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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 1,693 records · Page 94
All sourcesNASA NTRSDOE OSTI
DOE OSTI2016

Benchmarking of manganese oxide materials with CO oxidation as catalysts for low temperature selective oxidation

Here CO oxidation behavior of different manganese oxide materials was studied as a model probe reaction to benchmark catalytic activities that could be useful for other aerobic oxidations. K-OMS-2, which showed intermediate activity [Ea = 3.0 and 6.3 kcal/mol for K-OMS-2 (made in solvent free procedure or SF) and K-OMS-2 (made via hydrothermal route or REF) respectively], were chosen for metal dopant studies using microwave assisted hydrothermal synthesis. These were further characterized using X-ray diffraction (XRD), N 2 sorption, Raman spectroscopy, scanning electron microscopy (SEM), and carbon monoxide temperature programmed reduction (CO-TPR). Additional characterization was carried out for Ni-K-OMS-2 materials using atomic absorption spectroscopy (AAS) and thermogravimetric analysis-mass spectroscopy (TGA-MS). Doping K-OMS-2 with Ni resulted in a large increase in oxygen mobility and re-adsorption, and the moderate activation energy for CO oxidation (13. kcal/mol) by Ni-K-OMS-2(SF) suggests that Ni-doped materials are good candidates for low temperature selective oxidation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Electrocatalytic benchmarking of ruthenium-based bimetallic anodes for the electrocatalytic oxidation of biomass-derived wastewater

In this paper, we report on the synthesis, characterization, and use of ruthenium oxide (RuO 2 ) doped with a secondary metal (M2) to enhance electrochemical activity and stability for the electrocatalytic oxidation (ECO) of biomass-derived wastewaters. We used different electrochemical methods such as cyclic voltammetry (CV), electrochemical surface area (ECSA), and Tafel analysis as well as physical characterization such as grazing incidence X-ray diffraction, X-ray photoelectron spectroscopy, and scanning electron microscopy to understand how the introduction of M2 affects electrochemical performance. Our results show that including an M2 improves the ECO performance regardless of the composition of the electrolyte. Specifically, we saw increase in ECSA, which could be due to enhanced charge transfer for the pH ranges evaluated. Furthermore, the introduction of organic compounds in wastewater generated during the hydrothermal liquefaction of food waste affected the ECO performance differently, depending on M2, the electrolyte composition, and anodic half-cell potential, highlighting the need to properly control the reaction conditions when testing and characterizing the electrocatalysts under different reaction regimes. We developed an in situ electrocatalytic benchmarking protocol, Boruah – Lopez-Ruiz – Strange (BLoRS), to quickly assess if the presence of M2 improves the ECO performance; thus, saving time and resources in ex situ characterization, testing, and product analysis. This foundational work provides the basis for characterization and benchmarking of electrodes of the ECO of organic compounds.

Electrocatalysis↗
DOE OSTI2021

Nanostructural evolution of Al(OH)3 gel formed by the cubic and orthorhombic ye'elimite clinkers of calcium sulfoaluminate cements in an ultra-wide hydration temperature range

This paper investigated the influence of hydration temperature on the nanostructure of the AH{sub 3} phase formed in calcium sulfoaluminate cements. Orthorhombic ye'elimite (st-ye'elimite) and cubic ye'elimite (ss-ye'elimite) were hydrated in an ultra-wide temperature range (5–220 °C). Results showed that the AH{sub 3} phase formed by ss-ye'elimite was always microcrystalline in nature at various curing temperatures (5–130 °C), and transformed into the AlOOH phase at 150 °C and above. However, the AH{sub 3} phase formed by st-ye'elimite grew from a microcrystal to a favorable crystal as the temperature increased, and transformed into the AlOOH phase at 170 °C and above. The nanostructure of hydration products was further investigated using TEM/SAED analysis together with FE-SEM images, directly evidencing that the formed AFm-12 phase was single-crystal in nature, and the formed AH{sub 3} phase was microcrystalline at low temperatures and grew into single-crystal hexagonal prisms with the preferred growth direction along [001] direction at high temperatures.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Microstructural diversity and digestion yields of select bituminous and subbituminous coals as raw material candidates for carbon fiber precursor production

