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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 37 records · Page 2

Manufacture aluminum alloy tube from powder with a single-step extrusion via ShAPE

Mechanical performance of aluminum in terms of strength, wear and corrosion resistance, especially high-temperature strength has been shown to improve with the addition of transition metal (TM) elements of Fe, Cr, and Ti. However, these feedstock materials occur as powders. As such, the traditional fabrication process is complex and expensive because it requires multiple procedures and consumes considerable energy. This study developed Shear Assisted Processing and Extrusion (ShAPE) as a single-step process that manufactures tubes directly from Al-TM powders obtained via gas atomization. Meter-long Al-TM alloy tubes are extruded from powders with different processing conditions. The ShAPE tubes have very low porosity and the average density is 2.94 kg/cm 3 , which is equal to or higher than parts fabricated by hot extrusion and sintering. The powder-to-tube fabrication process was revealed and discussed by examining the microstructural evolution. The Vickers hardness of ShAPE tubes ranges from 110 to 140 HV through wall thickness and at different extrusion speeds. The variation in hardness was correlated with the extent of refinement of intermetallics and attributed to the shear deformation per unit extrusion length. Energy cost analysis shows that ShAPE save ~60% energy compared to the conventional sintering and extrusion processes. Results indicate ShAPE is a low-cost, high-efficiency manufacturing process for producing tubes from metallic powders.

36 MATERIALS SCIENCE↗

Criticality Control Overpack Fire Testing (Phase III)

This report will describe the one test conducted during phase III of the Pipe Overpack Container (POC) test campaign, present preliminary results from these tests, and discuss implications for the Criticality Control Overpack (CCO). The goal of this test was to see if aerosol surrogate material inside the Criticality Control Container (CCC) gets released when the drum lid of the CCO comes off during a thirty-minute long, fully-engulfing, fire test. As expected from POC tests conducted in Phase I and II of this test campaign, the CCO drum lid is ejected about one minute after the drum is exposed to fully-engulfing flames. The remaining pressure inside the drum is high enough to eject the top plywood dunnage a considerable distance from the drum. Subsequently, most of the bottom plywood dunnage supporting the CCC burns off during and after the fire. High pressure buildup inside the CCC and inside two primary containers holding the surrogate powder also results in damage to the filter media of the CCC and the filter-house, thread attachment of the primary canisters. No discernable release of surrogate powder material was detected from the two primary containers when pre- and post-test average mass were compared. However, when the average masses are corrected to account for possible uncertainties in mass measurements, error overlap does not preclude the possibility that some surrogate powder mass may have been lost from these primary canisters. Still, post-test conditions of the secondary canisters enclosing these two primary canisters suggest it is very unlikely this mass loss would have escaped into the CCC.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Indirectly Detected DNP-Enhanced 17 O NMR Spectroscopy: Observation of Non-Protonated Near-Surface Oxygen at Naturally Abundant Silica and Silica-Alumina

Recent studies have shown that dynamic nuclear polarization (DNP) can be used to detect 17 O solid-state NMR spectra of naturally abundant samples within a reasonable experimental time. Observations using indirect DNP, which relies on 1 H mediation in transferring electron hyperpolarization to 17 O, are currently limited mostly to hydroxyls. Direct DNP schemes can hyperpolarize non-protonated oxygen near the radicals; however, they generally offer much lower signal enhancements. In this study, we demonstrate the detection of signals from non-protonated 17 O in materials containing silicon. The sensitivity boost that made the experiment possible originates from three sources: indirect DNP excitation of 29 Si via protons, indirect detection of 17 O through 29 Si nuclei using two-dimensional 29 Si{ 17 O} D-HMQC, and Carr-Purcell-Meiboom-Gill refocusing of 29 Si magnetization during acquisition. This 29 Si-detected scheme enabled, for the first time, 2D 17 O– 29 Si heteronuclear correlation spectroscopy in mesoporous silica and silica-alumina surfaces at natural abundance. In contrast to the silanols showing motion-averaged 17 O signals, the framework oxygens exhibit unperturbed powder patterns as unambiguous fingerprints of surface sites. Furthermore, along with hydroxyl oxygens, detection of these moieties will help in gaining more atomistic-scale insights into surface chemistry.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

The relationship between grain size distribution and ductile to brittle transition temperature in FeCrAl alloys

A FeCrAl (Fe12Cr6Al2Mo) alloy was prepared by two methods, (a) traditional wrought and (b) powder metallurgy (PM). Further, both alloys exhibited the same average grain size (~40 um), but the PM alloy displayed a wider grain size distribution. Charpy impact testing showed that the ductile to brittle transition temperature width is dependent on the grain size distribution width.

