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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 433 records · Page 24
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Influence of mineralogical and chemical compositions on alkali-silica-reaction of Tennessee limestones

The paper aims to identify potential correlations between mineralogical and chemical compositions of AAR reactive dolomitic limestone aggregates from Tennessee and their expansion on ASTM C1293 for quick evaluation of reactivity. The chemical compositions of 26 limestones, namely the silica content (SiO 2 ), showed a strong correlation with the expansion in the concrete prism test. The early and highly expansive limestones are characterized by a high clay/ mica content (>5%). The reactivity of Tennessee limestones is mainly caused by crypto/microcrystalline quartz, chert, and finely disseminated silica in carbonate and clay/mica matrices, and it can be reasonably evaluated using X-ray diffraction and chemical analysis coupled with petrographic examinations.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Performance of biochar assisted catalysts during hydroprocessing of non-edible vegetable oil: Effect of transition metal source on catalytic activity

Biochar-supported catalysts were developed from nickel (Ni) - and cobalt (Co)- nitrates and hydroxides and tested for the hydrotreatment of carinata oil. Nitrate-based (from water-soluble salts) and hydroxide-based (from water-insoluble salts) catalysts of Ni and Co were prepared via wetness impregnation and aqueous dispersion methods, respectively. The catalysts were characterized using various tools such as, confocal XRF, BET specific surface area analyzer, NH3-TPD, and SEM-EDS. Synchroton method showed nitrate-sourced metals were dispersed mostly in the pores while, the hydroxide-sourced metals were distributed mainly on the catalyst surface. C = C saturation and cracking of triglycerides, decarboxylation, and hydrogenation of aromatic structures appeared to be dominant on the hydroxides of transition metals, hence took place on catalyst surface. Methanation and dehydrogenation (thus aromatization), however, seemed to be a pore phenomenon, catalyzed more over nitrate-based catalysts. A reaction network was proposed based on chemical analysis of upgraded carinata oil and erucic acid model compound. Catalytic cracking followed by hydrotreatment performed better in terms of fuel properties than other approaches in this study.

Biochar catalysts↗
DOE OSTI2025

Understanding the impacts of inorganic species in woody biomass for preprocessing and pyrolysis–A review

Woody biomass represents an abundant resource for sustainable biofuels, biochemicals, and bioproducts. Technologies for converting woody biomass have been established for decades, and research consistently highlights the critical role of inorganic species and ash plays in feedstock handling and conversion processes, including equipment plugging, corrosion, and catalyst deactivation. A thorough understanding of the variability, transport behavior, and downstream impact of inorganic species in woody biomass is essential for defining feedstock quality specifications and developing effective management strategies for conversion processes. This review compiles critical information in five main sections: 1) inorganic species concentration in woody biomass, based on anatomical fractions and their sources of variability; 2) technique features for quantifying inorganic elemental chemical analysis; 3) impacts of inorganic species on biomass preprocessing; 4) impacts of inorganic species on pyrolysis, and 5) mitigation strategies. Additionally, this review explores future challenges and opportunities in addressing the impacts of inorganic species on biomass quality. These insights aim to support the sustainable development of the biomass-to-bioenergy pipeline and ensure high-quality lignocellulosic feedstocks for efficient downstream conversions. The findings offer valuable guidance to policy makers, industry stakeholders, and researchers in developing effective strategies for managing inorganic species in woody biomass and fostering the sustainable processes for lignocellulosic biorefineries.

09 BIOMASS FUELS↗
DOE OSTI2023

The combined effects of Mg 2+ and Sr 2+ incorporation during CaCO 3 precipitation and crystal growth

