NTRSDOE OSTI
DOE OSTI2016

Comparative study of GeO{sub 2}/Ge and SiO{sub 2}/Si structures on anomalous charging of oxide films upon water adsorption revealed by ambient-pressure X-ray photoelectron spectroscopy

The energy difference between the oxide and bulk peaks in X-ray photoelectron spectroscopy (XPS) spectra was investigated for both GeO{sub 2}/Ge and SiO{sub 2}/Si structures with thickness-controlled water films. This was achieved by obtaining XPS spectra at various values of relative humidity (RH) of up to ∼15%. The increase in the energy shift is more significant for thermal GeO{sub 2} on Ge than for thermal SiO{sub 2} on Si above ∼10{sup −4}% RH, which is due to the larger amount of water molecules that infiltrate into the GeO{sub 2} film to form hydroxyls. Analyzing the origins of this energy shift, we propose that the positive charging of a partially hydroxylated GeO{sub 2} film, which is unrelated to X-ray irradiation, causes the larger energy shift for GeO{sub 2}/Ge than for SiO{sub 2}/Si. A possible microscopic mechanism of this intrinsic positive charging is the emission of electrons from adsorbed water species in the suboxide layer of the GeO{sub 2} film to the Ge bulk, leaving immobile cations or positively charged states in the oxide. This may be related to the reported negative shift of flat band voltages in metal-oxide-semiconductor diodes with an air-exposed GeO{sub 2} layer.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2017

Electronic structure of ferromagnetic heavy fermion, YbPdSi, YbPdGe, and YbPtGe studied by photoelectron spectroscopy, x-ray emission spectroscopy, and DFT + DMFT calculations

Here, the electronic structures of ferromagnetic heavy fermion Yb compounds of YbPdSi, YbPdGe, and YbPtGe are studied by photoelectron spectroscopy around the Yb 4d–4f resonance, resonant x-ray emission spectroscopy at the Yb L 3 absorption edge, and density functional theory combined with dynamical mean field theory calculations. These compounds all have a temperature-independent intermediate Yb valence with large ${\rm Yb}^{3+}$ and small ${\rm Yb}^{2+}$ components. The magnitude of the Yb valence is evaluated to be YbPtGe $<$ YbPdGe $\lesssim $ YbPdSi, suggesting that YbPtGe is the closest to the quantum critical point among the three Yb compounds. Our results support the scenario of the coexistence of heavy fermion behavior and ferromagnetic ordering which is described by a magnetically-ordered Kondo lattice where the magnitude of the Kondo effect and the RKKY interaction are comparable.

30 DIRECT ENERGY CONVERSION↗
DOE OSTI2020

Defect Study of Group V Doped CdTe By Thermoelectric Effect Spectroscopy

Shallow acceptors in single crystal CdTe induced by Group V (P, As, and Sb) doping are identified by thermoelectric effect spectroscopy (TEES). Understanding defects in Group V doped CdTe is critical to improving and controlling the acceptor density and lifetime in the absorber material which is an important factor determining the open circuit voltage and efficiency in CdTe solar cells.

14 SOLAR ENERGY↗
DOE OSTI2016

A Method to Estimate the Atomic Number and Mass Thickness of Intervening Materials in Uranium and Plutonium Gamma-Ray Spectroscopy Measurements

To accurately characterize shielded special nuclear materials (SNM) using passive gamma-ray spectroscopy measurement techniques, the effective atomic number and the thickness of shielding materials must be measured. Intervening materials between the source and detector may affect the estimated source isotopics (uranium enrichment and plutonium grade) for techniques which rely on raw count rates or photopeak ratios of gamma-ray lines separated in energy. Furthermore, knowledge of the surrounding materials can provide insight regarding the configuration of a device containing SNM. The described method was developed using spectra recorded using high energy resolution CdZnTe detectors, but can be expanded to any gamma-ray spectrometers with energy resolution of better than 1% FWHM at 662 keV. The effective atomic number, Z, and mass thickness of the intervening shielding material are identified by comparing the relative attenuation of different gamma-ray lines and estimating the proportion of Compton scattering interactions to photoelectric absorptions within the shield. While characteristic Kα x-rays can be used to identify shielding materials made of high Z elements, this method can be applied to all shielding materials. This algorithm has adequately estimated the effective atomic number for shields made of iron, aluminum, and polyethylene surrounding uranium samples using experimental data. The mass thicknesses of shielding materials have been estimated with a standard error of less than 1.3 g/cm2 for iron shields up to 2.5 cm thick. The effective atomic number was accurately estimated to 26 ± 5 for all iron thicknesses.

