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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 613 records · Page 34
All sourcesNASA NTRSDOE OSTI
NASA NTRS1998

Solid Lubrication Fundamentals and Applications

This chapter describes powerful analytical techniques capable of sampling tribological surfaces and solid-film lubricants. Some of these techniques may also be used to determine the locus of failure in a bonded structure or coated substrate; such information is important when seeking improved adhesion between a solid-film lubricant and a substrate and when seeking improved performance and long life expectancy of solid lubricants. Many examples are given here and through-out the book on the nature and character of solid surfaces and their significance in lubrication, friction, and wear. The analytical techniques used include the late spectroscopic methods.

Miyoshi, Kazuhisa↗
NASA NTRS2002

Monitoring Photodeposition of Polymer Films from Diacetylene Monomer Solutions Using In Situ Real-Time Spectroscopic Ellipsometry

Photodeposition of thin polymer (PDAMNA) films from diacetylene monomer (DAMNA) solutions onto gold coated silica substrates with UV light was studied using the technique of in-situ real time spectroscopic ellipsometry. The dielectric function of PDAMNA was determined; and the thickness of the growing PDAMNA films over a 4 hour time interval was determined using a linear regression fit of the experimental data to a homogeneous four phase optical model. It was found that stirring the solution dramatically lowers the rate of film deposition, suggesting that convection can affect the attachment kinetics of the film to the substrate. Lastly, the morphology of the PDAMNA films was examined using non-contact mode atomic force microscopy.

Hui, Du↗
DOE OSTI2023

Exploring the speciation of actinide salts in the presence of contaminants related to molten salt reactors

Molten salt reactors (MSR) are up-and-coming Generation IV nuclear reactors with either coolant and/or radioactive fuel in molten salt form. Due to their improved safety, efficiency, affordability and convenient waste processing system, these reactors are considered a superior alternative to conventional ones. However, prior to commercial implementation, it is necessary to have an extensive understanding of the reactions occurring in the MSR. The safety parameters of the MSR are determined by the rheological properties such as density and viscosity of the molten salt and these properties are governed by the local structure of the molten salts. Due to the high operational temperatures of MSR's, corrosion plays an important role. Because of their influence, the container corrosion products become part of the fuel salt matrix. In this work, we are investigating how these corrosion products, e.g., Mo, Ni, Cr, would impact the speciation of the actinide metal centers. For the initial studies, lanthanides are used as a surrogate for actinides. Lanthanide chloride salts (LnCl3) are mixed with transition metals and excess of alkali or alkali earth metal salts or salt mixtures (LiCl, NaCl, KCl). These are added to an alumina crucible, placed in a quartz tube, and sealed under a vacuum. This is heated up to around 1000 °C and slowly cooled to a temperature above the melting point of the salt and at that temperature, the reaction is taken out of the furnace. The excess salt is removed, and the resulting product is analyzed using X-ray diffraction techniques, scanning electron microscopy, and spectroscopic methods such as Raman, UV-Visible, and FTIR spectroscopy.

37 - INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL C↗
NASA NTRS1990

Monitoring of catalyst performance in CO2 lasers using frequency modulation spectroscopy with diode lasers

Closed-cycle CO2 laser operation with removal of O2 and regeneration of CO2 can be achieved by catalytic CO-O2 recombination. Both parametric studies of the optimum catalyst formulation and long-term performance tests require on line monitoring of CO, O2 and CO2 concentrations. There are several existing methods for molecular oxygen detection. These methods are either intrusive (such as electrochemical method or mass spectrometry) or very expensive (such as CARS, UV laser absorption). Researchers demonstrated a high-sensitivity spectroscopic measurement of O2 using the two-tone frequency modulation spectroscopy (FMS) technique with a near infrared GaAlAs diode laser. Besides its inexpensive cost, fast response time, nonintrusive measurements and high sensitivity, this technique may also be used to differentiate between isotopes due to its high spectroscopic resolution. This frequency modulation spectroscopy technique could also be applied for the on-line monitoring of CO and CO2 using InGaAsP diode lasers operation in the 1.55 microns region and H2O in the 1.3 microns region. The existence of single mode optical fibers at the near infrared region makes it possible to combine FMS with optical fiber technology. Optical fiber FMS is particularly suitable for making point-measurements at one or more locations in the CO2 laser/catalyst system.