Calcite (CaCO 3 ) composition and properties are defined by the chemical environment in which CaCO 3 forms. However, a complete understanding of the relationship between aqueous chemistry during calcite precipitation and resulting chemical and physical CaCO 3 properties remains elusive; therefore, we present an investigation into the coupled effects of divalent cations Sr 2+ and Mg 2+ on CaCO 3 precipitation and subsequent crystal growth. Through chemical analysis of the aqueous phases and microscopy of the resulting calcite phases in compliment with density functional theory calculations, we elucidate the relationship between crystal growth and the resulting composition (elemental and isotopic) of calcite. The results of this experimental and modeling work suggest that Mg 2+ and Sr 2+ have cation-specific impacts that inhibit calcite crystal growth, including: (1) Sr 2+ incorporates more readily into calcite than Mg 2+ (D Sr > D Mg ), and increasing [Sr 2+ ] t or [Mg 2+ ] t increases D Sr ; (2) the inclusion of Mg 2+ into structure leads to a reduction in the calcite unit cell volume, whereas Sr 2+ leads to an expansion; (3) the inclusion of both Mg 2+ and Sr 2+ results in a distribution of unit cell impacts based on the relative positions of the Sr 2+ and Mg 2+ in the lattice. These experiments were conducted at saturation indices of CaCO 3 of ~4.1, favoring rapid precipitation. This rapid precipitation resulted in observed Sr isotope fractionation confirming Sr isotopic fractionation is dependent upon the precipitation rate. We further note that the precipitation and growth of calcite favors the incorporation of the lighter 86 Sr isotope over the heavier 87 Sr isotope, regardless of the initial solution conditions, and the degree of fractionation increases with D Sr . In sum, these results demonstrate the impact of solution environment to influence the incorporation behavior and crystal growth behavior of calcite. These factors are important to understand in order to effectively use geochemical signatures resulting from calcite precipitation or dissolution to gain specific information.

58 GEOSCIENCES↗
DOE OSTI2025

Electrochemical recovery of Gd into liquid Bi in molten LiCl-KCl-GdCl 3

The electrochemical recovery of Gd into liquid Bi electrodes was investigated in molten LiCl-KCl-GdCl 3 electrolyte at 773–973 K using constant currents of 10–150 mA cm −2 . High round-trip coulombic efficiency (>97 %) was demonstrated for deposition and removal of Gd into and from liquid Bi at all temperatures, confirming chemically reversible electrode reactions towards high recovery yield of Gd using liquid Bi. Furthermore, the overpotential associated with deposition of Gd into the liquid Bi electrode gradually increased with current density and decreased with temperature. At the lowest temperature of 773 K, a steep increase in overpotential was evident at high current densities due to slower mass transport and low solubility of Gd in liquid Bi (0.5 at.% Gd). Based on the impedance spectra of Bi electrodes at 773–973 K, the exchange current density was estimated to be 110–220 mA cm −2 , indicating facile charge transfer at the liquid electrode-electrolyte interface. Post-mortem characterization of Bi cathodes after electrolysis at 873 K indicated the formation of a solid GdBi(s) compound layer at the Bi electrode surface. Chemical analysis of Bi cathodes at various deposited Gd compositions resulted in Faradaic efficiencies of ∼75–84 %, promising a high recovery yield of Gd from molten salts using a strongly-interacting liquid Bi electrode.

36 - MATERIALS SCIENCE↗
DOE OSTI2021

Synergic grain boundary segregation and precipitation in W- and W-Mo-containing high-entropy borides

The structures of W- and W-Mo-containing high-entropy borides (HEBs) are systematically studied by combining atomic-resolution transmission electron microscopy imaging, electron diffraction, and chemical analysis. Here, we reveal that W or W-Mo addition in HEBs leads to segregation of these elements to the grain boundaries (GBs). In the meantime, W- or W-Mo-rich precipitates also form along the GBs. Crystallographic analysis and atomic-scale imaging show that the GB precipitates in both W- and W-Mo-containing HEBs have a cube-on-cube orientation relationship with the matrix. With further strain analysis, the coherency of the precipitate/matrix interface is validated. Nanoindentation tests show that the simultaneous GB segregation and coherent precipitation, as a supplement to the grain hardening, provide additional hardening of the HEBs. Our work provides an in-depth understanding of the GB segregation and precipitation behaviors of HEBs. It suggests that GB engineering could be potentially used for optimizing the performance of high-entropy ceramics.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2021

Evolution of the structure and chemical composition of the interface between multi-component silicate glasses and yttria-stabilized zirconia after 40,000 h exposure in air at 800 °C