Here, this work investigates the use of coals as raw materials for carbon fiber precursor production as a new alternative to coal utilization. Coal being a highly complex and heterogeneous material with different macerals and minerals complicates this task. Extensive microstructural characterization as well as preliminary digestion studies are performed on three bituminous coals (Herrin and Springfield from the Illinois Basin and the Blue Gem from the Central Appalachians) and one subbituminous coal from the Powder River Basin (Monarch), as raw material candidates. The subbituminous coal was richer in oxygen, lower in sulfur, and had a higher volatile matter yield. Microstructural investigations were performed using X-ray diffraction, X-ray/neutron computed tomography, scanning electron microscopy with energy dispersive spectroscopy, and petrology. Mild solvent extraction studies were conducted using creosote and decant oil as solvents in microreactors. The extraction yield was sensitive to temperature and time (350 to 450 °C between 30 and 120 mins.) for both creosote and decant oil digestions. While the Blue Gem coal had more desirable microstructural properties with less mineral content and cleaner macerals, it had the lowest coal conversion to quinoline soluble ‘liquid’ (of the bituminous coals). The lower coal conversion yield was hypothesized to be connected to the lack of FeS2 which could act as a catalyst when Fe is liberated from the structure under solvent extraction conditions. The Herrin and Springfield coals revealed similar microstructures and coal conversion efficiencies (higher than Blue Gem). These coals were the most promising candidates for further examination from this first approximations study. The subbituminous Monarch coal, however, was deemed less suitable due to poor coal conversion and less desirable microstructures. Additionally, the presented results with combined microstructural data from multiple length scales established a framework necessary for a first approximations study in this new coal utilization approach.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2021

Facet-specific oxidation of Mn(II) and heterogeneous growth of manganese (oxyhydr)oxides on hematite nanoparticles

It is recognized that different facets of minerals vary distinctively in their chemical reactivity with aqueous solutions. However, detailed molecular and atomistic understandings of these phenomena are relatively limited. This study investigated the interaction of aqueous Mn2+ and dissolved oxygen on various facets of two morphology-types of iron oxide (hematite) nanocrystals. These interactions result in the oxidation of manganese and the heterogeneous nucleation and growth of Mn(II)/Mn(III), and Mn(III) oxides. The nanoscale morphology and atomic structure of the manganese oxide products were characterized in detail. Our results, for the first time, directly demonstrate the facet-dependent oxidation of Mn 2+ and nucleation of Mn(II/III) oxides, followed by their epitaxial growth on hematite. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), and electron diffraction measurements reveal the growth of MnOx nanowires on {012} facets of both hematite nanoplates (HNP) and hematite nanocubes (HNC), while the basal {001} facets on the HNP particles do not produce precipitates. The average oxidation state of the MnO x on HNP and HNC determined using electron energy-loss spectroscopy (EELS) show that both Mn(II) and Mn(III) are present. The facet-dependent oxidation of Mn 2+ may be attributed to adsorption-induced electron transfer (ET), and hematite {001} facets generally exhibiting weaker ability in the uptake of ions relative to {012} facets, and the bulk ET from {012} to {001} facets through the conduction band of hematite. Nevertheless, the mineral composition and growth mechanisms of MnOx catalyzed by HNP and HNC are similar. High-resolution TEM analysis reveals the presence of both hausmannite and manganite on HNP and HNC. The nanoscale observations and thermodynamic considerations indicate that the growth mechanisms/processes of MnO x include heterogeneous nucleation of hausmannite nanoparticles, crystallization by particle attachment, transformation from hausmannite to manganite, and self-catalyzed MnO x growth. It is possible that all of these processes are concurrent. The crystallographic relationship between the heterogeneously formed manganite with hematite, which has not been reported before, proves that hematite provides reaction sites and functions as an atomic template for the formation of MnO x nanowires. These findings advance our understanding of the redox chemistry and heterogeneous growth of minerals as controlled by the surficial structure of the substrate mineral. This has important geochemical implications as the catalytic growth of less common, highly reactive phases like MnO x are known to be consequential in complex natural and anthropogenic environments.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Cold Spray Deposition of 304L Stainless Steel to Mitigate Chloride-Induced Stress Corrosion Cracking in Canisters for Used Nuclear Fuel Storage