CdZnTe detectors, gamma-ray imaging, gamma-ray spe↗
DOE OSTI2025

Neutron powder diffraction, Mossbauer Spectroscopy and Optical Spectroscopy to study magnetic and nuclear lattices in Fe-based oxychlorides Ca2FeO3Cl, Sr2FeO3Cl and Sr3Fe2O5Cl2

Data for Neutron Diffraction, Mossbauer Spectoscopy and Optical Spectroscopy are contained on all three samples (Ca2FeO3Cl, Sr2FeO3Cl, and Sr3Fe2O5Cl2). Mossbauer data are in the folder "MossbauerSpectroscopy". This contains details of files and examples to read the data. The Optical Spectroscopy are in the folder "AbsorptionData", this contains one file with explanatory headers. The neutron diffraction data are in the "NeutronDiffractionData" folder. The data was collected on the HB-2A powder diffractometer at HFIR. The autoreduced files are corrected using a vanadium standard and are in arbitrary intensity units. The RawData folder contains the uncorrected data with metadata for motor positions and temperature. All measurements were collected with a constant neuton wavelength of 2.41 Angstrom. An excel spreadsheet "NeutronDiffractionData_IPTS-29118_summary" contains details for each scan. Sr3Fe2O5Cl2 data were collected at only room temperature. Ca2FeO3Cl and Sr2FeO3Cl data were collected at 4K and room temperature. The autoreduced .dat fileformat is three columns corresponding to: Two-theta, Intensity and Intensity_error.

fe-based oxychlorides↗
DOE OSTI2018

Microbeam X-Ray Absorption Near-Edge Spectroscopy of Alloying Elements in the Oxide Layers of Irradiated Zircaloy-2

Hydrogen pickup of zirconium-based fuel cladding and structural materials during in-reactor corrosion can degrade fuel components because the ingress of hydrogen can lead to the formation of brittle hydrides. In the boiling water reactor (BWR) environment, Zircaloy-2 fuel cladding and structural components such as water rods and channels can experience accelerated hydrogen pickup, whereas Zircaloy-4 components exposed to similar conditions do not. Because the principal difference between the two alloys is that Zircaloy-2 contains nickel, accelerated hydrogen pickup has been hypothesized to result from the presence of nickel. However, an understanding of the mechanism by which this acceleration occurs is still lacking. We investigated the link between hydrogen pickup and the oxidation behavior of alloying elements when incorporated into the oxide layers formed on zirconium alloys when corroded in the reactor. Synchrotron radiation microbeam X-ray absorption near-edge spectroscopy (XANES) at the Advanced Photon Source was performed on carefully selected BWR-corroded Zircaloy-2 water rods at an assembly-averaged burnup ranging from 32.8 to 74.6 GWd/MTU to determine the oxidation states of alloying elements, such as iron and nickel, within the oxide layers as a function of distance from the oxide-metal interface at high burnup. Samples were chosen for comparison based on having similar oxide thicknesses, processing, elevation, reactors, and fluences but different hydrogen pickup fractions. Examinations of the oxide layers formed on these samples showed that (1) the oxidation states of these alloying elements changed with distance from the oxide-metal interface, (2) these elements exhibited delayed oxidation relative to the host zirconium, and (3) nickel in Zircaloy-2 remained metallic in the oxide layer at a longer distance from the oxide-metal interface than iron. An analysis of these results showed an apparent correlation between the delayed oxidation of nickel and higher hydrogen pickup of Zircaloy-2 at high burnup.