The chemical and structural stability of two commercial multicomponent silicate glasses (SCN and G6) in contact with yttria-stabilized zirconia (YSZ) was investigated after exposure times of up to 40,000 h in air at 800 °C. With exposure time, interfacial layers develop at the SCN-YSZ and G6-YSZ interfaces, which were characterized in detail using both quantitative chemical analysis and atomic-resolution imaging. At the SCN-YSZ interface, a Ca-Ba-Si-O reaction phase was found to grow by diffusion control. In G6-YSZ, Raman spectroscopy and electron microscopy revealed a disorganized interfacial reaction later between G6 and YSZ, and the occurrence of cubic to tetragonal to monoclinic phase transformations in YSZ. Finally, this microstructural evolution is discussed in terms of devitrification resistance of glass and diffusion processes at interfaces.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Structural investigation of the temperature-stable relaxor dielectric Ba 0.8 Ca 0.2 TiO 3 -Bi(Mg 0.5 Ti 0.5 )O 3

Aberration corrected scanning transmission electron microscopy (STEM) and electron diffraction have been used to disclose local structure and nano-chemistry in a Ca modified BaTiO 3 -Bi(Mg 0.5 Ti 0.5 )O 3 relax or dielectric ceramic which exhibits high and near-invariant relative permittivity over a wide temperature range. High resolution, synchrotron X-ray diffraction indicated a globally cubic structure ($Pm$$\overline{3}$$m$), but direct atomic-scale imaging by STEM revealed local tetragonal distortions. Nanopolar clusters were identified from B-site atomic displacement vectors measured relative to oxygen ion positions along < 100 > and < 110 > zone axes of integrated differential phase contrast (iDPC) STEM images, highlighting cluster sizes of 2–5 nm. Chemical analysis by STEM-energy dispersive X-ray spectroscopy and full pattern refinements of X-ray powder diffraction data each implied high levels of Bi vacancies within the matrix. The possibility that these A-site vacancies modulate the nanopolar structure and promote flattening of the permittivity-temperature response in this class of dielectric is discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Glass waste form options for rare-earth fission products from electrochemical reprocessing

Herein, we describe a first-of-a-kind study where lead tellurite (Pb-Te-O), iron phosphate (Fe-P-O), and lanthanide aluminoborosilicate (LABS) waste forms are evaluated for treating and/or immobilizing waste streams containing high rare-earth (RE) content, e.g., RECl 3 , REOCl, and/or REO x . Results from this study show that NdOCl can be immobilized in 78TeO 2 -22PbO glass at up to 10 mass%. Higher loadings of up to 15 mass% were demonstrated, but with a small fraction of crystallization. Two Fe-P-O glasses produced from either RECl 3 (RE = Nd,Ce) or NdOCl revealed products with very similar properties, demonstrating that the phosphate process can be used to chlorinate a variety of RE-containing waste streams. Two LABS glasses produced from Nd 2 O 3 or NdOCl showed similar properties, but the LABS-NdOCl glass did have some residual Cl present. Characterization is provided for all waste forms including chemical analysis, X-ray diffraction, and bulk density.

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

Development of small-scale plutonium electrorefining in molten CaCl 2

Molten salt extraction and electrorefining of plutonium were successfully conducted with only a 200-g initial charge. Due to this small scale, the electrorefining cell components were redesigned relative to conventional, multi-kg standards. The efficiency and yield of this small-scale process are comparable to those of larger-scale exemplars. Chemical analysis of the plutonium product and the anode heel is presented. Here, the product was 99.8% pure. The anode heel was able to be depleted beyond the expected freezing point without significant impurity carryover.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2022

Transmission Electron Microscopy based Characterization of a U-20Pu-10Zr Fuel Irradiated in Experimental Breeder Reactor-II

U-Pu-Zr metallic fuels are important fuel candidate for future advanced and/or test reactors. To better understand fuel performance and guide future fuel development, a U-20Pu-10Zr (in weight) metallic fuel irradiated in the Experimental Breeder Reactor was revisited using advanced electron microscopies. This fuel was irradiated to a burnup of 7.6 % at a peak cladding temperature of 521 °C. In this research, several transmission electron microscopy samples were extracted from different but representative radial locations of the fuel cross section using focused ion beam technique. Phase identification and chemical analysis with sub-micron spatial resolution was carried out using scanning transmission electron microscopy. Multiple phenomena that are critical to fuel performance, such as Zr phase and its distribution in a different matrix, were revealed in an unpreceded and highly detailed manner. An improved understanding of fuel reconstruction in U-Pu-Zr metallic fuel under reactor irradiation is provided.