Wang, Liang-Guo↗
DOE OSTI2020

Comparison of machine learning techniques to optimize the analysis of plutonium surrogate material via a portable LIBS device

The utilization of machine learning techniques has become commonplace in the analysis of optical emission spectra. These methods are often limited to variants of principal components analysis (PCA), partial-least squares (PLS), and artificial neural networks (ANNs). A plethora of other techniques exist and are well established in the world of data science, yet are seldom investigated for their use in spectroscopic problems. In this study, machine learning techniques were used to analyze optical emission spectra of laser-induced plasma from ceria pellets doped with silicon in order to predict silicon content. Additionally, a boosted regression ensemble model was created, and its predictive accuracy was compared to that of traditional PCA, PLS, and ANN regression models. Boosted regression tree ensembles yielded fits with R-squared (R2) values as high as 0.964 and mean-squared errors of prediction (MSEPs) as low as 0.074, providing the most accurate predictive model. Neural networks performed with slightly lower R2 values and higher MSEPs compared to the ensemble methods, thus indicating susceptibility to overfitting.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Containerless Techniques for in-situ X-Ray Measurements on Materials in Extreme Conditions

This article reviews containerless methods in the context of measuring materials in-situ using x-ray techniques. Non-contact processing enables high chemical purity to be achieved even at temperatures above 2000 °C. The absence of extrinsic heterogenous nucleation allows supercooling and supersaturation of liquids and solutions. In many cases new types of glass can be made, particularly from fragile liquids. Current methods for containerless processing are briefly reviewed. The application of scattering, spectroscopic and emerging x-ray techniques is described. Examples including measurements on molten metal oxides, molten metallic alloys and organic molecules are presented. The work is discussed in the broader context of combining structure and property data to predict how to make new applied materials.

36 MATERIALS SCIENCE↗
NASA NTRS2005

Energetics of RHESSI X-Class Flares

The thermal and nonthermal energies of several X-class flares seen with the Reuven Ramaty High Energy Solar Spectroscopic Imager (RHESSI) will be presented. The same techniques described by Emslie et al. (JGR, 109, A10104, 2004) are used to take the RHESSI imaging spectroscopic observations and compute the energies in the thermal plasma and in the nonthermal electrons as a function of time throughout the flares. Radiative and conductive cooling rates are estimated and total thermal and nonthermal energies are computed for each flare. Typically, the energy in nonthermal electrons integrated up to the time of peak soft X-ray emission is equal to or exceeds the energy in the thermal plasma at that time. This suggests that energy must have been converted into a form not visible with RHESSI and that the total energy released by the flares may be significantly greater than the sum of energies calculated from the RHESSI observations alone. This conclusion is supported by the high radiative energy seen with SORCE during the impulsive phase of the 28 October 2003 flare. The peak increase in total solar irradiance of 270 mW per square meters measured with SORCE was over two orders of magnitude higher than the peak soft X-ray flux seen with GOES or RHESSI. The implications of this new observation as compared to the energetics derived from the X-ray observations of that flare will be discussed along with the energetics analysis of most of the other X- class flares in October/November 2003.

Dennis, Brian R.↗
NASA NTRS2018

Water-Rock Interactions in Outer Solar System Bodies: Evidence from the Coordinated Analysis of Interplanetary Dust

NASA has an ongoing program of collecting interplanetary dust particles (IDPs) in the stratosphere using high altitude research aircraft. The collected IDPs are derived from asteroids and comets and here we report studies of a subset of hydrated IDPs rich in carbonaceous matter that are proposed to have a cometary origin. Our studies are aimed at understanding the evolution of oxygen reservoirs in the Solar System and their interaction with cometary minerals and organic matter. The small size (<20 μm) and fragility of these IDPs present a number of analytical challenges. We have pioneered techniques for performing chemical, mineralogical, isotopic, and spectroscopic measurements on the same sample in a carefully coordinated sequence. Coordinated analyses of nanogram-size samples is made possible by several delicate sample preparation techniques. To avoid organic contamination, we embed IDPs in elemental sulfur and use ultramicrotomy to partly section the particles (the first few micrometers). Multiple thin sections (50-70 nm thick) are placed on different substrates depending on the analysis technique. We use a JEOL 2500SE scanning, transmission electron microscope (STEM) to determine the mineralogy, microstructure, and elemental compositions of constituent minerals in the thin sections through a combination of high resolution imaging, electron diffraction, quantitative energy-dispersive x-ray mapping, and electron energy-loss spectroscopy. Following the STEM analyses, we use a NanoSIMS 50L for high spatial resolution isotopic measurements of H, C, N, and O to search for presolar grains and to understand the origin of the indigenous organic matter. The isotopic analyses are performed on the same sections analyzed in the STEM in order to correlate isotopic properties with the elemental and mineralogical data. We reserve other thin sections for non-destructive analyses utilizing synchrotron-based techniques including Fourier-transform infrared (FTIR) micro-spectroscopy and X-ray absorption near-edge structure (XANES) analyses, especially for functional group analysis of organic matter in the particles. The remainder of the IDP is extracted from the sulfur bead that was used for microtomy and is pressed into Au foil for quantitative analysis (including light elements) using a JEOL 8530F field emission electron probe microanalyzer (EPMA). After the EPMA measurements, high precision oxygen isotopic analyses are obtained using Cameca IMS1270/1290 instruments at UCLA. The hydrated IDPs in this study are dominated by saponitic clays, with minor magnetite, carbonate and abundant organic matter. The remarkable oxygen isotopic compositions, high carbon contents, and the abundance of isotopically anomalous organic matter, together suggest that the high carbon, hydrated IDPs are derived from primitive sources not yet represented in meteorite collections such as outer main belt P- and D-type asteroids or comets.

