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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 73 records · Page 4
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Investigation of Rechargeable Calcium Metal-Selenium Batteries Enabled by Borate-Based Electrolytes

Calcium-ion batteries (CIBs) are a promising next-generation energy storage system given the low redox potential of calcium metal and high abundance of calcium compounds. For continued CIB development, the discovery of high energy density calcium ion cathodes is needed to achieve practical energy density values. Here, we report on the use of elemental Se as a promising candidate for a high-capacity cathode material for CIBs that operates via a conversion mechanism in a Ca metal battery at room temperature. The Se electrodes demonstrate a reversible specific capacity of 180 mA h g –1 with a discharge plateau near 2.0 V (vs Ca 2+ /Ca) at 100 mA g –1 using an electrolyte based on the salt calcium tetrakis(hexafluoroisopropyloxy)borate (Ca(B(hfip) 4 ) 2 ) in 1,2-dimethoxyethane (DME) and Ca metal. The reversible electrochemical reaction between calcium and selenium is investigated using operando synchrotron-based techniques and the possible reaction mechanism discussed.

25 ENERGY STORAGE↗
DOE OSTI2025

Inorganic Alterations in Unconventional Shale Reservoirs: Importance of Additive and Base Fluid Chemistry

The effective development of unconventional petroleum systems requires the use of significant water resources. In an effort to reduce the consumption of freshwater resources for hydraulic fracturing, highly saline produced waters are increasingly recycled for use as a base fluid. However, there are significant knowledge gaps regarding potential water–rock interactions resulting from the introduction of produced waters and associated additives into shale reservoirs such as formation and deposition of mineral scale, which can negatively affect hydrocarbon production through wellbore restriction and damage to hydraulically generated fractures. To assess the impacts of field stimulation practices in the subsurface, a series of laboratory experiments were completed using (a) three distinct sedimentary rock formations of the Midland Basin (Texas, USA) and (b) additives with two different base fluids: municipal fresh water and clean brine. The experimental approach used relevant injection sequences and mixing ratios in specialized reactors for 3 weeks. Static pressurized experiments and nonpressurized time-resolved experiments were undertaken. The resulting solids and liquids were analyzed by using a variety of laboratory- and synchrotron-based techniques. The use of an acid spearhead (15% HCl) resulted in texturing of both clay-rich and calcareous shales, which can temporarily enhance porosity but subsequently result in mineral scale deposition. The primary matrix scale was Fe(III)-bearing phases, which occurred in all experiments regardless of base fluid chemistry. Additionally, strontium sulfate (SrSO 4 ) precipitated on shale surfaces when clean brines were used. It was concluded that clean brine was the main source of Sr 2+ species, while persulfate breaker degradation and oxidation of pyrite were the sources of SO 4 2– . Sulfate scaling was more pronounced in clay-rich shales, suggesting that Sr sorption is important for promoting celestite formation. This work demonstrates that mineral scale deposition is a complex phenomenon, whereby the type and proportions of various mineral phases are determined from reservoir alteration processes and coprecipitation of constituents from injection fluids. In conclusion, the experimental results shown here should be considered when evaluating different base fluids and additives in order to mitigate mineral precipitation in unconventional shale reservoirs, which could result in reservoir degradation.

Jew, Adam D. [SLAC National Accelerator Laboratory↗
DOE OSTI2020

Tuning the Morphology and Electronic Properties of Single-Crystal LiNi 0.5 Mn 1.5 O 4-δ : Exploring the Influence of LiCl–KCl Molten Salt Flux Composition and Synthesis Temperature