A feasibility study of the cold spray deposition process of 304L stainless steel on 304L stainless steel substrates as a mitigation method for chloride-induced stress corrosion cracking (CISCC) has been investigated under various substrate conditions. The study is aimed at the application of this technology to mitigate CISCC that may potentially occur in or nearthe fusion welded regions of stainless steel canisters in Dry Cask Storage System (DCSS) for used nuclear fuels. Spherical gas-atomized 304L stainless steel powder, in the size range of 25 µm to 44 µm, was used as a feedstock powder for the cold spray process. The powder was deposited on four types of 304L substrates with various surface conditions: as-polished, oxidized, cold-rolled, plates with prototypical CISCC. The effects of cold spray parameters on quality of cold spray coatings were investigated. Thickness, porosity, and phases in the as-deposited materials were evaluated using scanning electron microscopy (SEM) and X-ray diffraction (XRD), and correlated with microhardness and adhesion strength measured via micro-indentation and ASTM C633 pulling test, respectively. XRD analysis of the coatings was also conducted to examine the effects of cold spray condition on residual stress state in the coating. Detailed cross-sectional examination of coating/substrate interfaces was performed with transmission electron microscopy (TEM) equipped with energy dispersive spectroscopy (EDS). Dense and continuous coatings with good adhesion strength and hardness were produced for the various substrate conditions by adjusting cold spray parameters. The results demonstrate that cold spray stainless steel coating is a viable option to provide a physical barrier against CISCC in fusion weld regions of stainless steel in corrosive chloride salt-bearing environments.

Dry Cask Storage Systems, cold spray, 304L stainle↗
DOE OSTI2021

Evolution of Microstructure and Surface Characteristics of FeCrAl alloys when Subjected to Flow Boiling Testing

FeCrAl alloys are candidate materials for manufacturing accident-tolerant fuel (ATF) cladding intended for light water reactors to increase fuel reliability and safety during design-basis and beyond-design-basis accident scenarios. The evolution of the materials' surface characteristics, microstructure, and mechanical properties when exposed to the Critical Heat Flux (CHF) in flow boiling testing is crucial for safety analysis while providing insights into their thermal-hydraulic performance in nuclear reactors. After CHF, the surface chemistry of two FeCrAl alloys, APMT and C26M, was studied to understand their evolution at the early stage of high-temperature excursions in short time periods. The results indicated a thin layer composed of oxides and hydroxides of Al, Cr, and Fe with varying proportions at different depths in the layer, as indicated by X-ray photoelectron spectroscopy (XPS) and depth profiling. The cross-sections prepared by focused ion beam (FIB) revealed the growth of an oxide layer, in the range of 90-180 nm thick, on the alloys' surfaces. The evolution of the materials' surface chemistry also led to a noticeable post CHF excursion increase in their wettability, with a slight increase in roughness. Further, the investigation of the materials' mechanical properties indicated a modest increase in hardness by 10-15% as well as an increase in their yield strength, as evidenced by the microindentation and ring compression tests conducted before and after CHF testing. Scanning electron Microscopy (SEM) and X-ray diffraction (XRD) were used to investigate microstructural features of the materials and their changes after CHF treatment.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Thickness and microstructure characterization of TGO in thermal barrier coatings by 3D reconstruction

Yttria-stabilized zirconia (YSZ) thermal barrier coatings (TBCs) are prepared by plasma spraying. Thermally grown oxide (TGO) would be formed between YSZ topcoat and bond coat after 50 h thermal service for YSZ TBCs. The electron back scattered diffraction (EBSD) results reveal that the TGO layer is composed of α-Al{sub 2}O{sub 3} and cubic Al{sub 2}NiO{sub 4} layers. Measured values of TGO thickness from the 2D-SEM image are greater than or equal to its real thickness due to the fact that the TGO layer is much rolling so that up and down surfaces of the TGO can't be completely perpendicular to the cross-section direction confirmed by 3D-SEM. Furthermore, 3D-SEM results reveal that the real thickness of TGO layer is 3.10 μm instead of 7.1 μm. In addition, 3D-EBSD confirmed that α-Al{sub 2}O{sub 3} layer in TGO is composed of single layer of grains and Al{sub 2}NiO{sub 4} layer consist of multilayer of grains while α-Al{sub 2}O{sub 3} layer is mixed with single layer and multilayer of α-Al{sub 2}O{sub 3} grains from observation of the 2D-EBSD image. It provides a new method to characterize real thickness and microstructure of TGO, which is also applied to other film materials. - Highlights: •This work provides a new method to measure the real thickness of TGO. •YSZ TBCs were prepared by plasma spraying. •TGO is formed in TBCs by simulating thermal service at 1100 °C for 50 h. •Real thickness and microstructure of TGO were investigated by 3D reconstruction.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Particle stimulated nucleation during dynamic and metadynamic recrystallisation of Ni-30%Fe-Nb-C alloy