Keller, Lindsay P.↗
DOE OSTI2020

Phase evolution during lithium–indium halide superionic conductor dehydration

Select rare-earth alkali halides have demonstrated high lithium ion conductivity. The conductivity appears to be related to the stability of the crystal phase, ordering of the lithium sublattice and the amount of residual H 2 O. Li 3 InCl 6 can be synthesized from concentrated aqueous solution through controlled dehydration. In this work, we track Li 3 InCl 6 dehydration using a multimodal approach that combines thermogravimetric, spectroscopic, X-ray diffraction, and neutron scattering techniques. In situ X-ray diffraction suggests a single phase transition caused by dehydration, in disagreement with spectroscopic and thermodynamic measurements. Neutron scattering, being sensitive toward the H 2 O and Li sublattices, reveals multiple phase transitions. We show that the loss of the final trace H 2 O leads to strain and grain boundary formation. Thus, controlled dehydration may be a viable strategy for high-throughput processing for roll-to-roll manufacturing of REAH solid electrolytes.

36 MATERIALS SCIENCE↗
NASA NTRS1976

Measurement techniques for analysis of fission fragment excited gases

Spectroscopic analysis of fission fragment excited He, Ar, Xe, N2, Ne, Ar-N2, and Ne-N2 have been conducted. Boltzmann plot analysis of He, Ar and Xe have indicated a nonequilibrium, recombining plasma, and population inversions have been found in these gases. The observed radiating species in helium have been adequately described by a simple kinetic model. A more extensive model for argon, nitrogen and Ar-N2 mixtures was developed which adequately describes the energy flow in the system and compares favorably with experimental measurements. The kinetic processes involved in these systems are discussed.

Schneider, R. T.↗
DOE OSTI2021

Structural Interconversion between Agglomerated Palladium Domains and Mononuclear Pd(II) Cations in Chabazite Zeolites

Palladium-exchanged zeolites are candidate materials for passive NO x adsorption in automotive exhaust aftertreatment, where mononuclear Pd cations behave as precursors to the purported NO x adsorption sites. Yet, the structures of zeolite lattice binding sites capable of stabilizing mononuclear Pd 2+ ions, and the mechanisms that interconvert agglomerated PdO and Pd domains into mononuclear Pd 2+ ions during Pd redispersion treatments, remain incompletely understood. In this work, we use a suite of spectroscopic methods and quantitative site titration techniques to characterize mononuclear and agglomerated Pd species on zeolites with varying material properties and treatment history. Aqueous-phase methods to introduce Pd onto NH 4 -form zeolites initially form mononuclear [Pd(NH 3 ) 4 ] 2+ complexes, but subsequent thermal treatments (573–723 K; air) lead to in situ formation of H 2 that first reduces Pd 2+ to metallic Pd domains, which are then oxidized by air to PdO domains. Progressive treatment of Pd-zeolites in air to higher temperatures (723–1023 K) converts larger fractions of agglomerated PdO to mononuclear Pd 2+ , as quantified by H 2 temperature programmed reduction, because higher temperature treatments facilitate Pd redispersion toward deeper locations within chabazite (CHA) crystallites, which is corroborated by complementary titrimetric and spectroscopic data. Pd-CHA zeolites synthesized with similar bulk Pd and framework Al content, but varying framework Al arrangement, provide evidence that six-membered rings (6-MR) hosting paired Al sites (Al–O–(Si–O) x –Al, x = 1, 2) stabilize Pd 2+ ions and that otherwise isolated Al sites can stabilize [PdOH] + species, identifiable by an IR OH stretch at 3660 cm –1 . These findings clarify the underlying chemical processes and gas environments that cause Pd agglomeration in zeolites and their subsequent redispersion to mononuclear Pd 2+ ions, which prefer binding at 6-MR paired Al sites in CHA, and indicate that higher temperature air treatments lead to more uniform Pd spatial distributions throughout zeolite crystallites.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Clustering redshift distribution calibration of weak lensing surveys using the DESI-DR1 spectroscopic dataset

