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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 667 records · Page 37
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Temperature-Swing Synthesis of Large-Size Single-Crystal LiNi 0.6 Mn 0.2 Co 0.2 O 2 Cathode Materials

Single-crystal lithium-nickel-manganese-cobalt-oxide (SC-NMC) has recently emerged as a promising battery cathode material due to its outstanding cycle performance and mechanical stability over the tradional polycrystalline NMC. It is favorable to further increase the grain size of SC-NMC particles to achieve a higher volumetric energy density and minimize surface-related degradations. However, the preparation of large-size yet high performance SC-NMC particles faces a challenge in choosing a suitable temperature for sintering. High temperature promotes grain growth but induces cation mixing that negatively impacts the electrochemical performance. Here we report a temperature-swing sintering (TSS) strategy with two isothermal stages that fulfils the needs for grain growth and structural ordering sequentially. A high-temperature sintering is first used for a short period of time to increase grain size and then the reaction temperature is lowered and kept constant for a longer period of time to improve structural ordering and complete the lithiation process. SC-LiNi 0.6 Mn 0.2 Co 0.2 O 2 materials prepared via TSS exhibit large grain size (~4 μm), a low degree of cation mixing (~0.9%), and outperform the control samples prepared by the conventional sintering method. Furthermore, this work highlights the importance of understanding the process-structure-property relationships and may guide the synthesis of other SC Ni-rich cathode materials.

25 ENERGY STORAGE↗
DOE OSTI2014

ARTIFACT FORMATION DURING NEUTRALIZATION OF TANK 50 SAMPLES

Degradation products have been identified in the extracts of Tank 50 samples analyzed by semivolatile organic compound analysis (SVOA) using gas chromatography/mass spectrometry (GC/MS). These materials, identified as short chain alkyl alcohols, were formed by acidification during sample preparation. A number of questions were raised about the formation of these and other materials reported in Tank 50 surface samples, and this report serves to address these questions.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2016

Mesoporous palladium–copper ferrites as highly efficient and magnetically separable catalysts for Suzuki coupling reaction

Highlights: • Mesoporous Cu–Pd ferrites were prepared by a facile, mild and environment-friendly route. • The catalysts have shown great efficiencies in Suzuki coupling reaction and up to 36.9 × 10{sup 3} h{sup −1} TOF can be obtained. • The catalyst can be magnetically separated easily and have shown prominent recyclability. - Abstract: Mesoporous Cu–Pd ferrites were prepared by using MCM-41 and SBA-15 mesoporous molecular sieves as hard templates and well characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), ICP-atomic emission spectroscopy, N{sub 2} adsorption–desorption and X-ray photoelectric spectroscopy (XPS). Compared with samples prepared by the sol–gel auto-combustion methods, the as-prepared mesoporous ferrites have shown uniform pore size and much higher specific surface areas. The samples showed a remarkably high activity in connection with the Suzuki coupling reaction, especially Cu{sub 0.99}Pd{sub 0.01}Fe{sub 2}O{sub 4} prepared by using MCM-41 as template obtained an excellent TOF as high as 36.9 × 10{sup 3} h{sup −1} and no obvious decrease in the activity was observed after ten consecutive runs.

36 MATERIALS SCIENCE↗
NASA NTRS1985

Characterization of material surfaces exposed to atomic oxygen on space shuttle missions

Material samples prepared for exposure to ambient atomic oxygen encountered during space shuttle flights in low Earth orbit were characterized by the experimental techniques of ELLIPSOMETRY, ESCA, PIXE, and RBS. The first group of samples, which were exposed during the STS-8 mission, exhibited some very interesting results. The second group of samples, which are to be exposed during the upcoming STS-17 mission, have been especially prepared to yield quantitative information on the optical changes, oxygen solution, and surface layer formation on metal films of silver, gold, nickel, chromium, aluminum, platinum, and palladium evaporated onto optically polished silicon wafers.