alloying elements↗
DOE OSTI2018

Detecting Fermi-level shifts by Auger electron spectroscopy in Si and GaAs

In this paper, changes in surface Fermi-level of Si and GaAs, caused by doping and cleaning, are investigated by Auger electron spectroscopy. Based on the Auger voltage contrast, we compared the Auger transition peak energy but with higher accuracy by using a more accurate detector and an improved peak position determination method. For silicon, a peak shift as large as 0.46 eV was detected when comparing a cleaned p-type and n-type wafer, which corresponds rather well with the theoretical difference in Fermi-level. If no cleaning was applied, the peak position did not differ significantly for both wafer types, indicating Fermi-level pinning in the band gap. For GaAs, peak shifts were detected after cleaning with HF and (NH4)2S-solutions in an inert atmosphere (N2-gas). Although the (NH4)2S-cleaning in N2 is very efficient in removing the oxygen from the surface, the observed Ga- and As-peak shifts are smaller than those obtained after the HF-cleaning. It is shown that the magnitude of the shift is related to the surface composition. After Si-deposition on the (NH4)2S-cleaned surface, the Fermi-level shifts back to a similar position as observed for an as-received wafer, indicating that this combination is not successful in unpinning the Fermi-level of GaAs. This work has been funded by J.D.'s PhD fellowship of the Fund of Scientific Research-Flanders (FWO-V) (Dossier No. 11U4516N). P.H. acknowledges support from Becas Chile-CONICYT. This research was also supported by the FWO Odysseus Program, the Belgian Hercules Stichting with the Project No. Her/08/25 and AKUL/13/19 and the KU Leuven project GOA "Fundamental challenges in Semiconductor Research". The authors would also like to thank Bastiaan Opperdoes and Ludwig Henderix for technical support. The work was supported by the U.S. Department of Energy (USDOE), Office of Science, Office of Basic Energy Sciences, Division of Materials Sciences and Engineering, and performed in the Environmental Molecular Sciences Laboratory, a national scientific user facility sponsored by the Department of Energy's Office of Biological and Environmental Research and located at Pacific Northwest National Laboratory (PNNL). Battelle operates PNNL for the USDOE under contract DE-AC05-76RL01830.

Environmental Molecular Sciences Laboratory↗
DOE OSTI2019

Unraveling the Mechanism of Water-Mediated Sulfur Tolerance via Operando Surface-Enhanced Raman Spectroscopy

While several proton-conducting anode materials have shown excellent tolerance to sulfur poisoning, the mechanism is still unclear due largely to the inability to probe miniscule amounts of sulfur-containing species using conventional surface characterization techniques. Here we present our findings in unraveling the mechanism of water-mediated sulfur tolerance of a proton conductor under operating conditions empowered by surface-sensitive, operando surface-enhanced Raman spectroscopy (SERS) coupled with impedance spectroscopy. Contrary to the conventional view that surface-adsorbed sulfur is removed mainly by oxygen anions, it is found that –SO 4 groups on the surface of the proton conductor are converted to SO 2 by a water-mediated process, as confirmed by operando SERS analysis and density functional theory (DFT)-based calculations. Furthermore, the combination of operando SERS performed on a model electrode and theoretical computation offers an effective approach to investigate into complex mechanisms of electrode processes in various electrochemical systems, providing information vital to achieve the rational design of better electrode materials.

25 ENERGY STORAGE↗
DOE OSTI2014

Electronic structure of cobalt doped CdSe quantum dots using soft X-ray spectroscopy

Here, the electronic structure and magnetic properties of cobalt doped CdSe quantum dots (QDs) are studied using electron microscopy, soft X-ray spectroscopy, and magnetometry. Magnetometry measurements suggest these QDs are superparamagnetic, contrary to a spin-glass state observed in the bulk analogue. Electron microscopy shows well formed QDs, but with cobalt existing as doped into the QD and as unreacted species not contained in the QD. X-ray absorption measurements at the Co L3-edge suggest that changes in spectra features as a function of particle size can be described considering combination of a cobalt ion in a tetrahedral crystal field and an octahedrally coordinated (impurity) phase. With decreasing particle sizes, the impurity phase increases, suggesting that small QDs can be difficult to dope.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Probing Battery Chemistry with Liquid Cell Electron Energy Loss Spectroscopy

We demonstrate the ability to apply electron energy loss spectroscopy (EELS) to follow the chemistry and oxidation states of LiMn 2 O 4 and Li 4 Ti 5 O1 2 battery electrodes within a battery solvent. The use and importance of in situ electrochemical cells coupled with a scanning/transmission electron microscope (S/TEM) has expanded and been applied to follow changes in battery chemistry during electrochemical cycling. Furthermore, we discuss experimental parameters that influence measurement sensitivity and provide a framework to apply this important analytical method to future in situ electrochemical studies.

25 ENERGY STORAGE↗
DOE OSTI2016

Structure-dependent vibrational dynamics of Mg(BH 4 ) 2 polymorphs probed with neutron vibrational spectroscopy and first-principles calculations

