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DOE OSTI2022

Double Paddle‐Wheel Enhanced Sodium Ion Conduction in an Antiperovskite Solid Electrolyte

Abstract Antiperovskite structure compounds (X 3 AB, where X is an alkali cation and A and B are anions) have the potential for highly correlated motion between the cation and a cluster anion on the A or B site. This so‐called “paddle‐wheel” mechanism may be the basis for enhanced cation mobility in solid electrolytes. Through combined experiments and modeling, the first instance of a double paddle‐wheel mechanism, leading to fast sodium ion conduction in the antiperovskite Na 3− x O 1− x (NH 2 ) x (BH 4 ), is shown. As the concentration of amide (NH 2 − ) cluster anions is increased, large positive deviations in ionic conductivity above that predicted from a vacancy diffusion model are observed. Using electrochemical impedance spectroscopy, powder X‐ray diffraction, synchrotron X‐ray diffraction, neutron diffraction, ab initio molecular dynamics simulations, and NMR, the cluster anion rotational dynamics are characterized and it is found that cation mobility is influenced by the rotation of both NH 2 − and BH 4 − species, resulting in sodium ion conductivity a factor of 10 2 higher at x = 1 than expected for the vacancy mechanism alone. Generalization of this phenomenon to other compounds could accelerate fast ion conductor exploration and design.

25 ENERGY STORAGE↗

DOE OSTI2021

Hybrid of multi‐dimensional fillers for thermally enhanced polyamide 12 composites fabricated by selective laser sintering

Abstract Selective laser sintering (SLS) is an additive manufacturing technology that can provide a novel strategy to manufacture complex polymer‐based composites with tailored properties. In this study, polyamide 12 (PA12) composite powders based on Al 2 O 3 , boron nitride (BN), and carbon nanotubes (CNTs) were prepared via a two‐step mixing approach. Morphology characterization techniques indicated that the fillers were uniformly dispersed in the PA12 matrix as expected. Under the optimum 3D‐printing parameters, the fabrication of SLS parts with high filler loading could be obtained. With 40 wt% Al 2 O 3 , 8 wt% BN, and 2 wt% CNT hybrid fillers, the thermal conductivity of PA12 composites could reach 1.09 W/mK. It could be attributed to the synergistic effect of multi‐dimensional fillers to form dense and continuous thermal conduction paths. The factors influencing the performance of PA12 composites such as melting and crystallization behaviors, dielectric properties, and mechanical properties were also discussed. The results show that these composites have favorable dielectric and mechanical properties. Overall, the PA12 composites fabricated by SLS technology in this study exhibit excellent thermal management ability.

Yuan, Yue↗

DOE OSTI2019

Quantitative Analysis of Micro-structural Changes in a Bituminous Coal After Exposure to Supercritical CO{sub 2} and Water

High-volatile bituminous coal samples were reacted in deionized water with supercritical CO{sub 2} (ScCO{sub 2}–water) under simulated in situ pressure and temperature conditions (8 MPa and 40 °C) in unconfined stress state for 14 days, in order to characterize potential CO{sub 2}–water–coal reactions. Micro-structural changes were identified pre- and post-experiment using X-ray powder diffraction (XRD) analysis for powdered coal (mineralogical changes), optical microscopy and scanning electron microscopy (SEM) for polished thin sections (surface feature changes) and micro-CT scanning for a small core (porosity and permeability changes). XRD analysis revealed that carbonic acid leaches out mineral matters in coal, including carbonates (calcite) and silicate minerals (albite, illite and kaolinite). Optical microscopy, SEM and CT images confirmed that the interaction of coal with ScCO{sub 2}–water causes an abundance of micro-cracks to open or propagate in unconfined coal samples. Most micro-cracks preferably propagated along maceral–mineral and maceral–maceral interfaces, which demonstrates that the micro-cracking was caused by differential swelling of different coal lithotypes. Wormhole formation was observed in coal caused by mineral dissolution and hydrocarbon mobilization, which significantly increases coal porosity compared with swelling-induced cracking. 3-D pore network models extracted from CT images show that ScCO{sub 2}–water treatment enlarges the pore and throat size, increases the numbers of pores and throats and improves pore network connectivity. Overall, CO{sub 2}–water–coal interactions under unconfined conditions enhance coal porosity, connectivity and permeability, which can be attributed to the combined effect of micro-cracking, mineral dissolution and hydrocarbon mobilization.

