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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 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Solid-State Sintering of Core-Shell Ceramic Powders Fabricated by Particle Atomic Layer Deposition

The properties of technical ceramics are highly dependent on their microstructure, which evolves during sintering. Sintering is the process by which ceramic parts are subjected to high temperatures to activate chemical diffusion and the consumption of porosity. During the initial stage of sintering, interparticle necks between neighboring particles form and subsequently increase in size, consuming porosity as the particle centers move closer together. To experimentally determine how this process depends on particle surface composition, particle atomic layer deposition (ALD) was used to deposit a thin film of amorphous aluminum oxide (Al2O3) onto yttria-stabilized tetragonal zirconia (3YSZ) particles, producing core-shell structured powders. The uniformity of the Al2O3 film was confirmed with transmission electron microscopy and energy dispersive spectroscopy. Scanning electron microscopy was used to observe microstructural evolution during sintering, and the dihedral angles of Al2O3 and 3YSZ grains were measured to determine the ratio of interfacial energies between the 3YSZ|3YSZ, 3YSZ|Al2O3, and Al2O3|Al2O3 interfaces. Analysis of the densification kinetics revealed that the initial stage of densification is dependent on the material at the surface of the particles (ie, the Al2O3 film) and is controlled by the diffusion of Al3+ cations through Al2O3. Once the Al2O3 film has coalesced, the sintering behavior is controlled by the densification of the core material (3YSZ). Thus, core-shell powders fabricated by particle ALD sinter by a two-step process where the kinetics are dependent on the material present at interparticle contacts.

alumina↗
DOE OSTI2022

Temperature-dependent diffuse reflectance measurements of ceramic powders in the near- and mid-infrared spectra

Radiative properties are critical to quantify radiative energy fluxes between surfaces and in participating media. However, there is limited experimental data on temperature-dependent radiative properties of materials. Herein, this work focuses on experimentally measuring temperature-dependent diffuse reflectance in the near- and mid-infrared spectra (1–20 μm) for ceramic particles with applications as heat-transfer and thermal-storage media in concentrated solar power (CSP) plants. Specifically, a commercially available sintered bauxite proppant, ACCUCAST ID80, and its primary chemical constituents—alumina (Al 2 O 3 ) and silica (SiO 2 )—are measured in powder form using a Fourier transform infrared spectrometer (FTIR) coupled with a specialized diffuse reflectance accessory and a heated stage. Room-temperature diffuse reflectance measurements show increased absorption in tests with greater mass fractions of the ceramic samples. There is a strong correlation in the measured reflectance spectra of ACCUCAST with alumina and silica in the spectral range 2000–500 cm –1 (5–20 μm). Whereas, for shorter wavelengths (< 5 μm), the absorptance for ACCUCAST is greater than the absorptance for alumina and silica, indicating contributions from other chemical species present in the composite material. For the first time, temperature-dependent diffuse reflectance measurements are reported for ACCUCAST up to 1000 °C. These results are compared against those of alumina and silica through the calculation of a thermal emittance. All three materials exhibit a calculated emittance of ~0.9 at room temperature. However, this value decreases to ~0.6 for ACCUCAST and drops to less than 0.4 for alumina and silica at 1000 °C. Thermal cycling in air at 1000 °C resulted in a visible color change from dark grey to light orange for ACCUCAST and a subsequent larger increase in reflectance for wavelengths less than 5 μm as compared to ACCUCAST thermally cycled at 1000 °C in vacuum. Alumina and silica spectra proved to be largely unaffected by thermal cycling under atmospheric conditions. Overall, this study establishes a powerful technique for the characterization of radiative properties of particulate materials as a function of temperature and presents a detailed case study of ACCUCAST, a candidate for next-generation particle-based CSP.