For the first time, a combination of scanning transmission electron microscopy and electron back-scattering diffraction is used to elucidate the early stages of particle stimulated recrystallisation at Nb carbides in Ni-30wt.%Fe alloy subjected to high temperature plane strain compression. While particles with sizes even below 1 μm were found to induce dynamic or metadynamic recrystallisation, only a small fraction of coarse particles served as nucleation sites. - Highlights: • The early stages of particle stimulated recrystallisation at Nb carbides are elucidated • A combination of transmission electron microscopy and electron back scattering diffraction used • Particles below 1 μm size could induce dynamic or metadynamic recrystallization.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructure control to improve creep strength of alumina-forming austenitic heat-resistant steel by pre-strain

Highlights: • The effect of pre-strain on creep strength of AFA steel was studied. • The creep test was performed at 700°C and 200Mpa, and the aging test was carried out using box furnace at 700°C to simulate the microstructural evolution during creep. • Microstuctural evolution was observed by using SEM, EBSD, and TEM to investigate the relationship between creep strength and microstructure. - Abstract: At 700 °C and 200 MPa, the creep rupture time of W-containing alumina-forming austenitic heat-resistant (WAFA) steel increases from 1044 to 3119 h by pre-strain. Pre-strain introduces a lot of dislocation into the matrix and most of the dislocations remain stable to the end of creep without recovery and recrystallization. In addition, the dislocations have enabled secondary NbC and Laves phase to be uniformly distributed and refined. However, the dislocations lower grain boundary strength due to the coarsening of precipitates along grain boundaries Therefore, the increase in the creep rupture time in spite of deterioration of grain boundary strength is attributed to the dislocation strengthening and enhanced precipitation hardening within grains.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Formation of intermetallic structures at the interface of steel-to-aluminium explosive welds

Highlights: • The interface of Fe-Al explosive welds was characterised by SEM/EDS and EBSD. • The intermetallics formed at the weld interface are rich in Al (Fe{sub 4}Al{sub 13}, Fe{sub 2}Al{sub 5}). • The presence of intermetallic phases on the interface deeply affects the weldability. • Al-rich intermetallics increase the solidification time of the weld interface. - Abstract: The formation of intermetallic structures at the interface of carbon steel to 6082 aluminium alloy explosive welds and their influence on the weldability of these two materials were studied. The morphology, the microstructure, the chemical and phase compositions of the welds were characterised by several types of microscopy techniques. The interface characterisation proved that explosive mixtures with a lower detonation velocity were revealed as being more suitable for achieving consistent welds since jet entrapment was prevented and continuous molten layers were not formed at the weld interface. It was also found that the physical properties of the intermetallic phases generated at the weld interface have a strong influence on the weldability of steel-to-aluminium explosive welds. Specifically, it was shown that the formation of aluminium-rich intermetallic phases at the weld interface increases the solidification time of the interfacial molten material, decreasing the weldability of these two materials. The formation of these intermetallic compounds should be avoided by reducing the interaction between the flyer and the baseplate as well as by avoiding excessive molten layers.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Effect of filling materials on the microstructure and properties of hybrid laser welded Al-Mg-Si alloys joints

