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At least 91 records · Page 5

Assessment of Gaseous Helium Cooling in a Superconducting Coil Test Rig

An experimental rig was designed and constructed at the NASA Glenn Research Center to measure the alternating current (AC) losses of round, multifilament, superconducting (SC), magnesium diboride (MgB2) wire in the temperature range from 20 to 30 K. The rig resembles a permanent magnet (PM) motor with the stator windings omitted. Experiment packs containing the superconductor samples will be placed in the annular space between the rotor and the stator back iron. The original plan was to measure the AC losses by calorimetry using nonboiling liquid hydrogen as the cooling fluid. The present plan is to use helium gas (GHe) under a few bar pressure instead. This report summarizes the calculations that indicate that reasonable results can be obtained, even though the mass density of the GHe will be only a fraction of that of liquid hydrogen. It is necessary to show that the heat transfer coefficient from SC wire to GHe can be high enough, that the temperature rise of the He between the experiment inlet and outlet can be small enough, and that sufficient He flow can be driven by a commercially available He fan. Both straight wire samples to validate loss models and coils to simulate motor stator coils can be tested in the rig. The lowest superconductor temperature that is feasible to reach in the rig is estimated. The temperature range available for samples will be wider with the gaseous He system than it would have been with liquid hydrogen.

supeconductors↗

Data-driven discovery of a formation prediction rule on high-entropy ceramics

The interest in high entropy ceramics (HECs) has increased steadily due to their superior properties. However, the prediction of their formation still poses challenges for the discovery of new systems. Here, we discover a rational rule for designing single-phase high entropy metal diborides (HEBs) using data-driven approach. The machine learning (ML) model is trained on data collected via high-throughput experiments (HTEs). K nearest neighbor (KNN) model shows an experimental validation accuracy of 93.75%. By implementing interpretable ML method, we demonstrate that a mismatch of the bonds between boron and transition metals (δ B-TM ) dominates the formation of HEBs. We propose an empirical rule that HEBs favor forming a single phase when δ B-TM < 3.66; otherwise, multiphase. The rule has a high accuracy of 93.33% for new HEBs predictions. In addition, we contribute 165 high quality HEBs data in total, which can promote the development of materials informatics in HEBs. Furthermore, this data-driven strategy can be expanded to accelerate the search for new HECs, paving a pathway to design novel HECs with superior properties rapidly.

36 MATERIALS SCIENCE↗

Response of 11 B enriched ZrB 2 ultra-high temperature ceramic to neutron irradiation at elevated temperatures

ZrB 2 , an ultra-high temperature ceramic (UHTC) is being considered for use in fusion reactor first-wall structures, yet its response to irradiation remains poorly understood. This study employed scanning/transmission electron microscopy (S/TEM), synchrotron X-ray diffraction (XRD), finite element calculations, and thermal property measurements to thoroughly investigate the neutron-irradiation effects on 11 B-enriched ZrB 2 . Neutron irradiations were conducted at 220 °C and 620 °C, with a neutron fluence of 2.2 × 10 25 neutron/m 2 (energy > 0.1 MeV), resulting in 3.9 dpa and 4200 appm He. The study revealed the unusual prevalence of prism loops and a > c anisotropic lattice swelling, likely linked to the low c/a ratio of ZrB 2 , leading to grain boundary microcracking. Reducing the grain sizes was effective in reducing intergranular cracking and macroscopic swelling. The observation of cavities in ZrB 2 irradiated at 620 °C, as opposed to 220 °C, prompts questions about the temperature at which vacancies in ZrB 2 become mobile, and the role of neutron absorption by 10 B in elevating irradiation temperatures. Isotopic enrichment in 11 B proves to be a viable strategy for mitigating helium production in transition-metal diborides, which is a critical consideration for nuclear applications. Irradiation-induced defects reduce the thermal diffusivity and conductivity of ZrB 2 by a factor of 4–9, which has important implications for its role as a plasma-facing material in fusion reactors that drive high heat fluxes through first-wall materials. Here, this comprehensive study lays the foundation for understanding ZrB 2 behavior under neutron irradiation and highlights important phenomena to consider for various material applications.