Fromhold, A. T.↗
DOE OSTI2018

Effects of Al content and annealing on the phases formation, lattice parameters, and magnetization of A l x F e 2 B 2 ( x = 1.0 , 1.1 , 1.2 ) alloys

AlFe 2 B 2 is a ferromagnet with the Curie temperature around 300 K and has the potential to be an outstanding rare-earth free candidate for magnetocaloric applications. However, samples prepared from the melt contain additional phases which affect the functional response of the AlFe 2 B 2 phase. Here, we report on the effects of Al content in samples with the initial (nominal) composition of Al x Fe 2 B 2 where x=1.0, 1.1, and 1.2 prepared by arc-melting followed by suction casting and annealing. The as-cast Al x Fe 2 B 2 alloys contain AlFe 2 B 2 as well as additional phases including the primary solidifying FeB and Al 13 Fe 4 compounds which are ferromagnetic and paramagnetic, respectively, at 300 K. The presence of these phases makes it difficult to extract the intrinsic magnetic properties of AlFe 2 B 2 phase. Annealing of Al x Fe 2 B 2 alloys at 1040°C for 3 days allows for reaction of the FeB with Al 13 Fe 4 to form the AlFe 2 B 2 phase, significantly reduces the amount of additional phases, and results in nearly pure AlFe 2 B2 phase as confirmed with XRD, magnetization, scanning electron microscopy, and electronic transport. The values of the magnetization, effective magnetic moment per Fe atom, specific heat capacity, electrical resistivity and Seebeck coefficient for the AlFe 2 B 2 compound have been established.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Facile Synthesis of Fe/N/S‐Doped Carbon Tubes as High‐Performance Cathode and Anode for Microbial Fuel Cells

Abstract As a renewable energy technology, microbial fuel cell (MFC) has been attracting increasing attention in recent decades. However, practical applications of MFCs has been hampered by the unsatisfactory electrode performance, in particular, at the cathode. Herein, Fe/N/S‐doped carbon hollow tubes were prepared by a facile two‐stage procedure involving hydrothermal treatment and pyrolysis at controlled temperatures. Electrochemical studies showed that the obtained samples exhibited an apparent electrocatalytic activity towards oxygen reduction reaction in both alkaline and acidic media, a performance comparable to that of commercial Pt/C, and the sample prepared at 800 °C stood out as the best among the series with a half‐wave potential of +0.81 V vs. RHE and an electron transfer number of 3.98 at +0.6 V vs. RHE. The Fe/N/S‐doped carbon tubes also exhibited a remarkable performance as an MFC anode by facilitating bacterial growth and electron transfer between the biofilm and electrode. In fact, an MFC based on the carbon tubes as both cathode and anode showed a markedly higher performance (maximum power density 479 W m −3 ) than the control MFC based on a graphene aerogel anode and Pt/C cathode (359 W m −3 ). These results suggest that Fe/N/S‐doped carbon composites can be used for the fabrication of high‐efficiency MFC electrodes.

Yang, Wei↗
DOE OSTI2018

Integration of paper spray ionization high‐field asymmetric waveform ion mobility spectrometry for forensic applications

Rationale Paper spray ionization (PSI) is an attractive ambient ionization source for mass spectrometry (MS) since it allows the combination of surface sampling and ionization. The minimal sample preparation inherent in this approach greatly reduces the time needed for analysis. However, the ions generated from interfering compounds in the sample and the paper substrate may interfere with the analyte ions. Therefore, the integration of PSI with high‐field asymmetric ion mobility spectrometry (FAIMS) is of significant interest since it should reduce the background ions entering the mass analyzer without complicating the analysis or increasing analysis time. Here we demonstrate the integration of PSI with FAIMS/MS and its potential for analysis of samples of forensic interest. Methods In this work, the parameters that can influence the integration, including sampling and ionization by paper spray, the FAIMS separation of analytes from each other and background interferences, and the length of time that a usable signal can be observed for explosives on paper, were evaluated with the integrated system. Results In the negative ion analysis of 2,4,6‐trinitrotoluene (TNT), pentaerythritol tetranitrate (PETN), octahydro‐1,3,5,7‐tetranitro‐1,3,5,7‐tetrazocine (HMX), and 1,3,5‐trinitroperhydro‐1,3,5‐triazine (RDX), amounts as low as 1 ng on paper were readily observed. The successful positive ion separation of a set of illicit drugs including heroin, methamphetamine, and cocaine was also achieved. In addition, the positive ion analysis of the chemical warfare agent simulants dimethyl methylphosphonate (DMMP) and diisopropyl methylphosphonate (DIMP) was evaluated. Conclusions The integration of PSI‐FAIMS/MS was demonstrated for the analyses of explosives in negative ion mode and for illicit drugs and CW simulants in positive mode. Paper background ions that could interfere with these analyses were separated by FAIMS. The compensation voltage of an ion obtained by FAIMS provided an additional identification parameter to be combined with the mass spectrum for each analyte.