Single-crystal materials have played a unique role in the development of high-performance cathode materials for Li batteries due to their favorable chemomechanical stability. The molten salt synthesis method has become one of the most prominent techniques used to synthesize single-crystal layered and spinel materials. In this work, the molten salt synthesis method is used as a technique to tune both the morphology and Mn 3+ content of high-voltage LiNi 0.5 Mn 1.5 O 4 (LNMO) cathodes. The resulting materials are thoroughly characterized by a suite of analytical techniques, including synchrotron X-ray core-level spectroscopy, which are sensitive to the material properties on multiple length scales. Furthermore, the multidimensional characterization allows us to build a materials library according to the molten salt phase diagram as well as to establish the relationship among synthesis, material properties, and battery performance. The results of this work show that the Mn 3+ content is primarily dependent on the synthesis temperature and increases as the temperature is increased. Additionally, the particle morphology is mostly dependent on the composition of the molten salt flux, which can be tailored to obtain well-defined octahedrons enclosed by (111) facets, plates with predominant ($11\tilde{2}$) facets, irregularly shaped particles, or mixtures of these. The electrochemical measurements indicate that the Mn 3+ content has a larger contribution to the battery performance of LNMO than do morphological characteristics and that a significant amount of Mn 3+ could become detrimental to the battery performance. However, with similar Mn 3+ contents, morphology still plays a role in influencing the battery cycle life and rate performance. The insights of molten salt synthesis parameters on the formation of LNMO, with deconvolution of the roles of Mn 3+ and morphology, are crucial to continuing studies in the rational design of LNMO cathode materials for high-energy Li batteries.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Ultrabroadband Nanocavity of Hyperbolic Phonon–Polaritons in 1D-Like α-MoO 3

The exploitation of phonon–polaritons in nanostructured materials offers a pathway to manipulate infrared (IR) light for nanophotonic applications. Notably, hyperbolic phonon–polaritons (HP 2 ) in polar bidimensional crystals have been used to demonstrate strong electromagnetic field confinement, ultraslow group velocities, and long lifetimes (up to ~12 ps). Here we present nanobelts of α-phase molybdenum trioxide (α-MoO 3 ) as a low-dimensional medium supporting HP 2 modes in the mid- and far-IR ranges. Through real-space nanoimaging techniques with synchrotron and tunable laser IR light, we observe HP 2 Fabry-Perot resonances that demonstrate distinct anisotropic propagation and frequency dependence. We remark an anisotropic propagation that critically depends on the frequency range. Our findings are supported by the convergence of experiment, theory, and numerical simulations. Our work shows that the low dimensionality of natural nanostructured crystals, like α-MoO 3 nanobelts, provides an attractive platform to study polaritonic light–matter interactions and offers appealing cavity properties that could be harnessed in future designs of compact nanophotonic devices.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

A novel integrated time-resolved array avalanche photodiode detection system for nuclear resonant scattering measurements

Here, the nuclear resonant scattering (NRS) experiment requires photon-counting detectors with high time resolution, short dead time, large dynamic range, low noise, and large detection area. An 8-channel avalanche photodiode (APD) array detector system with high integrity, flexibility, and reliability has been developed to adapt to the demands of NRS experiments. The detector system mainly consists of four key parts: (i) an array-APD sensor, (ii) 8-channel integrated fast preamplifiers, (iii) the time-to-digital converter readout electronics, and (iv) a data acquisition system and EPICS support software. Remarkably, the system exhibits a time resolution of better than 500 ps and has a sufficiently low noise level, allowing for the lowest detection energy threshold of 4 keV. The performance of the new array-APD system as well as its real application in nuclear forward scattering (NFS) and nuclear resonant inelastic x-ray scattering (NRIXS) experiments was tested in two synchrotron facilities. With the new system, the NFS signal very close to the prompt electronic scattering signal can be extracted. Thanks to the customized EPICS-areaDetector-based control software, NRIXS spectra can be readily measured with time and energy information of the NRIXS signal stored in the raw data, which is promising for developing NRIXS data analysis in the time domain. The array-APD detector can be deployed for nuclear resonant scattering experiments at various synchrotron radiation facilities.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2024

Attosecond x-ray free-electron lasers utilizing an optical undulator in a self-selection regime

Accelerator-based x-ray free-electron lasers (XFELs) are the latest addition to the revolutionary tools of discovery for the 21st century. The two major components of an XFEL are an accelerator-produced electron beam and a magnetic undulator, which tend to be kilometer-scale long and expensive. A proof-of-principle demonstration of free-electron lasing at 27 nm using beams from compact laser wakefield accelerators was shown recently by using a magnetic undulator. However, scaling these concepts to x-ray wavelengths is far from straightforward as the requirements on the beam quality and jitters become much more stringent. Here, we present an ultracompact scheme to produce tens of attosecond x-ray pulses with several GW peak power utilizing a novel aspect of the FEL instability using a highly chirped, prebunched, and ultrabright tens of MeV electron beam from a plasma-based accelerator interacting with an optical undulator. The FEL resonant relation between the prebunched period and the energy selects resonant electrons automatically from the highly chirped beam which leads to a stable generation of attosecond x-ray pulses. Furthermore, two-color attosecond pulses with subfemtosecond separation can be produced by adjusting the energy distribution of the electron beam so that multiple FEL resonances occur at different locations within the beam. Such a tunable coherent attosecond x-ray sources may open up a new area of attosecond science enabled by x-ray attosecond pump/probe techniques. Published by the American Physical Society 2024