14 SOLAR ENERGY↗
DOE OSTI2024

One-Pot Coating of Ceramic Powders by Exfoliated Boron Nitride Layers with a Dense CO 2 Medium and Ultrasound-Aided Mixing

The coating or doping of substrates by two-dimensional materials to impart superior functional properties (such as improved thermal conductivity, bacterial resistance, reduced friction) is receiving increased attention. Environmentally benign, rapid and scalable coating techniques are desirable for this purpose. Here, we report a novel process for coating alumina, silicon carbide and boron carbide substrates with hexagonal boron nitride (h-BN) layers. The process consists of two sequential steps. First, h-BN layers are exfoliated from bulk h-BN in supercritical carbon dioxide (scCO 2 ) using ultrasound-aided mixing. This step is followed by self-assembly (i.e., coating) of the exfoliated h-BN on the substrates in liquid CO 2 also aided by ultrasound. The liquid CO 2 state is achieved by simply lowering the pressure and temperature of the first step below the critical point of CO 2 (P c = 72.8 atm; T c = 31.1 °C). Scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) micrographs clearly reveal the exfoliation of h-BN under scCO 2 conditions as well as the h-BN assembly on various substrates under liquid CO 2 conditions. X-ray diffraction patterns confirm the structural integrity of the coated h-BN layers. It was also confirmed that without a transition to the liquid CO 2 phase following exfoliation in scCO 2 , there was negligible coating of h-BN on the substrates. Researchers in the field could consider this benign process to rapidly coat or dope materials with h-BN and other 2D materials to impart improved functional properties in myriad applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Metal-ceramic composite powders

A process for manufacturing metal-ceramic composite material powder comprising ball milling metal powder and ceramic nanoparticles to yield a metal-ceramic composite powder comprising ceramic nanoparticles embedded in a metal matrix powder particles; wherein the ball milling is performed using a ceramic milling media and a milling vessel having a ceramic interior surface. Metal matrix nanocomposite powders comprising ceramic nanoparticles imbedded in metal matrix powder particles; wherein the metal matrix powder particles have a spherical shape; wherein there is uniform distribution the ceramic nanoparticles; wherein the nanocomposite powders have good flowability.

Chen, Lianyi↗
DOE OSTI2026

Characterization of ceramic fuel powder packing fractions to support INFLUX

Triply periodic minimal surface (TPMS)-based structures show marked potential in novel nuclear reactor fuel designs, as their high surface area-to-volume ratio increases the efficiency of heat transfer out of the fuel, enabling safer, more innovative reactor designs. This milestone report addresses the role of dUO 2 powder processing route on the fill behavior of TPMS-based cladding shells to understand and advance the feasibility of manufacturing TPMS-based nuclear fuel forms. dUO 2 powder was processed through either a dry granulation route, varying consolidation pressure, or through milling, varying milling time, milling method and milled size distribution. The lowest tapped bulk densities (TBD), but best powder flowabilities, were obtained when testing unprocessed dUO 2 powder which was prone to self-agglomeration and formed low-density spheroids. The highest TBD and lowest flowabilities were obtained when using powder produced by hammer-milling dUO 2 powder to pass through a 200-mesh sieve, which led to particles with angular morphologies. Powder produced by dry granulation exhibited TBD that varied according to the consolidation pressure used to form the initial pellets and exhibited improved flowabilities when compared to hammer-milled material. Because of the large span of granule sizes formed as well as the irregular shape associated with the granules, a packing fraction of 0.69 was achieved, exceeding the analytical solution for random close packing of mono-sized spheres. TPMS polymer shells were loaded with unprocessed, granulated, and hammer-milled dUO 2 powders, and their qualitative packing behaviors were analyzed using x-ray computed tomography (xCT). TBDs calculated after loading TPMS polymer shells were 10-20% lower when compared to tapped bulk density measurements taken in a glass graduated cylinder, indicating a non-trivial impact on the tapped bulk density of either the TPMS channel size, TPMS channel surface material, powder cohesiveness, or a combination of the two parameters. A metallic zircaloy-4 TPMS shell will be loaded with hammer-milled dUO 2 powder upon receipt of the shell from Oak Ridge National Laboratory (ORNL) and shipped to Idaho National Labs (INL) for subsequent hot isostatic pressing (HIP) densification experiments.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2023

Development of Binder Jet Compatible Silicon Carbide Mixtures for Increased Sintered Density