We estimate the source redshift distribution of current weak lensing surveys by applying the clustering-based redshift calibration technique, using the galaxy redshift sample provided by the Dark Energy Spectroscopic Instrument Data Release 1 (DESI-DR1). We cross-correlate the Bright Galaxy Survey (BGS), Luminous Red Galaxies (LRGs) and Emission Line Galaxies (ELGs) from DESI, within the redshift range $0.1 < z < 1.6$, with overlapping tomographic source samples from the Dark Energy Survey (DES), Kilo-Degree Survey (KiDS), and Hyper Suprime-Cam (HSC) survey. Using realistic mock catalogues, we test the stability of the clustering-redshift signal to fitting scale, reference-sample choice, and the evolution of source galaxy bias, and we explicitly model and marginalise over magnification contributions, which become non-negligible at $z \gtrsim 1$ due to the depth of the DESI ELG sample. We then compare the resulting bias-weighted redshift distributions to those calibrated using self-organising map (SOM) techniques, finding agreement within uncertainties for all surveys and tomographic bins. Our results demonstrate that clustering redshifts enabled by DESI's unprecedented spectroscopic sample provides a robust, complementary, and independent constraint capable of reducing one of the dominant systematic uncertainties in weak lensing cosmology.

Ruggeri, R. [Queensland U.]↗
NASA NTRS1993

Quantitative Mapping of Pore Fraction Variations in Silicon Nitride Using an Ultrasonic Contact Scan Technique

An ultrasonic scan procedure using the pulse-echo contact configuration was employed to obtain maps of pore fraction variations in sintered silicon nitride samples in terms of ultrasonic material properties. Ultrasonic velocity, attenuation coefficient, and reflection coefficient images were obtained simultaneously over a broad band of frequencies (e.g., 30 to 110 MHz) by using spectroscopic analysis. Liquid and membrane (dry) coupling techniques and longitudinal and shear-wave energies were used. The major results include the following: Ultrasonic velocity (longitudinal and shear wave) images revealed and correlated with the extent of average through-thickness pore fraction variations in the silicon nitride disks. Attenuation coefficient images revealed pore fraction nonuniformity due to the scattering that occurred at boundaries between regions of high and low pore fraction. Velocity and attenuation coefficient images were each nearly identical for machined and polished disks, making the method readily applicable to machined materials. Velocity images were similar for wet and membrane coupling. Maps of apparent Poisson's ratio constructed from longitudinal and shear-wave velocities quantified Poisson's ratio variations across a silicon nitride disk. Thermal wave images of a disk indicated transient thermal behavior variations that correlated with observed variations in pore fraction and velocity and attenuation coefficients.

Roth, Don J.↗
DOE OSTI2020

Design and performance of high-temperature furnace and cell holder for in situ spectroscopic, electrochemical, and radiolytic investigations of molten salts

To facilitate the development of molten salt reactor technologies, a fundamental understanding of the physical and chemical properties of molten salts under the combined conditions of high temperature and intense radiation fields is necessary. Optical spectroscopic (UV–Vis–near IR) and electrochemical techniques are powerful analytical tools to probe molecular structure, speciation, thermodynamics, and kinetics of solution dynamics. In this paper, we report the design and fabrication of three custom-made apparatus: (i) a multi-port spectroelectrochemical furnace equipped with optical spectroscopic and electrochemical instrumentation, (ii) a high-temperature cell holder for time-resolved optical detection of radiolytic transients in molten salts, and (iii) a miniaturized spectroscopy furnace for the investigation of steady-state electron beam effects on molten salt speciation and composition by optical spectroscopy. Initial results obtained with the spectroelectrochemical furnace (i) and high-temperature cell holder (ii) are reported.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2020

Understanding Functionalization of Titanium Carbide (MXene) with Quinones and Their Pseudocapacitance