58 GEOSCIENCES↗

DOE OSTI2019

Rare earth elements of fly ash from Wyoming's Powder River Basin coal

The advancement and increasing interests in green energy production and environmental protection technologies have spurred the demand for rare earth elements. On the other hand, the U.S. has to rely 100% on import of these materials as the industry was crashed because of the environmental issues associated with mining and processing, and more importantly lack competitiveness. As rare earth elements have many applications in defense and national security sectors, some of the elements were listed as strategic materials or critical materials because of the uncertainties in supply and prices. Therefore, it has become imperative in searching for alternative resources for supplying rare earth elements including unconventional resources. With the strong incentive, coal fly ash is identified as one of the candidates among them. In this study, we present rare earth element data for the 42 ash samples (all derived from Powder River Basin coal) that we collected from seven states (UT, WY, IO, WI, ND, CO, and MI) representing 158 million tons of fly ash. Overall, the results indicate scattered distributions of rare earth elements with concentration ranging from 156 to 590 ppm although all the ash samples originated from the same coal basin (Powder River Basin). The rare earth element resource in these ashes is estimated between 74000 and 106000 t. The ash samples were also characterized by elemental analysis, XRD, SEM-EDS and BET surface area. The characterizations of the ashes were discussed as they might have implications in the subsequent rare earth element extraction processes. In summary, fly ash may represent a potential resource for rare earth element production.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2021

Strain rate effects on the mechanical behavior of porous titanium with different pore sizes

High strain-rate (up to 6600 s –1 ) and quasi-static compression tests are conducted on a powder-sintered porous titanium with different pore sizes (mean: 30 μm and 120 μm). In situ X-ray imaging is implemented to characterize the pores-scale deformation dynamics. The yield strength as a function of strain rate exhibits two stages of rate sensitivity, and the transition occurs at 1600 s –1 . X-ray images show that pore compaction and strain localizations occur preferentially at pores oriented perpendicular to the loading direction under quasi-static loading, but become more random under high strain-rate loading as a result of higher driving force and plastic deformation nucleation rate. Here, the more homogeneous nucleation of plastic deformation contributes to the increased rate sensitivity beyond 1600 s –1 . At the same strain rate, the yield strength of porous Ti as well as strain field homogeneity decreases significantly with increasing pore size. The small pore spacing in fine-pored Ti reduces the degree of stress concentrations around pores. Therefore, the higher stress concentrations in coarse-pored Ti lead to an earlier yield of matrix around pores and thus a lower bulk yield strength.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Spatially Resolved Product Speciation during Struvite Synthesis from Magnesite (MgCO 3 ) Particles in Ammonium (NH 4 + ) and Phosphate (PO 4 3– ) Aqueous Solutions

While population growth necessitates a significant increase in crop production, stringent environmental regulations require that it be done using sustainable nutrient sources. Nutrients in the form of NH 4 + and PO 4 3– are recovered from wastewater streams via precipitation, using water-soluble magnesium ions to form sustainable, slow-release fertilizer, struvite (MgNH 4 PO 4 ·6H 2 O). Furthermore, the magnesium needed is mainly incorporated in the crystal lattices of very low-solubility minerals. This work utilizes a combination of powder X-ray diffraction (pXRD) and ex situ Raman and energy-dispersive X-ray spectroscopies combined with ion chromatography to characterize transformation products of low-solubility MgCO 3 particles in NH 4 + - and PO 4 3– - containing aqueous solutions with and without Ca 2+ ions present.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Chromium Poisoning Mitigation Strategy in Strontium-Doped Lanthanum Manganite-Based Air Electrodes in Solid Oxide Fuel Cells

Abstract Chromium poisoning of the air electrode remains an obstacle to the long-term performance of solid oxide fuel cells (SOFCs). In Sr-doped LaMnO3 (LSM) air electrodes, the poisoning process results in two types of deposits, chromium oxide (Cr2O3), and Mn, Cr spinel (MnCr2O4). The former forms electrochemically and the latter forms via a chemical reaction. By applying a small anodic reverse bias, Cr2O3 deposits can be removed because their formation is electrochemical in nature. However, MnCr2O4 deposits remain because their formation is chemical, rather than electrochemical, in nature. In situ chemical decomposition of the Mn, Cr spinel was investigated as an alternate removal method as thermodynamics supports its decomposition into constituent oxides below ∼540 °C in pure oxygen. The spinel decomposition process was characterized using thermogravimetric and X-ray diffraction analyses. The experimentally determined rate of spinel decomposition was undetectable (very slow) with isolated MnCr2O4 powders. The addition of 10 mol% gadolinia doped ceria (GDC) and silver powders significantly increased the rate of decomposition. However, the rate is limited by the diffusion of oxygen through the decomposed oxide layer. Although one strategy may be the addition of GDC and silver to the LSM air electrode to enhance spinel decomposition, the more effective mitigation strategy would be to prevent the formation of MnCr2O4 spinel in the first place through the removal of the reactants: Cr2O3 via electrochemical cleaning and mobile Mn ions in the zirconia electrolyte by incorporating a diffusion barrier layer such as GDC between the air electrode and electrolyte.