36 MATERIALS SCIENCE↗

Observation of a reduced-turbulence regime with boron powder injection in a stellarator

Abstract In state-of-the-art stellarators, turbulence is a major cause of the degradation of plasma confinement. To maximize confinement, which eventually determines the amount of nuclear fusion reactions, turbulent transport needs to be reduced. Here we report the observation of a confinement regime in a stellarator plasma that is characterized by increased confinement and reduced turbulent fluctuations. The transition to this regime is driven by the injection of submillimetric boron powder grains into the plasma. With the line-averaged electron density being kept constant, we observe a substantial increase of stored energy and electron and ion temperatures. At the same time, the amplitude of the plasma turbulent fluctuations is halved. While lower frequency fluctuations are damped, higher frequency modes in the range between 100 and 200 kHz are excited. We have observed this regime for different heating schemes, namely with both electron and ion cyclotron resonant radio frequencies and neutral beams, for both directions of the magnetic field and both hydrogen and deuterium plasmas.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Amorphous complexion-aided sintering enables scalable processing of bulk nanocrystalline Cu-Zr with high strength and compressive plasticity

Nanocrystalline alloys can have exceptional strengths, yet due to limited microstructural stability it is difficult to fabricate bulk pieces through traditional processing routes that retain nanosized grains. In this study, centimeter-sized Cu-Zr alloy pellets were fabricated via a simple and improved powder metallurgy processing route. Different consolidation temperatures and times were employed to investigate the effect of amorphous grain boundary complexions on densification and the resulting mechanical properties. Bulk compression tests were carried out, with the samples that were hot pressed at 900 °C for 10 h exhibiting an excellent combination of average yield strength of 722 ± 45 MPa and average failure strain of 25.3 ± 2.4 %. Furthermore, we find that a powder processing route which enables amorphous complexion-assisted sintering leads to samples that (1) reach full density without requiring quenching treatments or other complex processing, (2) demonstrate appreciable plasticity, and (3) have strength that competes with commercially available high-strength Cu alloys.

Bulk nanocrystalline alloy↗

Microstructure development and properties of micro-alloyed copper, Cu-0.3Zr-0.15Ag, produced by electron beam additive manufacturing

A micro-alloyed copper powder, Cu-0.3Zr-0.15Ag wt.%, was produced using gas atomization reaction synthesis. Zirconium was added to copper to sequester the oxygen present as copper oxide surface films on the powder particles. The as-received powders, as well as the intentionally oxidized powders were used to fabricate solid test articles by electron beam powder bed fusion additive manufacturing. Dense samples fabricated from as-received powder demonstrated nominal UTS, yield, and elongation values at 260 MPa, 150 MPa, and 34%, respectively. The average electrical conductivity of these samples was measured at 95% of the international annealed copper standard (IACS). Samples fabricated from the oxidized powder exhibited nominal UTS, yield, and elongation of 241 MPa, 146 MPa, and 43%, respectively, with an electrical conductivity of 95 % IACS. During characterization, it was observed that, rather than forming nano-scale dispersoids, the Zirconia (ZrO 2 ) appeared as discontinuous stringers in the metallographic cross-sections that crossed grain and melt pool boundaries. This was rationalized by tracing the presence of the micro-alloying addition of elemental zirconium, which was found to react with surface oxides dissociated in the melt pool to form ZrO 2 , which then solidified on the surface of the melt pool through an allotropic transformation to monoclinic ZrO 2 in discontinuous films and spheroids ranging in size from nanometers to microns. This was confirmed by microscopic analysis of the tops of the melt pools. On subsequent melt passes, these ZrO 2 structures were displaced and redistributed within the melt pool.

36 MATERIALS SCIENCE↗

Local structure elucidation of tungsten-substituted vanadium dioxide (V$$_{1-x}$$W$$_x$$O$$_2$$)

Abstract Initially, vanadium dioxide seems to be an ideal first-order phase transition case study due to its deceptively simple structure and composition, but upon closer inspection there are nuances to the driving mechanism of the metal-insulator transition (MIT) that are still unexplained. In this study, a local structure analysis across a bulk powder tungsten-substitution series is utilized to tease out the nuances of this first-order phase transition. A comparison of the average structure to the local structure using synchrotron x-ray diffraction and total scattering pair-distribution function methods, respectively, is discussed as well as comparison to bright field transmission electron microscopy imaging through a similar temperature-series as the local structure characterization. Extended x-ray absorption fine structure fitting of thin film data across the substitution-series is also presented and compared to bulk. Machine learning technique, non-negative matrix factorization, is applied to analyze the total scattering data. The bulk MIT is probed through magnetic susceptibility as well as differential scanning calorimetry. The findings indicate the local transition temperature ( $$T_c$$ T c ) is less than the average $$T_c$$ T c supporting the Peierls-Mott MIT mechanism, and demonstrate that in bulk powder and thin-films, increasing tungsten-substitution instigates local V-oxidation through the phase pathway VO $$_2\, \rightarrow$$ 2 → V $$_6$$ 6 O $$_{13} \, \rightarrow$$ 13 → V $$_2$$ 2 O $$_5$$ 5 .