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2019

Experimental observations of large changes in electron density distributions in β - Ge

We report the electron density distributions in β-Ge have been experimentally determined at in situ high-pressure conditions using synchrotron diffraction techniques in a diamond anvil cell. Upon decompression, the electron density along the $c$ axis in tetragonal β-Ge displays a sudden drop at 10–11 GPa close to that of the structural α-β transition, while the β-Ge samples remain as single crystals until transforming to metastable Ge phases around 6.7–8.5 GPa. In contrast to the covalently bonded α-Ge that displays only a weak participation of $d$ electrons in the valence band under compression above 7.7 GPa, our experimental results suggest that a large change in $d$-orbital participation can occur in the β-Ge lattice which has mixed covalent and metallic bonding. The β-Ge below 10 GPa may display large fluctuations in electronic properties, which sheds light for exploring novel materials with intriguing electronic and optical properties.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Fixed Target Serial Data Collection at Diamond Light Source

Serial data collection is a relatively new technique for synchrotron users. A user manual for fixed target data collection at I24, Diamond Light Source is presented with detailed step-by-step instructions, figures, and videos for smooth data collection.

Horrell, Sam↗
NASA NTRS2004

Crystal Growth of CdTe by Gradient Freeze in Universal Multizone Crystallizator (UMC)

In the case of unsealed melt growth of an array of II-VI compounds, namely, CdTe, CdZnTe and ZnSe, there is a tremendous amount of experimental data describing the correlations between melt conditions and crystal quality. The results imply that the crystallinity quality can be improved if the melt was markedly superheated or long-time held before growth. It is speculated that after high superheating the associated complex dissociate and the spontaneous nucleation is retarded. In this study, crystals of CdTe were grown from melts which have undergone different thermal history by the unseeded gradient freeze method using the Universal Multizone Crystallizator (UMC). The effects of melt conditions on the quality of grown crystal were studied by various characterization techniques, including Synchrotron White Beam X-ray Topography (SWSXT), infrared microscopy, chemical analysis by glow discharge mass spectroscopy (GDMS), electrical conductivity and Hall measurements.

Su, Ching-Hua↗
NASA NTRS2007

Crystal Growth and Characterization of CdTe Grown by Vertical Gradient Freeze

In this study, crystals of CdTe were grown from melts by the unseeded vertical gradient freeze method. The quality of grown crystal were studied by various characterization techniques including Synchrotron White Beam X-ray Topography (SWBXT), chemical analysis by glow discharge mass spectroscopy (GDMS), low temperature photoluminescence (PL), and Hall measurements. The SWBXT images from various angles show nearly strain-free grains, grains with inhomogeneous strains, as well as twinning nucleated in the shoulder region of the boule. The GDMS chemical analysis shows the contamination of Ga at a level of 3900 ppb, atomic. The low temperature PL measurement exhibits the characteristic emissions of a Ga-doped sample. The Hall measurements show a resistivity of 1 x l0(exp 7) ohm-cm at room temperature to 3 x 10(exp 9) ohm-cm at 78K with the respective hole and electron concentration of 1.7 x 10(exp 9) cm(exp -3) and 3.9 x 10(exp 7) cm(exp -3) at room temperature.

Su, Ching-Hua↗
DOE OSTI2020

XTIP – the world's first beamline dedicated to the synchrotron X-ray scanning tunneling microscopy technique

In recent years, there have been numerous efforts worldwide to develop the synchrotron X-ray scanning tunneling microscopy (SX-STM) technique. Here, the inauguration of XTIP, the world's first beamline fully dedicated to SX-STM, is reported. The XTIP beamline is located at Sector 4 of the Advanced Photon Source at Argonne National Laboratory. It features an insertion device that can provide left- or right-circular as well as horizontal- and vertical-linear polarization. XTIP delivers monochromatic soft X-rays of between 400 and 1900 eV focused into an environmental enclosure that houses the endstation instrument. This article discusses the beamline system design and its performance.