Tsai, Chia‐Wei↗
DOE OSTI2018

Effect of NaOH Concentration and Adding Sequences on Structural and Magnetic Properties of Ni{sub 0.4}Co{sub 0.6}Fe{sub 2}O{sub 4} Nanopowders Prepared Via Co-precipitation Route

Ni{sub 0.4}Co{sub 0.6}Fe{sub 2}O{sub 4} nanopowders were prepared via the co-precipitation route followed by annealing treatment. The structural and magnetic properties of the as-synthesized samples were determined by XRD, FT-IR, TG-DSC, and PPMS measurements, respectively. The XRD patterns indicated a single-phase cubic spinel structure for all the Ni-Co ferrite samples, regardless of adding sequences of the reactants or NaOH concentration. The analysis of the XRD patterns revealed that the enhancement in lattice constant with increasing NaOH concentration is related to the prevention of oxidization of Co{sup 2+} ions in the Ni-Co ferrite lattice. The FT-IR spectra indicated that samples prepared in the B process have fewer impurities than those prepared in the A process. The enhancement in saturation magnetization with the increase in sodium hydroxide concentration could be attributed to the strengthening of super-exchange interaction between A and B sublattices, due to replacements of Co{sup 3+} ions (magnetic moment of 0 μ{sub B}) by Co{sup 2+} ions (magnetic moment of 3 μ{sub B}) at B sublattices. The obvious increase in the coercivity field with the increase in concentration of NaOH solutions can be interpreted in terms of enhancement of magneto-crystalline anisotropy that originated from gradual substitutions of Co{sup 3+} ions with Co{sup 2+} ions at the octahedral sites.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2017

Influence of Osmotic Drying with an Aqueous Poly(ethylene Glycol) Liquid Desiccant on Alumina Objects Gelcast with Gelatin

Gelcasting and liquid desiccant drying are novel forming and drying methods used to mitigate common issues associated with the fabrication of complex advanced ceramic objects. Here, the molecular weight and osmotic pressure of aqueous poly(ethylene glycol) (PEG) desiccant solutions were simultaneously varied to understand their influence on the net mass loss rates of gelcast alumina samples prepared using gelatin as a gelling agent. Additionally, the amount of PEG diffusion and water diffusion to and from the ceramic samples after 150 min of immersion in the liquid desiccant was correlated to the solution properties as was the final bulk density of the sintered samples. Furthermore, solutions with high molecular weight and low osmotic pressure resulted in low PEG gain and low water loss, while solutions with low molecular weight and high osmotic pressure resulted in high PEG gain and high water loss. In some cases, more than 40 wt% of the total water per sample was removed through the liquid desiccant drying process.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Residual resistance ratio measurement system for Nb 3 Sn wires extracted from Rutherford cables

Residual resistance ratio (RRR) of superconducting strands is an important parameter for magnet electrical stability. RRR serves as a measure of the low-temperature electrical conductivity of the copper within a conductor that has a copper stabilization matrix. For Nb 3 Sn, due to the need of a reaction heat treatment, the technical requirements for high quality measurements of strands extracted from Rutherford cables are particularly demanding. Quality of wire, cabling deformation, heat treatment temperature, heat treatment atmosphere, sample handling, and measurement methods can all affect the RRR. Therefore, as an integral part of the electrical quality control (QC) of Nb 3 Sn Rutherford cables manufactured at the Lawrence Berkeley National Laboratory, it was prudent that we established a RRR measurement system that can isolate the assessment of cable-fabrication-related impacts from sample preparation and measurement factors. Here we describe a bespoke cryocooler-based measurement system, capable of measuring RRR of over 80 samples in a single cooldown. The samples are mounted on custom-designed printed circuit boards that accommodate the shape of strands extracted from a Rutherford cable without added deformation, which we will show is critical in ensuring that the measurements accurately represent the RRR values of the conductor within the cable. Using this sample mounting solution, we routinely measure the overall RRR of the strand as well as individual intra-strand sections corresponding to both cable edges and cable broad faces with high reproducibility. Such measurements provide valuable information on the variation of RRR along the length of the strands as well as across strand productions and cable runs over time.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2026

Elemental analysis of air-sensitive frozen molten salt samples using an inert transfer chamber for LIBS/LA-ICP-TOF-MS analysis