Wilson, Catrina E. (ORCID:0000000173397318)↗

Soft-Chemical Synthesis, Structure Evolution, and Insulator-to-Metal Transition in Pyrochlore-like λ-RhO 2

λ-RhO 2 , a prototype 4d transition metal oxide, has been prepared by the oxidative delithiation of spinel LiRh 2 O 4 using ceric ammonium nitrate. Average-structure studies of this RhO 2 polytype, including synchrotron powder X-ray diffraction and electron diffraction, indicate the room-temperature structure to be tetragonal, in space group I4 1 /amd, with a first-order structural transition to cubic $Fd\bar{3}m$ at T = 345 K on warming. Synchrotron X-ray pair distribution function analysis and 7 Li solid-state nuclear magnetic resonance measurements suggest that the room-temperature structure displays local Rh-Rh bonding. The formation of these local dimers appears to be associated with a metal-to-insulator transition with a nonmagnetic ground state, as also supported by density functional theory-based electronic structure calculations. In conclusion, this contribution demonstrates the power of soft chemistry to kinetically stabilize a simple binary oxide compound.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Comparative Life Cycle Assessment of Injection Molded and Big Area Additive Manufactured NdFeB Bonded Permanent Magnets

Permanent magnets are expected to play a crucial role in the realization of the clean economy. In particular, the neodymium-iron-boron (Nd2Fe14B or NdFeB) magnets, which have the highest energy density among rare earth permanent magnets, are needed for building more efficient windmill generators, electric vehicle motors, etc. Currently, near-net shape magnets can be either made through sintering and compression molding with extensive post machining or directly through injection molding. However, injection molding has a loading volume fraction limitation of 0.65 for nylon binders. A novel method of manufacturing bonded permanent magnets with loading fraction greater than 0.65 has been demonstrated using Big Area Additive Manufacturing (BAAM) printers. As energy density is directly proportional to the square of the magnet loading fraction, magnets produced using BAAM printers require less volume and magnetic material compared to that of injection molded magnets on average. A comparative LCA shows that this difference in magnetic powder consumption nearly constitutes the difference in the environmental impact categories. Even after assuming recycled magnetic input, the BAAM magnets perform better environmentally than injection molded magnets, especially in the ozone depletion category. Since BAAM printers can accommodate even higher loading fractions, at scale, BAAM printers possibly can bring about a significant decrease in rare earth mineral consumption and environmental emissions. So furthermore, single screw extrusion enables BAAM printers to have high print speeds and allow them to be economically competitive against injection molding. Therefore, BAAM printed magnets show promise in transitioning towards the clean economy.

36 MATERIALS SCIENCE↗

Active Divertor Heat Flux Control using Impurity Powder Dropper

Divertor plasma-facing components (PFCs) in a tokamak are typically designed to withstand average steady-state heat loads of about 5–10 MW/m 2 , a limit that applies to both solid and liquid lithium (LL) PFCs. Exceeding these design values can result in surface damage to tungsten PFCs or excessive lithium (Li) evaporation in liquid lithium divertor (LLD) PFCs. Since exceeding the divertor heat load limits has serious consequences, it is therefore prudent to develop a tool to reduce the divertor heat load and bring the heat load to within the design limit without affecting the plasma performance. Active low Z impurity injection such as Li has been suggested as a potential solution to mitigate excess heat flux as suggested previously, given that non-coronal radiation can be quite large ~ 20–30 MJ per mole of injected Li. Li is considered desirable for reducing the edge neutral recycling helping to improve plasma energy confinement. In this paper, we model the Impurity Power Dropper (IPD) to investigate its potential of divertor heat flux control. The IPD is typically located at the top of the tokamak device and uses a vertical drift tube of a few meters. In the 2 m drift tube case, the IPD powder is accelerated to ~ 6 m/sec before reaching the plasma with the upper divertor configuration, matching the condition for the in-board side pellet injection case. By modeling the IPD geometry we determined the IPD powder deposition profile, and thus the non-coronal radiation and ionization profiles in time as well. From the enhanced radiation power loss, it is therefore possible to reduce the divertor heat load using the divertor simulation code. In conclusion, the IPD divertor heat flux control can be tested in the facilities with IPD including ST-40, DIII-D, EAST, WEST and NSTX-U.