Electrochemistry↗

DOE OSTI2025

Manufacturing of Al-Ce/Metal-Matrix-Composites (MMC) for Harsh Environments

An integrated modeling/simulation and experimental approach will be used to design and synthesize Al-Ce/MMC for use in key technologies where improved energy efficiency and performance is harsh environments is required. Modeling and simulation work including thermodynamic modeling, DFT calculations, and continuum modeling of casting processes and mechanical behavior, will be combined with lab-scale synthesis to identify potential matrix and reinforcing phase compositions for large-scale synthesis. The experimental synthesis work will rely on lab-scale casting and gas atomization to identify the optimal matrix compositions for pilot/commercial-scale synthesis is Al-Ce/MMC. Selected Al-Ce/MMC will be synthesized by commercial scale melt processing, powder metallurgy and thermomechanical processing. The corrosion resistance, mechanical properties as a function of temperature, and thermal conductivity of the composites will be characterized to validate target properties are met or exceeded. This work will focus on two selected applications; however, the design framework will have broad applicability for composites for numerous harsh service condition applications. We will have synthesized Al-Ce/MMC that exhibit better performance in harsh environments than currently used materials.

36 MATERIALS SCIENCE↗

NASA NTRS1975

Effect of polymer properties and adherend surfaces on adhesion

The surface properties associated with good adhesive joints were evaluated in terms of application of adhesive bonding in aerospace technology. The physical and chemical nature was determined of Ti and Al adherend surfaces after various surface treatments, and the effects on fracture surfaces of high temperature aging, and variations in amide, anhydride, and solvent during polymer synthesis. The effects were characterized of (1) high temperature during shear strength testing, (2) fiber-reinforced composites as adherends, (3) acid/base nature of adherends, (4) aluminum powder adhesive filler, and (5) bonding pressure.

Dwight, D. W.↗

NASA NTRSDate not supplied

Al6061-RAM2 Development and Hot-Fire Testing using Additive Manufacturing Laser Powder Directed Energy Deposition for Liquid Rocket Engine Channel-Cooled Nozzles

Aluminum 6061-RAM2 is a high-strength aluminum feedstock developed for additive manufacturing (AM)processes. This alloy leverages Reactive Additive Manufacturing (RAM) technology. The RAM aluminum alloys were developed to be weldable—therefore printable—while equaling or exceeding strength properties of high strength wrought aluminum alloys. NASA and industry partners developed Laser Powder Directed Energy Deposition (LP-DED)additive manufacturing of Al6061-RAM2 for use in aerospace applications. Efforts included establishing build parameters, characterizing the alloy, fabricating components, and completing hot-fire testing of complex internal channel-cooled nozzles. These efforts are to address the growing need for large-scale parts using high-performance light-weight materials. Two rocket engine nozzles were fabricated using LP-DED Al6061-RAM2 that included integral cooling channels. The Al6061-RAM2 has completed process development and initial properties were established. This paper provides an overview of the LP-DED process development, material characterization and properties, component manufacturing, supplemental development, and hot-fire testing. Results from hot-fire testing are provided for a lander-class 31kN (7,000lbf)thrust engine using Liquid Oxygen (LOX)/Liquid Hydrogen(LH2) and LOX/Methane(LCH4).