A novel inert sample transfer system was developed and employed to enable, for the first time, the analysis of air-sensitive salt samples in a two-volume ablation cell using simultaneous laser-induced breakdown spectroscopy (LIBS) and laser ablation (LA)-inductively coupled plasma (ICP)-time-of-flight (TOF)-mass spectrometry (MS) analysis. Molten salts are of growing interest as a medium for advanced nuclear reactors and nuclear fuel reprocessing technologies continue to be developed around their use. However, compositional analysis of molten salt samples can be challenging because of their air-sensitive nature and varying solubilities leading to inaccurate measurements when digested. LA-based analysis provides an alternate method to digestion and can provide rapid elemental information with little sample preparation. In this study, LIBS and LA-ICP-TOF-MS were used to analyze the Ce content in frozen salt samples taken from a series of electrochemical experiments. Calibrations were built for each technique, and the resulting limits of detection for Ce were estimated to be 107 and 58 µg g −1 for LIBS and LA-ICP-TOF-MS, respectively. Test samples from the electrochemical experiments were analyzed using these calibrations. The results matched bulk digestion-based ICP-optical emission spectroscopy values, and daily trends in Ce concentration changes were identified. Additionally, the LIBS and LA-ICP-TOF-MS analysis was demonstrated for identifying microgram per gram levels of components and detecting trace contaminants. The impurities detected by LIBS included Al, Mg, Ca, and Na. The impurities detected by LA-ICP-TOF-MS included W, Ag, Al, Fe, Ni, Mo, Nd, Sm, Th, and U.

Andrews, Hunter B. [Oak Ridge National Laboratory ↗
DOE OSTI2022

A Laboratory-driven Multiscale Investigation of X-Ray Induced Mass Loss and Photochemical Evolution in Cosmic Carbon and Silicate Dust

We present the results of an integrated laboratory and modeling investigation into the impact of stellar X-rays on cosmic dust. Carbonaceous grains were prepared in a cooled (< 200 K) supersonic expansion from aromatic molecular precursors, and were later irradiated with 970 eV X-rays. Silicate (enstatite) grains were prepared via laser ablation, thermally annealed, and later irradiated with 500 eV X-rays. Infrared spectra of the 3.4 μm band of the carbon sample prepared with benzene revealed 84% ± 5% band area loss for an X-ray dose of 5.2 x 10 23 eV.cm -2 . Infrared spectra of the 8 -12 μm Si-O band of the silicate sample revealed band area loss up to 63% ± 5% for doses of 2.3 x 10 23 eV.cm -2 . A hybrid Monte Carlo particle trajectory approach was used to model the impact of X-rays and ensuing photoelectrons, Auger and collisionally ionized electrons through the bulk. As a result of x-ray ionization and ensuing Coulomb explosions on surface molecules, the calculated mass loss is 60% for the carbonaceous sample and 46% for the silicate sample, within a factor of 2 of the IR band loss, supporting an X-ray induced mass-loss mechanism. We apply the laboratory X-ray destruction rates to estimate the lifetimes of dust grains in protoplanetary disks surrounding 1 M ⊙ and 0.1 M ⊙ G and M stars. In both cases, X-ray destruction timescales are short (a few million years) at the disk surface, but are found to be much longer than typical disk lifetimes (≳10 Myr) over the disk bulk.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2019

Comparative Study of Magnetocaloric Effect in La{sub 0.67}Ca{sub 0.20}Sr{sub 0.13}MnO{sub 3} Manganite Prepared by Sol-Gel Method and Spark Plasma Sintering

The La{sub 0.67}Ca{sub 0.20}Sr{sub 0.13}MnO{sub 3} nanoparticles and bulks were prepared by using sol-gel method (SGM) and spark plasma sintering (SPS), respectively. The X-ray diffraction analysis indicates each sample crystal in a single rhombohedral perovskite structure (space group R 3-bar c). The Curie temperature is slightly improved and the phase transition is sharpened after processing with SPS. The enhancement of magnetocaloric effect (MCE) is also observed in the samples prepared by SPS. For a field change of 3 T, the maximum isothermal entropy change is improved by 32 and 117% when different sintering temperatures and sintering pressures are applied. The magnetic phase transition and MCE can be well described by the Landau theory. The present studies suggest that the perovskite bulks prepared by SPS could be useful for the application of magnetic refrigeration.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2012

HRTEM study of track evolution in 120-MeV U irradiated Gd2Ti2O7

High resolution Scanning Transmission Electron Microscopy (HRTEM) experiments were performed on Gd2Ti2O7 pyrochlores irradiated with 120-MeV U ions. A judicious choice of irradiation energy, sample preparation (using Focused Ion Beam) and analytical technique (HRTEM) allowed us to visualize the complete evolution of tracks from the surface of samples down to depths exceeding the projected range of irradiating ions. Such features as variation of track diameters, changes in track directions and discontinuous segments of tracks were clearly documented at various depths. By using two different STEM imaging modes: High- and Low-Angle Annular Dark Field imaging (HAADF and LAADF), it was possible to observe the layered structure of tracks composed of an amorphous core surrounded by a strained crystalline envelope.