36 MATERIALS SCIENCE↗

Synthesis and flash sintering of (Hf 1-x Zr x )B 2 solid solution powders

(Hf 1-x Zr x )B 2 solid solution powders were synthesized by two methods. First, solution-based processing of HfCl 4 , ZrCl 4 , sucrose, and H 3 BO 3 was conducted followed by heat treatment in Argon to carry out the carbothermal reduction (CTR) reaction to form the diboride powders. Alternatively, in the so-called borohydride reduction (BHR) method, HfCl 4 , ZrCl 4 and NaBH 4 were mixed in an Argon glove box followed by heat treatment in Argon at 700-1500°C. The synthesized powders were characterized by XRD, SEM, TEM, EDS, and TGA, and the influence of different parameters such as starting composition, heat treatment temperature and time on products characteristics were revealed. Both CTR and BHR solid solution powders were then consolidated within ~5 min in a homemade flash sintering (FS) setup. Here, the composition, microstructure, hardness, and thermal-oxidation properties of flash sintered ceramics were characterized, and the implication of this study and directions for future research were discussed.

36 MATERIALS SCIENCE↗

Fabrication and thermophysical properties of UO 2 -UB 2 and UO 2 -UB 4 composites sintered via spark plasma sintering

Uranium dioxide (UO 2 ) composites with uranium diboride (UB 2 ) and uranium tetraboride (UB 4 ) have been proposed as advanced fuel candidates due to their high thermal conductivity, high melting point, high fissile density and their ability to incorporate a built-in burnable poison by tailoring the targeted 10 B/ 11 B ratio. As such, it is important to assess the fabrication, and thermal and micromechanical properties of such composites. In this work, UO 2 -UB 2 and UO 2 -UB 4 samples with boride phase fractions of 5, 15 and 30 wt% were fabricated to high densities (above 95 % theoretical density) via spark plasma sintering (SPS). This enabled sintering at relatively low temperatures and short timescales. SPS also aided in maintaining the target phase fractions of the samples as reactions between the constituent phases were suppressed due to the short timescales and reducing environment during sintering. Here, thermal diffusivity measurements from 299 to 1273 K were conducted through laser flash analysis (LFA). The diffusivity increased as a function of boride weight fraction, and UB 2 additions increased the thermal diffusivity of the composites more than UB 4 additions. Assessment of the LFA results indicated in-situ reactions between the UO 2 and boride phases that suppress the thermal diffusivity occur above 800 K for all samples. Oxidation of the boride phase was proposed as the underlying reaction. This was supported by thermodynamic assessments from the literature, as well as microstructural, crystallographic, and nanoindentation characterization performed on these samples.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Comparative neutron-irradiation effects on thermal conductivity degradation and dimensional stability of TiC, TiB 2 , and ZrB 2 at 200–1000 °C

Ultra-high-temperature ceramics (UHTCs), including TiC, Ti 11 B₂, and Zr 11 B₂, show great potential for plasma-facing components due to their excellent high-temperature properties prior to irradiation. However, their response to neutron irradiation remains insufficiently understood, limiting robust assessment of their viability for fusion energy applications. Here, this study examines the thermal conductivity, dimensional stability and microstructure of TiC, TiB₂, and ZrB₂ following neutron irradiation at temperatures of 200–1000 °C and fast neutron fluences of 2.0 × 10 25 to 1.1 × 10 26 n/m 2 (E > 0.1 MeV). Lattice swelling measured by synchrotron X-ray diffraction in all three UHTCs was maximized at 200 °C and decreased with increasing irradiation temperature, with no evidence of amorphization observed at 200 °C. Above 600 °C, significant macroscopic volume swelling was observed in irradiated Ti 11 B₂ and Zr 11 B₂, but not in TiC, likely due to cavity formation in the diborides. The post-irradiation thermal conductivity, measured at the irradiation temperature, ranged from 28 to 45 W/m·K, representing a 34–45% reduction relative to the unirradiated material. Notably, neutron-irradiated UHTCs exhibit recoverable thermal conductivity at elevated temperatures, comparable to ferritic–martensitic steels and potentially superior to W when transmutation effects are considered, highlighting promise for shielding or armor plasma-facing components. At 600 °C, both thermal conductivity degradation and lattice swelling saturated at doses exceeding 2–4 dpa.

fusion materials↗

Wafer-Scale MgB 2 Superconducting Devices

Progress in superconducting device and detector technologies over the past decade has realized practical applications in quantum computers, detectors for far-infrared telescopes, and optical communications. Superconducting thin-film materials, however, have remained largely unchanged, with aluminum still being the material of choice for superconducting qubits and niobium compounds for high-frequency/high kinetic inductance devices. Magnesium diboride (MgB 2 ), known for its highest transition temperature (T c = 39 K) among metallic superconductors, is a viable material for elevated temperature and higher frequency superconducting devices moving toward THz frequencies. However, difficulty in synthesizing wafer-scale thin films has prevented implementation of MgB 2 devices into the application base of superconducting electronics. Here, we report ultrasmooth (<0.5 nm root-mean-square roughness) and uniform MgB 2 thin (<100 nm) films over 100 mm in diameter and present prototype devices fabricated with these films demonstrating key superconducting properties including an internal quality factor over 10 4 at 4.5 K and high tunable kinetic inductance in the order of tens of pH/sq in a 40 nm thick film. This advancement will enable development of elevated temperature, high-frequency superconducting quantum circuits, and devices.