Al6061-RAM2↗

NASA NTRSDate not supplied

Al6061-RAM2 Development and Hot-Fire Testing using Additive Manufacturing Laser Powder Directed Energy Deposition for Liquid Rocket Engine Channel-Cooled Nozzles

Al6061-RAM2↗

NASA NTRSDate not supplied

Al6061-RAM2 Development and Hot-Fire Testing using Additive Manufacturing Laser Powder Directed Energy Deposition for Liquid Rocket Engine Channel-Cooled Nozzles

Aluminum 6061-RAM2 is a high-strength aluminum feedstock developed for additive manufacturing (AM)processes. This alloy leverages Reactive Additive Manufacturing (RAM) technology. The RAM aluminum alloys were developed to be weldable—therefore printable—while equaling or exceeding strength properties of high strength wrought aluminum alloys. NASA and industry partners developed Laser Powder Directed Energy Deposition (LP-DED)additive manufacturing of Al6061-RAM2 for use in aerospace applications. Efforts included establishing build parameters, characterizing the alloy, fabricating components, and completing hot-fire testing of complex internal channel-cooled nozzles. These efforts are to address the growing need for large-scale parts using high-performance light-weight materials. Two rocket engine nozzles were fabricated using LP-DED Al6061-RAM2 that included integral cooling channels. The Al6061-RAM2 has completed process development and initial properties were established. This paper provides an overview of the LP-DED process development, material characterization and properties, component manufacturing, supplemental development, and hot-fire testing. Results from hot-fire testing are provided for a lander-class 31kN (7,000lbf) thrust engine using Liquid Oxygen (LOX)/Liquid Hydrogen (LH2) and LOX/Methane (LCH4).

Al6061-RAM2↗

DOE OSTI2022

Method and apparatus for real time, in situ sensing and characterization of roughness, geometrical shapes, geometrical structures, composition, defects, and temperature in three-dimensional manufacturing systems

Methods and apparatuses for manufacturing are disclosed, including (a) providing an apparatus having: a laser; scanner; powder injection system; powder spreading system; dichroic filter; imager-and-processor; and computer; (b) programming the computer with specifications of a sample; (c) using the computer to set initial parameters based on the sample specifications; (d) adjusting a stage to position the sample; (e) focusing and scanning electromagnetic radiation onto the sample while powder is concurrently injected onto the sample in order to deposit a layer; (f) capturing two-dimensional images of the sample and probing the sample to determine whether the deposited layer was manufactured per the specifications; (g) use the computer to adjust the three-dimensional manufacturing parameters based on the determination made in step (f) prior to additively manufacturing a subsequent layer or making repairs; and (h) repeating steps (d), (e), (f), and (g) until the manufacture is complete. Other embodiments are described and claimed.

Liu, Jian↗

NASA NTRS1998

Chemically Derived Dense Alumina-Zirconia Composites for Improved Mechanical and Wear Erosion Properties

As a result of this funded project high purity Zirconia-Toughened Alumina (ZTA) ceramic powders with and without yttria were produced using metal alkoxide precursors. ZTA ceramic powders with varying volume percents of zirconia were prepared (7, 15, and 22%). Aluminum tri-sec butoxide, zirconium propoxide, and yttrium isopropoxide were the reagents used. Synthesis conditions were varied to control the hydrolysis and the aging conditions for the sol to gel transition. FTIR analysis and rheological characterization were used to follow the structural evolution during the sol to gel transition. The greater extent of hydrolysis and the build-up of structure measured from viscoelastic properties were consistent. Heat treatment was conducted to produce submicron grain fully crystalline ZTA ceramic powders. This improved materials should have enhanced properties such strength, toughness, and wear resistance for advanced structural applications, for example engine components in high technology aerospace applications.

Source record↗

DOE OSTI2021

Copper-Tantalum Metal Matrix Composites Consolidated from Powder Blends by Severe Plastic Deformation

We investigated the effectiveness of severe plastic deformation by equal channel angular extrusion (ECAE) for consolidation of metal powders into metal matrix composites. Equal volumes of copper (Cu) and tantalum (Ta) powders were consolidated at ambient temperature via different ECAE routes. Composites processed by ECAE routes 4E and 4Bc were also processed at 300 °C. The resulting materials were characterized by scanning electron microscopy (SEM) and compression testing. Processing by route 4Bc at 300 °C resulted in the highest compressive strength, lowest anisotropy, and least strain rate sensitivity. We conclude that the superior properties achieved by this route arise from mechanical bonding due to interlocking Cu and Ta phases as well as enhanced metallurgical bonds from contact of pristine metal surfaces when the material is sheared along orthogonal planes.