Binder jet additive manufacturing can process a variety of ceramic powder feedstocks to manufacture near net shape green parts that are subsequently sintered to achieve densification. In particular, silicon carbide (SiC) is a promising ceramic material for heat exchangers in energy storage applications and binder jet is a well-suited process for manufacturing these heat exchangers due to the often geometrically complex designs. However, the need for good powder flowability in binder jet printing often limits the feedstock powder to be larger particles rather than that of ultra fine submicron powders used in conventional ceramic processing, which are more readily densified during sintering. The present work explores the use of various powder mixtures and sintering settings to identify strategies for achieving high density sintered parts in binder jet compatible systems without the use of infiltration. Liquid-phase sintering additives and bimodal powder mixtures are explored alongside different sintering temperatures, rates, atmospheres, and hold times. Two mixtures were found to be good candidates for further exploration: 1) 90 wt% 0.6 µm SiC + 6.25 wt% Al 2 O 3 + 3.75 wt% Y 2 O 3 mixture achieved the highest sintered relative density of 91.2%; and 2) a bimodal mixture comprised of 45 wt% 10 µm SiC + 45 wt% 0.6 µm SiC + 6.25 wt% Al 2 O 3 + 3.75 wt% Y 2 O 3 had the best powder flowability of the powders measured and a 75.1% sintered relative density.

25 ENERGY STORAGE↗
DOE OSTI2022

Energy Efficient, Incrementally Scalable, Continuous Basalt Fiber Manufacturing Process (Final Technical Report)

This project focused on new materials, bushing materials, that had the ability to produce continuous basalt or glass fiber. The original scope of the project was designed to identify bushing materials and produce fiber, but that scope did change during the program. The team put significant work into bushing material development in the place of producing fiber. The final bushing materials had to be able to produce fiber and the final sets of the project saw single strands of fiber be produced. The final materials selected was a unique MMC bushing composition. Using advanced chemistry, the interface chemistry was tailored between metallic and ceramic powders. Powders and fibers were consolidated using cold isostatic pressing and electrified ceramic hot pressing to form a near net shape composite bushing.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Fusion welding of refractory metals and ZrB 2 -SiC-ZrC ceramics

Molybdenum and a molybdenum alloy were fusion welded to ZrB2-based ceramics to determine if the electrical and thermal properties of the metals and ceramics affected their weldability. Commercial ceramic powders were hot pressed, machined into coupons, and preheated to 1600 °C before joining the ceramics to commercial metals using plasma arc welding. Weldability varied as indicated by the range of porosity observed within the fusion zones. Measured thermal and electrical properties appeared to have little to no effect on the weldability of metal-ceramic welds despite the large range of values measured across each property. Differences in melting temperatures between metal and ceramic coupons did affect weldability by changing the weld penetration depth into ceramic coupons. Finally, future studies on metal-ceramic welds are suggested to investigate the effect that work function, melt viscosity, wetting, or other properties have on weldability.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Direct ink writing of boron carbide monoliths

Direct ink writing – an extrusion-based additive manufacturing process – followed by pressureless sintering was investigated to produce boron carbide monoliths. The effects of ceramic powder loading and Pluronic binder concentration on the rheology of boron carbide pastes were studied and linked to both processing behaviour and final outcome in terms of sintered density and hardness. The effects of printing parameters, in particular orifice diameter and printing speed, were also investigated. Reducing the size of the extrusion nozzle from 584 μm to 406 μm led to significantly better shape retention, lower surface roughness, as well as higher density and hardness. A 203 μm printing orifice was also trialled but was unsuccessful due to faster drying kinetics that occurred with smaller ceramic struts resulting in rapid warping and nozzle clogging. Carbon-black – 8 wt% relative to B 4 C – acted as an effective sintering aid to increase both density and hardness. After optimisation of feedstock and printing parameters, few-layer samples (3–5 layers) had a density as high as ~ 97 % TD and a hardness of ~ 30 GPa. On the other hand, 18-layer specimens had a sintered density of ~ 87 % TD, despite a fully dense microstructure, due to the formation of a 3D array of inter-strut pores. Nevertheless, several issues that arose during manufacturing and post-processing were detrimental to the density and structural integrity of printed specimens; these issues were identified, discussed, and suggestions for future work are provided in this report.