Boron↗

Spontaneous dynamical disordering of borophenes in MgB2 and related metal borides

Abstract Layered boron compounds have attracted significant interest in applications from energy storage to electronic materials to device applications, owing in part to a diversity of surface properties tied to specific arrangements of boron atoms. Here we report the energy landscape for surface atomic configurations of MgB 2 by combining first-principles calculations, global optimization, material synthesis and characterization. We demonstrate that contrary to previous assumptions, multiple disordered reconstructions are thermodynamically preferred and kinetically accessible within exposed B surfaces in MgB 2 and other layered metal diborides at low boron chemical potentials. Such a dynamic environment and intrinsic disordering of the B surface atoms present new opportunities to realize a diverse set of 2D boron structures. We validated the predicted surface disorder by characterizing exfoliated boron-terminated MgB 2 nanosheets. We further discuss application-relevant implications, with a particular view towards understanding the impact of boron surface heterogeneity on hydrogen storage performance.

36 MATERIALS SCIENCE↗

Single-photon detection using large-scale high-temperature MgB2 sensors at 20 K

Abstract Ultra-fast single-photon detectors with high current density and operating temperature can benefit space and ground applications, including quantum optical communication systems, lightweight cryogenics for space crafts, and medical use. Here we demonstrate magnesium diboride (MgB 2 ) thin-film superconducting microwires capable of single-photon detection at 1.55 μ m optical wavelength. We used helium ions to alter the properties of MgB 2 , resulting in microwire-based detectors exhibiting single-photon sensitivity across a broad temperature range of up to 20 K, and detection efficiency saturation for 1 μ m wide microwires at 3.7 K. Linearity of detection rate vs incident power was preserved up to at least 100 Mcps. Despite the large active area of up to 400 × 400 μ m 2 , the reset time was found to be as low as ~ 1 ns. Our research provides possibilities for breaking the operating temperature limit and maximum single-pixel count rate, expanding the detector area, and raises inquiries about the fundamental mechanisms of single-photon detection in high-critical-temperature superconductors.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Hybrid s -wave superconductivity in CrB 2

In a metal with multiple Fermi pockets, the formation of s-wave superconductivity can be conventional due to electron-phonon coupling or unconventional due to spin fluctuations. Here, we analyze the hexagonal diboride CrB 2 , which is an itinerant antiferromagnet at ambient conditions and turns superconducting upon increasing pressure. While the high-pressure behavior of T c suggests conventional s-wave pairing, we find that spin fluctuations promoting unconventional s-wave pairing become important in the vicinity of the antiferromagnetic dome. As the symmetry class of the s-wave state is independent of its underlying mechanism, we argue that CrB 2 is a realization of a hybrid s-wave superconductor where unconventional and conventional s-wave mechanisms team up to form a joint superconducting dome.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Investigation of Materials for Radio Frequency Antenna Plasma Facing Components

Here, the interaction of radio frequency (RF) sheaths with fusion reactor relevant materials (e.g., tungsten and titanium diboride) is being studied on the RF Plasma Interaction Experiment (RF PIE). The RF PIE consists of an electron cyclotron resonance (ECR) plasma source (2.45 GHz, 5 kW) with a biased and heated RF electrode that is used to simulate antenna surfaces in contact with the edge plasma. Helium plasmas (density of ~1e18/m 3 , electron temperature of 4–5 eV) are being used to explore sheath formation on material surfaces with biases up to 500 V. The erosion of a tungsten surface is being studied spectroscopically using a mirror-linked 1 m Czerny-Turner UV imaging spectrometer with a spectral resolution of 0.012 nm for measuring plasma emission in and near the sheath. Tungsten line emission intensity is higher for RF versus dc biasing for similar plasma conditions and average ion energy. RF biasing causes a broadening of the ion energy distribution function (IEDF) due to the RF sheath, as determined from the hPIC2 code, and results in enhanced sputtering. Calculations of the expected sputtering yield for dc and RF biasing are consistent with experimental observations of changes in the 400.9 nm tungsten line emission intensity as a function of ion energy.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Final-stage densification kinetics of direct current–sinteredZrB2