Active lithium injection↗

X-ray Diffraction of Water in Polyvinylpyrrolidone

PVP is a hydrophilic polymer commonly used as an excipient in pharmaceutical formulations. Here we have performed time-resolved high-energy X-ray scattering experiments on pellets of PVP at different humidity conditions for 1-2 days. A two-phase exponential decay in water sorption is found with a peak in the differential pair distribution function at 2.85 Å, which is attributed to the average (hydrogen bonded) carbonyl oxygen-water oxygen distance. Additional scattering measurements on powders with fixed compositions ranging from 2 to 12.3 wt % H 2 O were modeled with Empirical Potential Structure Refinement (EPSR). Further, the models reveal approximately linear relations between the carbonyl oxygen-water oxygen coordination number (nO C - O W ) and the water oxygen-water oxygen coordination number (nO W - O W ) versus water content in PVP. A stronger preference for water-water hydrogen bonding over carbonyl-water bonding is found. At all the concentrations studied the majority of water molecules were found to be randomly isolated, but a wide distribution of coordination environments of water molecules is found within the PVP polymer strands at the highest concentrations. Overall, the EPSR models indicate a continuous evolution in structure versus water content with nO W - O W =1 occurring at similar to 12 wt % H 2 O, i.e., the composition where, on average, each watermolecule is surrounded by one other water molecule.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Observations of wall conditioning by means of boron powder injection in DIII-D H-mode plasmas

In this paper, we report observations from the DIII-D tokamak indicating that boron (B) powder injection in tokamak plasmas improves wall conditions similarly to glow discharge boronization (GDB). Isotopically enriched B powder (B 11 > 95%) was introduced gravitationally in a sequence of H-mode plasma discharges at rates up to ~160 mg s -1 for durations up to 3 s. Boron injection to cumulative amounts ≤0.1 g appeared to improve wall conditions similarly to boronization, with indications of reduced wall fueling, reduced recycling at the outer strike point and reduced impurity content at breakdown. Post-mortem analysis of graphite samples exposed to far scrape-off layer plasma fluxes during boron injection confirm the formation of a B-C layer, with average surface composition B:C ~ 1. The results suggest that injecting boron-rich powders in tokamak plasmas can effectively replenish boron films on carbon plasma facing components to improve wall conditions and extend the duration of the beneficial effects of GDB.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Infrared laser ablation of poly(vinylidene fluoride): The Loss of HF

The mechanism and kinetics of infrared laser ablation of poly(vinylidene fluoride) (PVDF) in vacuum have been investigated to understand how this can be used as a polymer processing technology. The laser heats the surface and initiates decomposition of macromolecules in the molten polymer layer which rapidly leads to production of an ablative flow of polymer decomposition products. There is only a short induction period of up to 2 s before ablation begins. After the initial period, the rate of mass loss increases linearly with the time of laser exposure. Spherical particles with an average diameter of about 100 nm are formed on the surface of the powder coating obtained by laser ablation. Here, the particle distribution ranges from 50 nm to 300 nm. The main gaseous product of ablation is HF from dehydrofluorination. A second important ablation process is the formation of gaseous carbenes generated during secondary reactions. Proposed ablation reactions due to laser-induced thermal dehydrofluorination occur in two stages. In the first stage, a double bond appears in PVDF due to direct loss of HF. Subsequent detachment of HF leads to the appearance of both triple bonds and cumulene bonds.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Excitation spectrum and low-temperature magnetism in the disordered defect-fluorite Ho2⁢Zr2⁢O7

In this work, we report on the thermomagnetic characterization and crystalline-electric field (CEF) energy scheme of the disordered defect-fluorite Ho2⁢Zr2⁢O7. This structural phase is distinguished by the coexistence of magnetic frustration and extensive disorder, with Ho3+ and Zr4+ sharing randomly the same 4⁢𝑎 site with even 50% occupancy, and an average 1/8 oxygen vacancy per unit cell. AC magnetic susceptibility measurements performed on powder samples down to 0.5 K revealed signs of slowing spin dynamics without glassy behavior, including a frequency dependent peak at ∼1K. Yet, no evidence for long-range magnetic order is found down to 200 mK in the specific heat. Inelastic neutron scattering measurements show a weak, low-lying CEF excitation around 2 meV, accompanied by a broad level centered at 60 meV. To fit our observations, we propose an approach to account for structural disorder in the crystal-field splitting of the non-Kramers Ho3+. Our model provides an explanation to the broadening of the high-energy, single-ion excitations and suggests that the zirconate ground-state wavefunction has zero magnetic moment. Through the breaking of local symmetry, structural disorder enables the magnetic response observed in Ho2⁢Zr2⁢O7, allowing the mixing of low-lying states at finite temperatures. Finally, we show that this scenario is in good agreement with the bulk properties reported in this work.

Gardner, Jason [ORNL] (ORCID:0000000278234072)↗