36 MATERIALS SCIENCE↗
DOE OSTI2022

The complex structural and chemical nature of monolithic U-10Mo fuel and Zr barrier layer

Nanoscale microstructural characterization by advanced transmission electron microscopy techniques on a U-10Mo/Zr barrier layer monolithic fuel plate was performed to evaluate the microstructural evaluation after high burn-up. Gas bubble superlattice evolution, grain restructuring, and evolution of the Zr interaction layer is investigated through detailed electron microscopy characterization. The use of automated crystallographic orientation mapping to irradiated U-10Mo fuel highlights that the restructured ultra-fine grains are separated by high angle grain boundaries at a burn up of 4.42 × 10 21 fissions/cm 3 . Additionally, advanced chemical analysis and multi-variable statistical analysis shows spatial clustering of solid fission product precipitates. Finally, characterization of a newly observed porous nanocrystalline Zr region in the barrier layer is studied. Finally, this work provides insights into the grain subdivision and restructuring process while using advanced microscopy techniques to analyze fission products in neutron-irradiated U-10Mo fuel.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Compositional inhomogeneity and its effect on the hardness of nanostructured refractory high-entropy alloys

The pronounced compositional inhomogeneity observed in refractory high-entropy alloys (HEAs), as opposed to non-refractory HEAs, has an important influence on their mechanical properties, thereby posing a significant challenge for the development of high-performance refractory HEAs. In this work, by combining transmission electron microscopy imaging, chemical analysis, and nano-hardness tests, we investigate the compositional inhomogeneities in a series of sintered nanostructured HEAs and elucidate their influence on the material's hardness. Further, we reveal that the compositional inhomogeneity of the sintered nanostructured HEAs is temperature- and component- dependent. By correlating the hardness of nanostructured HEAs to the evolving compositional inhomogeneity, our work demonstrates that the compositional inhomogeneity in nanostructured HEAs can be tuned by sintering temperature or alloying towards optimized microstructure and hardness.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2023

Stable electrospray signal on a microfabricated glass chip with three-dimensional open edge and tiered depth geometries

This paper presents the microfabrication and performance of a three-dimensional electrospray ionization (ESI) emitter tip made from glass, which achieves stable current signals important for chemical analysis. Our novel microfabrication process and custom-built signal conditioning hardware provides the advantage of providing accurate features and steady signals. The fabrication process relies on standard microfabrication techniques (i.e., deposition, photolithography, and wet etching). This fabrication method involves the novel application of two layers of positive and negative photoresists in addition to Parafilm® wax tape. Open edge and tiered depth details were successfully created from a multilayer planar mask. This is a benefit for integrated miniaturized and microfluidic systems that often require micro features for their functionality but relatively large millimeter size features for their physical periphery. We demonstrate the fundamental performance of electrospray with this microfluidic chip. The emitter tip was fixed on a linear axis stage with high resolution (10 μm) to finely control the tip distance from a metal counter electrode plate. Further, a custom printed circuit board system was built to safely control four voltages applied to the microchip ports from a single high voltage power supply. To readily form the electrospray, non-aqueous solvents were used for their low viscosity and a constant voltage of +2.7 kV was applied to the sheath electrospray microchannel. The liquid being sprayed was 80/20 (v/v) methanol/acetonitrile with 0.1% acetic acid in the sheath microchannel and with ammonium acetate (10–40 mM) in its remaining microchannels. The electrospray signal was measured in response to varying the distance (1.4 to 1.6mm) between the electrospray emitter tip and a metal counter electrode plate in addition to the varying concentration of the background electrolyte, ammonium acetate. Stable and repeatable electrospray signal showed linear relationships with emitter tip distance and concentration (r 2 ≥ 0.95).