120↗
DOE OSTI2025

Detection and quantification of trace technetium in the presence of molybdenum using laser-induced breakdown spectroscopy

Technetium (Tc) is a very important element that is encountered in many aspects, from its presence in radioactive waste and its potential environmental impact to its use as a medical radioisotope. Its detection and quantification in liquid samples is traditionally cumbersome, involving detailed sample preparation and analysis by mass spectrometry or scintillation. This article demonstrates the first comprehensive emission spectral analysis of Tc from a liquid sample by immobilization in a polymer and analysis by laser-induced breakdown spectroscopy (LIBS). A survey of LIBS spectra was completed to identify the strongest analytical lines for quantification of trace Tc in the presence of Mo. The quantification of Tc in a Mo-containing matrix was selected because Tc radioisotopes are the daughter products of Mo isotope decay. The first reported calibration curves by LIBS are provided with limits of detection and quantification down to 0.710 µg mL −1 and 1.39 µg mL −1 , respectively. Ultimately, this study demonstrated the feasibility of trace Tc quantification using LIBS and will serve as a reference for future research related to monitoring this radioactive species.

Andrews, Hunter B. [Oak Ridge National Laboratory ↗
DOE OSTI2014

230 Th/U ages Supporting Hanford Site-Wide Probabilistic Seismic Hazard Analysis

This product represents a USGS Administrative Report that discusses samples and methods used to conduct uranium-series isotope analyses and resulting ages and initial 234U/238U activity ratios of pedogenic cements developed in several different surfaces in the Hanford area middle to late Pleistocene. Samples were collected and dated to provide calibration of soil development in surface deposits that are being used in the Hanford Site-Wide probabilistic seismic hazard analysis conducted by AMEC. The report includes description of sample locations and physical characteristics, sample preparation, chemical processing and mass spectrometry, analytical results, and calculated ages for individual sites. Ages of innermost rinds on a number of samples from five sites in eastern Washington are consistent with a range of minimum depositional ages from 17 ka for cataclysmic flood deposits to greater than 500 ka for alluvium at several sites.

58 GEOSCIENCES↗
DOE OSTI2013

Measuring thermal diffusivity of mechanical and optical grades of polycrystalline diamond using an AC laser calorimetry method

Because of its extremely high thermal conductivity, measuring the thermal conductivity or diffusivity of optical-grade diamond can be challenging. Various methods have been used to measure the thermal conductivity of thick diamond films. For the purposes of commercial quality control, the AC laser calorimetry method is appealing because it enables fairly rapid and convenient sample preparation and measurement. In this paper, the method is used to measure the thermal diffusivity of optical diamond. It is found that sample dimensions and measurement parameters are critical, and data analysis must be performed with great care. The results suggest that the method as it is applied to optical-grade diamond could be enhanced by a more powerful laser, higher frequency beam modulation, and post-processing based on 2D thermal simulation.

AC laser calorimetry↗
DOE OSTI2016

Magnetic studies of nickel ferrite nanoparticles prepared by sol-gel technique

Ni-ferrite nanoparticles were synthesized by sol–gel technique by varying the solvent concentration. X-ray diffraction studies confirmed the phase purity in the samples. The lattice constant and grain size were found to be in the range of 0.833-0.834 nm and 14-26 nm respectively. There was no systematic variation in magnetization value with the solvent concentration and grain size. The highest magnetization, remanence and coercivity values of 60 emu/g, 12 emu/g and 180 Oe respectively were observed at 300K in the present study for the sample prepared in 75ml of solvent. The observed magnetization value is 20% higher than the bulk value of 50 emu/g. The magnetization, coercivity and remanence values were enhanced at 60K compared to those at 300K. The observed high magnetization value in the nanoparticles can be explained on the basis of modified cation distribution in the lattice sites. The enhanced magnetic properties at 60K may be understood due to the reduced thermal fluctuation and increased anisotropy at low temperature.

77 NANOSCIENCE AND NANOTECHNOLOGY↗