Highlights: • A serious comparison was made on the hybrid laser welded AA6061-T6 joint with different filling materials. • The microstructure of the welded joint was characterized using EBSD and SEM. • A strength model was successfully built to predict the strength of the hybrid laser welded AA6061-t6 joint. • The study shed new insights on how to select appropriate filling materials when using hybrid laser welding. - Abstract: A serious investigation was conducted to examine the influence of filling materials on the microstructure and properties of hybrid laser welded AA6061-T6 joints. The results of the tensile tests showed that the welded joint with ER4043 filling materials had higher tensile strength than that with ER5356 filling material. Based on the results obtained a strength model was built to predict and explain the enhancement of the yield strength of the hybrid laser welded AA6061-T6 joint with different welding wires. In contrast to the tensile strength, the ER4043 joint showed lower fatigue strength than that of the ER5356 joint due to extensive presence of micropores in fusion zone. Further, the corrosion experiment illustrated that the ER4043 joint had poorer resistance to the corrosive attack under 3.5% NaCl solution. A summary was made on the performance of both welded joints to shed new insights on selecting appropriate filling materials when welding AA6061-T6 by hybrid laser welding method.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Advanced processing of EBSD data to distinguish the complex microstructure evolution of a Cu-Ni-Si alloy induced by fatigue

Highlights: • Microstructure investigation of the fatigue behaviour of a Cu-Ni-Si alloy • Use of ECCI and EBSD to investigate the microstructure evolution related to fatigue dislocations structures • Characterisation of local plastic accommodation through EBSD misorientation criteria - Abstract: The present work aims at identifying the evolution of the microstructure of a Cu-Ni-Si (Corson alloy) alloy after low cycle fatigue by means of advanced electron microscopy analysis techniques (SEM-ECCI, Orientation Imaging Microscopy by means of SEM-EBSD and TEM). Deep attention is paid on the material subjected to high cyclic strains where a transient cellular dislocation structure transformed into precipitate free bands. It is shown that the formation of dislocation cells leads to a high GROD and high GOSaera value and its standard deviation. However, the presence of precipitate free bands results in the low GOSarea level and its low standard deviation.

36 MATERIALS SCIENCE↗
DOE OSTI2020

XRD and SEM/EDS characterization of two quaternary fuel alloys (U-2.5Mo-2.5Ti-5.0Zr and U-1.5Mo-1.5Ti-7.0Zr in wt. %) for fast reactors

The current study focuses on characterization of two potential fuel alloys for sodium-cooled fast reactors: U-2.5Mo-2.5Ti-5.0Zr (U-MT5Z) and U-1.5Mo-1.5Ti-7.0Zr (U-MT7Z) in wt. %. As-cast alloys and annealed (600°C, 500h) alloys are studied by X-ray powder diffraction (XRD) for their bulk structures, and scanning electron microscopy / energy dispersive X-Ray spectroscopy (SEM/EDS) for their microstructures and phase constituents. For as-cast alloys, the XRD results show that U-MT5Z mainly contains γ, while U-MT7Z alloy contains a. In both alloys, there are three phases indicated by EDS, a U-rich phase, secondary phase, and Zr-rich phase. Further, the elemental compositions varied in different phases and in different alloys. After annealing, both alloys exhibit the structures of α-U and U 2 Ti according to XRD. The EDS results suggest there are five phases found in both alloys.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2020

Coupling computational thermodynamics with density-function-theory based calculations to design L12 precipitates in Fe Ni based alloys

Achieving a high-volume fraction of thermodynamically stable L12-type precipitates that are resistant to coarsening is of great importance for the development of low-cost FeNi based austenitic steels. With the aid of computational thermodynamics, this work designed two model alloys: Fe-37.4Ni-6.1Al-2.9Ti (FNAT) and Fe-45.2Ni-5.9Al-8.5Si (FNAS). Both alloys were designed to contain a similar amount of L1 2 precipitate in Fe-Ni matrix without forming other precipitates. Density-Function-Theory (DFT) calculation was coupled with computational thermodynamics to predict the critical radius at which the precipitates change shape from spherical to cuboidal. The calculation results suggest that critical radius for the FNAT alloy is about two orders of magnitude larger than that for the FeNiAlSi alloy. Phase stability and morphology of the L1 2 precipitates in these two alloys were experimentally investigated through X-ray diffraction, atom probe tomography, and scanning and transmission electron microscopy. The L1 2 precipitates in the FeNiAlSi system were found to be cuboidal and rod shaped, with much larger size than the spherical ones in the FeNiAlTi system, agreeing with the calculation results. This work suggested that coupling computational thermodynamics with DFT calculations can be reliably used to design L1 2 precipitates in FeNi based alloys.

36 MATERIALS SCIENCE↗