We investigated the structure-dependent vibrational properties of different Mg(BH 4 ) 2 polymorphs (α, β, γ, and δ phases) with a combination of neutron vibrational spectroscopy (NVS) measurements and density functional theory (DFT) calculations, with emphasis placed on the effects of the local structure and orientation of the BH 4 - anions. DFT simulations closely match the neutron vibrational spectra. The main bands in the low-energy region (20–80 meV) are associated with the BH4 - librational modes. The features in the intermediate energy region (80–120 meV) are attributed to overtones and combination bands arising from the lower-energy modes. The features in the high-energy region (120–200 meV) correspond to the BH 4 - symmetric and asymmetric bending vibrations, of which four peaks located at 140, 142, 160, and 172 meV are especially intense. There are noticeable intensity distribution variations in the vibrational bands for different polymorphs. We can explain these differences using the spatial distribution of BH 4 - anions within various structures. An example of the possible identification of products after the hydrogenation of MgB 2 , using NVS measurements, is presented. Our results provide fundamental insights of benefit to researchers currently studying these promising hydrogen-storage materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2011

An instrument for the investigation of actinides with spin resolved photoelectron spectroscopy and bremsstrahlung isochromat spectroscopy

A new system for spin resolved photoelectron spectroscopy and bremsstrahlung isochromat spectroscopy has been built and commissioned at Lawrence Livermore National Laboratory for the investigation of the electronic structure of the actinides. Actinide materials are very toxic and radioactive and therefore cannot be brought to most general user facilities for spectroscopic studies. The technical details of the new system and preliminary data obtained therein will be presented and discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Improving metastable impact electron spectroscopy and ultraviolet photoelectron spectroscopy signals by means of a modified time-of-flight separation

The separation of ultraviolet photoelectron spectroscopy (UPS) and metastable impact electron spectroscopy (MIES) is usually performed by a time-of-flight (ToF) separation using pre-set ToF for both types of signal. In this work, we present a new, improved ex situ signal separation method for the separation of MIES and UPS for every single measurement. Signal separation issues due to changes of system parameters can be overcome by changing the ToF separation and therefore allowing for the application of a wider range of measuring conditions. The method also enables to identify and achieve separation of the two signals without any time consuming calibration and the use of any special material for the calibration. Furthermore, changes made to the discharge source are described that enable to operate an existing MIES/UPS source over a broader range of conditions. This allows for tuning of the yield of UV photons and metastable rare gas atoms leading to an improved signal to noise ratio. First results of this improved setup are well in agreement with spectra reported in literature and show increased resolution and higher signal intensities for both MIE and UP spectra compared to the previous, non-optimized setup.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2012

A portable optical emission spectroscopy-cavity ringdown spectroscopy dual-mode plasma spectrometer for measurements of environmentally important trace heavy metals: Initial test with elemental Hg

A portable optical emission spectroscopy-cavity ringdown spectroscopy (OES-CRDS) dual-mode plasma spectrometer is described. A compact, low-power, atmospheric argon microwave plasma torch (MPT) is utilized as the emission source when the spectrometer is operating in the OES mode. The same MPT serves as the atomization source for ringdown measurements in the CRDS mode. Initial demonstration of the instrument is carried out by observing OES of multiple elements including mercury (Hg) in the OES mode and by measuring absolute concentrations of Hg in the metastable state 6s6p {sup 3}P{sub 0} in the CRDS mode, in which a palm-size diode laser operating at a single wavelength 405 nm is incorporated in the spectrometer as the light source. In the OES mode, the detection limit for Hg is determined to be 44 parts per 10{sup 9} (ppb). A strong radiation trapping effect on emission measurements of Hg at 254 nm is observed when the Hg solution concentration is higher than 50 parts per 10{sup 6} (ppm). The radiation trapping effect suggests that two different transition lines of Hg at 253.65 nm and 365.01 nm be selected for emission measurements in lower (<50 ppm) and higher concentration ranges (>50 ppm), respectively. In the CRDS mode, the detection limit of Hg in the metastable state 6s6p {sup 3}P{sub 0} is achieved to be 2.24 parts per 10{sup 12} (ppt) when the plasma is operating at 150 W with sample gas flow rate of 480 mL min{sup -1}; the detection limit corresponds to 50 ppm in Hg sample solution. Advantage of this novel spectrometer has two-fold, it has a large measurement dynamic range, from a few ppt to hundreds ppm and the CRDS mode can serve as calibration for the OES mode as well as high sensitivity measurements. Measurements of seven other elements, As, Cd, Mn, Ni, P, Pb, and Sr, using the OES mode are also carried out with detection limits of 1100, 33, 30, 144, 576, 94, and 2 ppb, respectively. Matrix effect in the presence of other elements on Hg measurements has been found to increase the detection limit to 131 ppb. These elements in lower concentrations can also be measured in the CRDS mode when a compact laser source is available to be integrated into the spectrometer in the future. This exploratory study demonstrates a new instrument platform using an OES-CRDS dual-mode technique for potential field applications.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