Final-stage sintering was analyzed for nominally phase pure zirconium diboride synthesized by borothermal reduction of high-purity ZrO2. Analysis was conducted on ZrB2 ceramics with relative densities greater than 90% using the Nabarro–Herring stress–directed vacancy diffusion model. Temperatures of 1900°C or above and an applied uniaxial pressure of 50 MPa were required to fully densify ZrB2 ceramics by direct current sintering. Ram travel data were collected and used to determine the relative density of the specimens during sintering. Specimens sintered between 1900 and 2100°C achieved relative densities greater than 97%, whereas specimens sintered below 1900°C failed to reach the final stage of sintering. The average grain size ranged from 1.0 to 14.7 μm. The activation energy was calculated from the slope of an Arrhenius plot that used the Kalish equation. The activation energy was 162 ± 34 kJ/mol, which is consistent with the activation energy for dislocation movement in ZrB2. The diffusion coefficients for dislocation motion that controls densification were 5.1 × 10−6 cm2/s at 1900°C and 5.1 × 10−5 cm2/s at 2100°C, as calculated from activation energy and average grain sizes. This study provides evidence that the dominant mechanism for final-stage sintering of ZrB2 ceramics is dislocation motion.

36 MATERIALS SCIENCE↗

Advantages of Superconducting Device using 26 MgB2 Wire

Superconducting undulator (SCU) which can run at higher temperature than 4 Kelvin range has been anticipated for a long time. However, the performance of high-temperature superconductor (HTS) tapes have not improved over the last decade as the industry mostly concentrates on the cost reduction. Magnesium Diboride (MgB2) has a critical temperature of 39 K and the 1 st generation (1G) wire has been in production but it was not sufficient to be used in SCU. Recently the 2 nd generation (2G) wire has been developed. It is estimated to give a similar performance as NbTi wire at 20K. In this paper the advantages of a SCU with 2G MgB2 wire compared to a conventional SCU with NbTi or Nb3Sn3 wire.

43 PARTICLE ACCELERATORS↗

Compositional Exploration of Additively Manufactured Ultra-High-Temperature Ceramic Composites for Use in Concentrated Solar Power Plant Heat Exchangers

The DOE has research interest in new technologies for high temperature concentrated solar power plants. Our project this summer was to explore the use of additively manufactured ultra-high-temperature ceramics in a heat exchanger. The heat exchanger would transfer heat between a molten chloride salt and supercritical CO 2 . We selected 22 compositions to test and were able to mix 14 of these compositions. We sintered these compositions using pressureless sintering and direct current sintering. We also conducted high temperature TGA on some ceramic samples. We also performed preliminary binder jet additive manufacturing trials with tungsten carbide powder. Our work so far points towards one of our titanium diboride samples being promising, but much more research needs to be done.

14 SOLAR ENERGY↗

UHT-CAMANCHE: Ultra-High Temperature Ceramic Additively Manufactured Compact Heat Exchangers

The conceptual basis for this project is the convergence of advanced ultra-high temperature ceramic materials and additive manufacturing technologies to produce compact ceramic heat exchangers with complex internal flow path geometries. Task areas were broadly divided into materials and manufacturing development, heat exchanger design, component testing, and techno-economic analysis. Technical challenges included the design and commissioning of new test facilities, improving feature resolution and deposition rate of ceramic additive manufacturing techniques, establishing process-structure-property relationships in additively manufactured ultra-high temperature ceramics, and assessing high temperature materials compatibility in CO 2 environments. The primary candidate material evaluated in this work is a composite comprising zirconium diboride (ZrB2) with 30 vol. % silicon carbide (SiC) which was selected based on its desirable combination of high temperature mechanical properties, high thermal and electrical conductivities, and oxidation resistance. High solids loaded ZrB2-SiC pastes suitable for extrusion-based additive manufacturing were developed for the first time as part of this work. Materials compatibility studies indicate this material oxidizes in CO 2 to form a protective borosilicate scale which transforms to pure silica above 1000°C. Parts made by additive manufacturing displayed enlarged grain sizes produced by pressureless sintering as compared to hot-press sintering. Increases in microstructural coarseness have outsized effect on oxidation performance up to 1400°C due to incomplete oxidation of coarse large diameter SiC particles resulting in lower amounts of silica that apparently inhibit protective scale formation. Additive manufacturing as a forming technique did not appear to significantly affect thermal conductivity, hardness, or elastic modulus, though flexural strength was reduced by half or more as compared to traditionally hot-pressed materials. This effect was attributed to the presence of strength-limiting flaws (ca. 40 microns in size) originating from extrudate inhomogeneities that could potentially be eliminated with further process improvements. Attempts to attain economies of scale for production of multi-kilowatt scale heat exchangers by ceramic additive manufacturing proved difficult. Lack of automation and a modest extrusion rate while retaining fine feature resolution made the overall process labor intensive and limited experimental throughput. A number of full-scale components were taken through post-process heat treatments including drying, binder burnout, and sintering; however, none survived without significant flaws or cracks. Therefore, no operational data from a newly installed heat exchanger test loop were able to be obtained during the performance period. Continued research and development is recommended to improve economic feasibility of ceramic additive manufacturing by standardizing the use of advanced sensors, artificial intelligence, and automation tools to reduce associated labor costs and accelerate production rates. The materials and manufacturing techniques demonstrated in this work are likely to find applications in defense and energy applications.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