42 ENGINEERING↗
DOE OSTI2024

The interactivity of sources and dietary levels of resistant starches – impact on growth performance, starch, and nutrient digestibility, digesta oligosaccharides profile, cecal microbial metabolites, and indicators of gut health in broiler chickens

In a 21-d study, 480 Cobb 500 (off-sex) male broiler chicks were used to investigate the effects of feeding different sources and levels of resistant starches (RS) on growth performance, nutrient and energy utilization, and intestinal health in broiler chickens. The birds were allocated to 10 dietary treatments in a 3 × 3 + 1 factorial arrangement. The factors were 3 RS-sources (RSS): banana starch (BS), raw potato starch (RPS), and high-amylose corn starch (HCS); each at 3 levels (RSL) 25, 50, or 100 g/kg plus a corn-soybean meal control diet. Birds and feed were weighed on d 0, 8, and 21. On d 21, samples of jejunal tissue and digesta were collected for chemical analysis. Data were analyzed using the mixed model procedure of JMP with factor levels nested with the control. In the 0 to 21 phase, the birds fed the RPS diets had higher (P = 0.011) FI than those fed HCS or control diets, and FCR was greater (P = 0.030) in birds that received BS diets than in other diets. RSS × RSL was significant (P < 0.05) for total tract nutrient retention, AME, and AMEn on d 21. The starch digestibility was higher (P < 0.001) in birds that received the control diet than in RS diets, and decreased as RS levels increased, except for HCS. The apparent metabolizable energy (AME) and nitrogen-corrected AME (AMEn) were higher (P < 0.001) in birds fed 100 g/kg HCS diet, with both decreasing with increasing levels of BS and RPS, except for HCS. Relative ileal oligosaccharides profile showed significant (P < 0.05) RSS × RSL with a higher relative abundance of Hex(3) (P = 0.01) and Pent(3) (P = 0.001) in HCS diets. In conclusion, RS may influence gut health and growth performance in broiler chickens through modulation of cecal SCFA and nutrient digestion, but these depend largely on the botanical origin and concentrations of individual RS.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2022

Isolating intermediate Mg 11 Cu 6 Al 12 phase in ternary Mg-Cu-Al alloy by electrolytic dealloying

While dealloying is widely used to create nanoporous materials, it has rarely been employed to isolate difficult-to-synthesize intermediate phases. Here, in this work, we show how air-free, electrolytic dealloying at room temperature can be used to isolate the ternary intermetallic Mg 11 Cu 6 Al 12 phase. We create a ternary Mg-Cu-Al parent alloy containing the Mg 11 Cu 6 Al 12 compound and other phases, then subsequently remove these other phases via electrolytic dealloying to isolate the Mg 11 Cu 6 Al 12 phase. Isolated Mg 11 Cu 6 Al 12 phase exhibits ≈1 μm diameter rod-shaped microstructure. Phase and chemical analysis conducted using various techniques, including inductively coupled plasma and lab and synchrotron-based X-ray diffraction, show minimal impurities. This new approach to isolate the Mg 11 Cu 6 Al 12 phase can unlock its use in fundamental research and can be applied to other difficult-to-synthesize intermetallic compounds.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Discrepant wear behavior of carbon nanotubes (CNTs) and dispersant in four-ball unidirectional and ball-on-flat reciprocating sliding tests

Carbon nanotubes (CNTs), basically rolled graphene sheets, have been studied lately as oil additives in the literature. However, we observed discrepant impact of CNTs on wear protection from two common tribological tests, four-ball unidirectional sliding and high frequency reciprocating rig (HFRR) ball-on-flat reciprocating sliding. To gain a stable suspension and dispersion of the CNTs in the oil, the CNT surface was functionalized with a phenyl ligand and a dispersant, polyisobutylene succinimide (PIBSI), was added. In the four-ball test, PIBSI alone failed to protect the surface but the CNTs effectively reduced the wear loss. The observations in the HFRR test however were the opposite: the PIBSI alone provided strong wear reduction but the CNTs had no positive impact. Here, such a discrepancy was hypothetically attributed to the different wear protection mechanisms by the PIBSI and CNTs which responded distinctively under different testing conditions. Additional unidirectional and reciprocating sliding tests with matching Hertzian contact pressures were able to validate the hypothesis. Worn surface morphological examination and tribofilm chemical analysis further supported the proposed wear mechanisms. Fundamental understanding gained in this study provides insights into the potential benefits and limitations of using CNTs in lubrication.

36 MATERIALS SCIENCE↗