36 MATERIALS SCIENCE↗

DOE OSTI2020

First impurity powder injection experiments in LHD

Injection of impurities in the form of sub-millimeter powder grains is performed for the first time in the Large Helical Device (LHD) plasma, employing the Impurity Powder Dropper (IPD) [A. Nagy et al., RSI 2018], developed and built by PPPL. Controlled amounts of boron (B) and boron nitride (BN) powder are injected into the helical plasma. Visible camera imaging, UV and charge exchange spectroscopy measurements show that the injected impurities effectively penetrate into the plasma in two different magnetic configurations.The prompt effects of the impurities on the plasma are characterized as the injection rate is scanned. The injected impurities provide a supplemental electron source, causing the plasma density to increase, together with the radiated power. Beneficial effects on the confined plasma temperature are observed at low plasma densities, due to an increased efficiency in NBI power absorption. For $n_{e,av}<10^{19}m^{-3}$ the powder grains penetrate deeper into the plasma, as they can be less effectively deflected by the plasma flow in the divertor leg, which they have to cross first as they are injected from the top of the machine.In this case, the created B ions are observed to move outwards from UV spectroscopy and charge exchange measurements, due to the outwards direction of the radial electric field. This makes low density plasmas a better candidate for powder boronization techniques.

Boron↗

DOE OSTI2019

Analysis of Powders Containing Illicit Drugs Using Magnetic Levitation

Magneto-Archimedes levitation (MagLev) enables the separation of powdered mixtures of illicit drugs (cocaine, methamphetamine, heroin, fentanyl, and its analogues), adulterants, and diluents based on density, and allows the presumptive identification of individual components. Small samples (mass <50 mg), with low concentrations of illicit drugs, present a particular challenge to analysis for forensic chemists. The MagLev device, a cuvette containing a solution of paramagnetic gadolinium(III) chelate in a non-polar solvent, placed between two like-poles-facing NdFeB magnets, allowed separation of seven relevant compounds simultaneously. In particular, initial separation with MagLev, followed by characterization by FTIR-ATR, enabled identification of fentanyl in a sample of fentanyl-laced heroin (1.3 wt % fentanyl, 2.6 wt % heroin, and 96.1 wt % lactose). MagLev allows identification of unknown powders in mixtures and enables confirmatory identification based on structure-specific techniques.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2018

Integrated Geologic Storage Prefeasibility Study Proximal to Dry Fork Power Station, Powder River Basin, Wyoming

The pre-feasibility study—funded by the Department of Energy CarbonSAFE program (DE-FE0029375)—is centred around Basin Electric’s Dry Fork Station (DFS) in Wyoming’s Powder River Basin. Dry Fork Station, completed in 2011, is a high efficient coal-fired power plant that emits 3.3 million tons of CO2 per annum. The DFS site also host’s the Wyoming Integrated Test Center (ITC) funded by a $15 million investment by the State of Wyoming. The ITC is a public-private partnership test bed for CCS technologies. Geologic storage sites are in immediate vicinity of the DFS providing significant opportunities for co-located source and saline storage. The Powder River Basin (PRB) of Wyoming and Montana, was identified by NETL (2010) as having a “high potential” for commercial-scale carbon sequestration. The basin contains as much as 17,000 feet of sedimentary rock and covers an area of approximately 24,000 square miles. The PRB has a long history of hydrocarbon production and remaining undiscovered reserves. Accumulations and production of hydrocarbons in the basin indicate the presence of reservoir formations with significant pore volumes and impermeable sealing formations. This attribute alone suggests the reservoir and seal characteristics of the formations provide significant opportunities for CO₂ storage in saline reservoirs. Four high quality potential reservoir and sealing complexes have been identified for geologic storage. These formations range in depth from 6,500-9,500 feet underneath DFS including: (1) the Pennsylvanian Minnelusa Formation reservoir and Permian Goose Egg Formation (Opeche Shale) seal; (2) the Jurassic Hulett and Canyon Springs Sandstones of the Sundance Formation sealed by the Late Jurassic Upper Sundance Member and Morrison Formation and (3) the Early Cretaceous Lakota and Dakota, and Muddy Formation reservoirs sealed by the Mowry Shale. The preliminary reservoir characterization results integrate data from petrophysical well logs, core measurements, faults/fractures analysis, artificial penetrations, and published literature to evaluate geologic storage capacity and potential risk, for the Powder River Basin. These reservoir and seal combinations reside within ideal depth constraints and show suitable reservoir and seal characteristics conducive to commercial-scale storage. Specifically, this paper presents 1) high level description of the geologic storage complex 2) a first order risk analysis associated with pre-existing oil and gas wells, and 3) preliminary storage capacity and Area of Review estimates.

Quillinan, Scott↗