In this work, the interaction mechanism of 1-aminoanthraquinone (AQ) on Ti 3 C 2 T x MXene by noncovalent (AQ@Ti 3 C 2 T x ) and covalent (AQ-Ti 3 C 2 T x ) functionalization is reported. Spectroscopic, X-ray, and scattering techniques confirmed noncovalent functionalization of AQ on Ti 3 C 2 T x MXene without its catalytic decomposition, resulting in intercalation and interaction of AQ with Ti 3 C 2 T x MXene. Diazonium reaction was further used to covalently functionalize AQ molecules on Ti 3 C 2 T x MXene. Optimized AQ-Ti 3 C 2 T x freestanding electrodes of ~44 μm thickness delivered capacitance of ~300 F/g and improved rate performance compared to the pristine counterpart (Ti 3 C 2 T x ) due to carbonyl redox of AQ and improved ionic transport between MXene layers due to pillaring of AQ molecules.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Spatially Resolved Mass Spectrometry at the Single Cell: Recent Innovations in Proteomics and Metabolomics

Biological systems are composed of heterogeneous populations of cells that intercommunicate to form a functional living tissue. Biological function varies greatly across populations of cells, as each single cell has a unique transcriptome, proteome, and metabolome that translates to functional differences within single species and across kingdoms. Over the past decade, substantial advancements in our ability to characterize omic profiles on a single cell level have occurred, including in multiple spectroscopic and mass spectrometry (MS)-based techniques. Of these technologies, spatially resolved mass spectrometry approaches, including mass spectrometry imaging (MSI), have shown the most progress for single cell proteomics and metabolomics. For example, reporter-based methods using heavy metal tags have allowed for targeted MS investigation of the proteome at the subcellular level, and development of technologies such as laser ablation electrospray ionization mass spectrometry (LAESI-MS) now mean that dynamic metabolomics can be performed in situ. In this Perspective, we showcase advancements in single cell spatial metabolomics and proteomics over the past decade and highlight important aspects related to high-throughput screening, data analysis, and more which are vital to the success of achieving proteomic and metabolomic profiling at the single cell scale. Finally, using this broad literature summary, we provide a perspective on how the next decade may unfold in the area of single cell MS-based proteomics and metabolomics.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2024

Phase-resolving spin-wave microscopy using infrared strobe light

The need for sensitively and reliably probing magnetization dynamics has been increasing in various contexts such as studying novel hybrid magnonic systems, in which the spin dynamics strongly and coherently couple to other excitations, including microwave photons, light photons, or phonons. Recent advances in quantum magnonics also highlight the need for employing the magnon phase as quantum state variable, which is to be detected and mapped out with high precision in on-chip micro- and nanoscale magnonic devices. Here, in this study, we demonstrate a facile optical technique that can directly perform concurrent spectroscopic and imaging functionalities with spatial and phase resolutions, using infrared strobe light operating at 1550-nm wavelength. To showcase the methodology, we spectroscopically studied the phaseresolved spin dynamics in a bilayer of Permalloy and yttrium iron garnet Y 3 Fe 5 O 12 (YIG), and spatially imaged the backward-volume spin-wave modes of YIG in the dipolar spin-wave regime. Using the strobe light probe, the detected precessional phase contrast can be directly used to construct the map of the spin wave's wave front, in the continuous-wave regime of spin-wave propagation and in the stationary state, without needing any optical reference path. By selecting the applied field, frequency, and detection phase, the spin-wave images can be made sensitive to the precession amplitude and phase. Our results demonstrate that infrared optical strobe light can serve as a versatile platform for magneto-optical probing of magnetization dynamics, with potential implications in investigating hybrid magnonic systems.

Xiong, Yuzan [University of North Carolina, Chapel↗
DOE OSTI2023

Real-Time Nitrate Ion Monitoring with Poly(3,4-ethylenedioxythiophene) (PEDOT) Materials

Nitrate (NO 3 ) pollution in groundwater, caused by various factors both natural and synthetic, contributes to the decline of human health and well-being. Current techniques used for nitrate detection include spectroscopic, electrochemical, chromatography, and capillary electrophoresis. It is highly desired to develop a simple cost-effective alternative to these complex methods for nitrate detection. Therefore, a real-time poly (3,4-ethylenedioxythiophene) (PEDOT)-based sensor for nitrate ion detection via electrical property change is introduced in this study. Vapor phase polymerization (VPP) is used to create a polymer thin film. Variations in specific parameters during the process are tested and compared to develop new insights into PEDOT sensitivity towards nitrate ions. Through this study, the optimal fabrication parameters that produce a sensor with the highest sensitivity toward nitrate ions are determined. With the optimized parameters, the electrical resistance response of the sensor to 1000 ppm nitrate solution is 41.79%. Furthermore, the sensors can detect nitrate ranging from 1 ppm to 1000 ppm. The proposed sensor demonstrates excellent potential to detect the overabundance of nitrate ions in aqueous solutions in real time.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