Combustion synthesis of nanoscale magnesium borides with improved hydrogen uptake and release

The overarching goal of the reported project was to develop reversible metal hydrides that can be dehydrogenated and recharged at relatively low temperatures and pressures. The project complemented the research on reversible metal hydrides for hydrogen storage conducted by the Hydrogen Materials – Advanced Research Consortium (HyMARC). The students involved were trained at both the University of Texas at El Paso (UTEP) and Sandia National Laboratories (SNL). The research objectives were to fabricate nanoscale magnesium boride powders with different B/Mg atomic ratios and to investigate the effects of B/Mg ratio and particle size on the hydrogenation properties of the obtained materials. Magnesium diboride (MgB 2 ) and tetraboride (MgB 4 ) were synthesized by using combustion synthesis and by heating in a tube furnace. The latter method resulted in materials with significantly reduced impurity levels. An effective method for the removal of magnesium oxide impurities was identified. High-energy ball milling produced submicron MgB 2 and MgB 4 powders. However, hydrogenation experiments at pressures up to 700 bar have not shown any uptake of hydrogen. Thermogravimetric analysis of the decomposition of the obtained MgB 2 and MgB 4 demonstrated higher thermodynamic stability of the latter. Thus, the boron-rich nature and phase stability of magnesium borides with high B/Mg ratios make them poor candidates for direct hydrogenation. However, the synthesized MgB 4 is a promising energetic additive to solid fuels for high-speed air-breathing propulsion as it offers a lower oxidation onset temperature and greater energy density than MgB 2 .

08 HYDROGEN↗

Water Vapor Resistant SiC/SiC Composite for Hydrogen-Based Turbines (Final Scientific Technical Report)

New material innovations are needed for the extreme environments of next generation, hydrogen-fueled turbine engines. Ceramic matrix composites (CMCs) offer high-temperature capability but are susceptible to degradation in high-temperature water vapor. Pratt & Whitney’s (P&W) baseline silicon carbide (SiC)/SiC CMC was initially applied to design a component in a hydrogen-fueled engine, verifying the existence of a design space and extracting boundary conditions to inform testing parameters. Several material innovations, including two fibers, interface coatings (IFC), and self-healing matrices (SHM), were investigated to improve high-temperature performance in water vapor. A boron-doped pyrocarbon (B-PyC) IFC and a SHM matrix with layers of zirconium nitride (ZrN) or zirconium diboride (ZrB 2 ) were developed to fabricate minicomposites with either standard Hi-Nicalon™ Type S (HNS) fibers or new Tyranno® SA4 fibers (SA4). The B-PyC IFC is functional but lacks in providing improved durability. A matrix consisting of thick layers of SiC and thin layers of ZrB 2 shows promise as a SHM that can effectively seal matrix cracks in this extreme environment. Minicomposites with HNS fibers generally outperform those with SA4 fibers.

08 HYDROGEN↗

Protective coating withstands high temperature in oxidizing atmosphere

Protective coating containing a plasma arc sprayed mixture of hafnium oxide and zirconium diboride will withstand high temperatures in an oxygen rich atmosphere. Used on a homogeneous tungsten thermocouple, it does not flake or crack on subsequent cooling and reheating, and does not degrade the thermocouple response time.

Mellor, C. H.↗