47 OTHER INSTRUMENTATION↗
DOE OSTI2026

Exploring the tempering behaviour of additively manufactured high-alloy tool steel using synchrotron X-ray and neutron techniques

Post-processing heat treatment provides a critical pathway toward the commercialisation of additively manufactured (AM) S390 high-speed steel, which is a representative high-alloy tool steel employed in precision manufacturing, offering up to 1.5 times longer tool life and over 20% higher cutting speeds compared to conventional grades. In this study, the phase evolution of AM S390 steel during heat treatment, with particular emphasis on carbide precipitation behaviour, was systematically investigated using a combination of synchrotron X-ray and neutron techniques. The metastable M2C carbides were found to dissolve during austenitisation, while the stable primary carbides MC and M6C experienced coarsening with an average size increase of about 60 nm after just 2 min of tempering. Moreover, the austenite lattice parameters reduced from 3.618 to 3.608 Å within the first 10 min of tempering, suggesting carbon depletion in the steel matrix was likely associated with the formation of secondary carbides. This interpretation was substantiated by small-angle scattering results, which revealed the presence of nanoscale precipitates with a volume fraction of 3.1% after 60 min of tempering. These microstructural evolutions collectively accounted for the observed peak hardness of 921 HV. Furthermore, a comparative analysis of synchrotron and neutron small-angle scattering data highlighted the complementary strengths of each technique, offering critical insight into their suitability for characterising nanoscale features in AM high-alloy steels.

Synchrotron X-ray diffraction↗
DOE OSTI2023

Understanding High-Voltage Behavior of Sodium-Ion Battery Cathode Materials Using Synchrotron X-ray and Neutron Techniques: A Review

Despite substantial research efforts in developing high-voltage sodium-ion batteries (SIBs) as high-energy-density alternatives to complement lithium-ion-based energy storage technologies, the lifetime of high-voltage SIBs is still associated with many fundamental scientific questions. In particular, the structure phase transition, oxygen loss, and cathode–electrolyte interphase (CEI) decay are intensely discussed in the field. Synchrotron X-ray and neutron scattering characterization techniques offer unique capabilities for investigating the complex structure and dynamics of high-voltage cathode behavior. In this review, to accelerate the development of stable high-voltage SIBs, we provide a comprehensive and thorough overview of the use of synchrotron X-ray and neutron scattering in studying SIB cathode materials with an emphasis on high-voltage layered transition metal oxide cathodes. We then discuss these characterizations in relation to polyanion-type cathodes, Prussian blue analogues, and organic cathode materials. Finally, future directions of these techniques in high-voltage SIB research are proposed, including CEI studies for polyanion-type cathodes and the extension of neutron scattering techniques, as well as the integration of morphology and phase characterizations.

25 ENERGY STORAGE↗
NASA NTRS1982

X-ray diffraction from high pressure Ge using synchrotron radiation

The high pressure structural phase transition in Ge has been studied using the energy dispersive X-ray diffraction technique and a synchrotron radiation source. Ge was observed to transform to the beta-Sn tetragonal structure in agreement with the earlier results of Jamieson, but the phase transition began at 80 + or - 5 kilobars, a somewhat lower value than generally reported. These experimental diffraction results are compared with the recent self-consistent pseudopotential calculations of Yin and Cohen (1981) and with the observed transition pressure for shock wave loaded Ge.

Baublitz, M., Jr.↗
DOE OSTI2021

X-ray multi-probe data acquisition: A novel technique for laser pump x-ray transient absorption spectroscopy

We report the development and implementation of a novel data acquisition (DAQ) technique for synchrotron-based laser pump X-ray Transient Absorption (XTA) spectroscopy, called X-ray Multi-Probe DAQ (XMP DAQ). This technique utilizes high performance analog to digital converters and home-built software to efficiently measure and process the XTA signal from all x-ray pulses between laser excitations. XMP DAQ generates a set of time resolved x-ray absorption spectra at thousands of different pump–probe time delays simultaneously. Two distinct XMP DAQ schemes are deployed to accommodate different synchrotron storage ring filling patterns. Current Integration (CI) DAQ is a quasi-analog technique that implements a fitting procedure to extract the time resolved absorption intensity from the averaged fluorescence detector response. The fitting procedure eliminates issues associated with small drifts in the voltage baseline and greatly enhances the accuracy of the technique. Photon Counting (PC) DAQ is a binary technique that uses a time resolved histogram to calculate the XTA spectrum. While PC DAQ is suited to measure XTA data with closely spaced x-ray pulses (~10 ns) and a low count rate (<1 detected photon/pulse), CI DAQ works best for widely spaced pulses (tens of ns or greater) with a high count rate (>1 detected photon/pulse). XMP DAQ produces a two-dimensional XTA dataset, enabling efficient quantitative analysis of photophysical and photochemical processes from the sub-nanosecond timescale to 100 μs and longer.

47 OTHER INSTRUMENTATION↗
DOE OSTI2021

Preface to the JPCM special issue on intense radiation sources in condensed matter and materials physics

This special issue is designed to honour the contributions of our colleague Neville Greaves who was among the first to apply newly-available synchrotron x-ray techniques to study the synthesis, structures and properties of advanced materials [1, 2]. His wide ranging work on ceramics, glasses and nanomaterials was celebrated in a recent issue of the J. Non-Cryst. Solids [3]. Neville's contributions to synchrotron research, highlighted here, focussed on design and construction of new beamline capabilities and sample environments to probe materials under different physical and chemical conditions, integrating various techniques to obtain complementary data on structure and bonding. The innovative nature of his work is illustrated by his studies of liquids and glasses, where he incorporated aerodynamic levitation into these experimental techniques, using both synchrotron x-ray and neutron beams to probe the structural transformations and dynamics combined with molecular dynamics simulations to study atomic scale organisation. His work has had a major impact on fundamental condensed matter physics and chemistry as well as applied materials science; and in this issue, we present contributions from colleagues using and developing new experimental techniques at current and next-generation synchrotron, neutron and free-electron laser sources and in their own laboratories, that probe the fundamental physics, chemistry and functional properties of novel materials and processes.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2024

Synchrotron small-angle X-ray scattering technique for battery electrode study

Structure dependent stability is a concern for the achievement of high energy density electrode with long cycling lifetime, especially for alloying-type and conversion-type anodes. Substantial alterations in volume upon discharge-discharge process leads to particle pulverization and continuous consumption of electrolyte. Moreover, the nucleation and growth mechanism of Li 2 O and Li 2 S, which determines the rate performance of Li-O 2 and Li-S batteries, are still understudy. Microstructure characterization techniques have been applied to disclose the structural changes of active material at different charge/discharge states. Synchrotron small-angle X-ray scattering (SAXS) attracts considerable attention because of the high flux, high time resolution and nondestructive characteristics. In addition, SAXS patterns provide statistics structural information of electrode at micrometer scale. The commonly used coin cell with punched holes simplifies the application of in situ/operando SAXS measurement. Here, this review discusses the research about the SAXS technique in the characterization of electrode in different batteries.

25 ENERGY STORAGE↗
DOE OSTI2025

Multi-Analytical Investigation of Arsenical Transfer and Remediation on Nineteenth-Century Green Books

Books containing heavy metals, specifically nineteenth-century green arsenical books, have been identified at Northwestern University Libraries, raising health and safety concerns related to handling. Copper acetoarsenite pigments, such as emerald green, were detected on book covers, decorative page edges, labels, and other components using noninvasive analytical techniques including X-ray fluorescence (XRF), Raman spectroscopy, and Fourier-transform infrared (FTIR) spectroscopy. Further examination of selected volumes using synchrotron radiation (SR) techniques revealed pigment migration, degradation, and arsenic transfer to adjacent books. This paper expands on initial findings through two related experiments. The first explored the transfer of arsenic using mechanical friction; Staedtler Mars® white vinyl erasers rubbed on arsenical books generated crumbs which were analyzed via scanning electron microscopy–energy-dispersive X-ray spectroscopy (SEM-EDX). Results confirmed the transfer of arsenic, copper, and lead, with decorative page edges being particularly prone to shedding arsenic onto other materials. The second experiment tested remediation methods on a book contaminated by prolonged exposure to an arsenical neighbor. Surface cleaning using erasers and a vacuum removed flecks of pigment but did not eliminate non-chromophoric arsenic as confirmed by SR analyses, which highlights its presence either as a degradation product embedded within the paper or present in the paper as part of its production process. Findings demonstrate the acute toxicity risk posed by arsenical books and support the need for safe handling protocols. However, materials with only trace levels of arsenic embedded during production may pose a lower risk of transfer. Cross contamination beyond prolonged direct contact appears limited. These results highlight critical considerations for library preservation practices and future research on arsenic in historical materials.

arsenic↗