36 MATERIALS SCIENCE↗
DOE OSTI2024

A new ductile, tougher resin for impregnation of superconducting magnets

A major remaining challenge for Nb 3 Sn high field magnets is their training due to random temperature variations in the coils. The main objective of our research is to reduce or eliminate it by finding novel impregnation materials in replacement of the epoxies currently used. An organic olefin-based thermosetting dicyclopentadiene resin, C 10 H 12 , commercially available in Japan as TELENE® by RIMTEC, was used to impregnate a short Nb 3 Sn undulator coil developed by ANL and FNAL. This magnet reached short sample limit after only two quenches, compared with ∼100 when CTD-101K® was used. Ductility, i.e. the ability to accept large strains, and toughness were identified as key properties to achieve these results. In addition, we have been investigating whether mixing TELENE with high heat capacity ceramic powders such as Gd 2 O 3 , Gd 2 O 2 S, and HoCu 2 , increases the specific heat (C p ) of impregnated Nb3Sn superconducting magnets. The viscosity, heat capacity, thermal conductivity, and other physical properties of TELENE with high-C p powder fillers were measured in this study as a function of temperature and magnetic field. The TELENE-87 wt%Gd 2 O 2 S had a peak in C p between 4.3 K and 5.3 K at fields between 0 and 8 T. We have also investigated the effect on the mechanical properties of pure and mixed TELENE under 10 MGy of gamma ray irradiation at the Takasaki Advanced Radiation Research Institute in Takasaki, Japan. TELENE-87 wt%Gd 2 O 2 S exhibited exceptional radiation resistance. Impregnating an undulator coil with TELENE mixed with Gd 2 O 2 S powder will verify whether the coils' thermal stability further improves, or whether its low diffusivity will require engineering the material with high-thermal conductivity components. Short magnet training will lead to better magnet reliability, lower magnet margins, lower risk and substantial saving in accelerators' commissioning costs. Part of this study is supported by the U.S.-Japan Science and Technology Cooperation Program in high energy physics operated by MEXT in Japan and DOE in the U.S.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2022

Processing, structure, and thermal properties of ZrW 2 O 8 , HfW 2 O 8 , HfMgW 3 O 12 , Al(HfMg) 0.5 W 3 O 12 , and Al 0.5 Sc 1.5 W 3 O 12 negative and zero thermal expansion coefficient ceramics

Negative and zero coefficient of thermal expansion (CTE) materials are of interest for developing polymer composites in electronic circuits that match the expansion of Si and in zero CTE supports for optical components, e.g., mirrors. In this work, the processing challenges and stability of ZrW 2 O 8 , HfW 2 O 8 , HfMgW 3 O 12 , Al(HfMg) 0.5 W 3 O 12 , and Al 0.5 Sc 1.5 W 3 O 12 negative and zero thermal expansion coefficient ceramics are discussed. Al 0.5 Sc 1.5 W 3 O 12 is demonstrated to be a relatively simple oxide to fabricate in large quantity and is shown to exhibit single phase up to 1300 °C in air and inert N 2 environments. The negative and zero CTE behavior was confirmed with dilatometry. Thermal conductivity and heat capacity were reported for the first time for HfMgW 3 O 12 and Al 0.5 Sc 1.5 W 3 O 12 and thermal conductivity was found to be very low (~0.5 W/mK). Grüneisen parameter is also estimated. Methods for integration of Al 0.5 Sc 1.5 W 3 O 12 with other materials was examined and embedding 50 vol% of the ceramic powder in flexible epoxy was demonstrated with a commercial vendor.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Exploring the structural uniformity and integrity of protonic ceramic thin film electrolyte using wet powder spraying

Thin protonic ceramic electrolyte contributes to lower ohmic resistance and enhances electrochemical performance of protonic ceramic electrochemical cells. However, manufacturing of large-scale thin electrolyte remains a challenge. Wet powder spraying is an attractive technique to deposit <10 µm thin electrolyte when advanced atomizing techniques and optimized spraying process are integrated. Here ultrasonic atomization is integrated in the wet powder spray technique to reduce the thickness of electrolyte. Moreover, a parametric study is conducted to optimize the wet powder spray process to deposit uniform and crack-free electrolyte film. It is illustrated that tuning of solid loading rates and spray passes can affect the morphology of the as-sprayed electrolyte film, enabling the structural compactness of the sintered electrolyte layer. To maintain chemical stability of the electrolyte layer during sintering, effect of sintering temperature is further investigated to produce a physically thin, structurally dense, and chemically homogeneous electrolyte layer. The protonic ceramic electrochemical cells fabricated with optimized spraying and sintering parameters demonstrate excellent performance under both fuel cell and electrolysis modes. In addition, the cells exhibit remarkable structural integrity during redox and long-term stability tests.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Binder jetting additive manufacturing of silicon carbide ceramics: Development of bimodal powder feedstocks by modeling and experimental methods

A limitation of binder jetting additive manufacturing is the low density of fabricated parts. Mixing powders with different sizes is a promising approach to increase powder bed packing density and, hence, printed part density. However, in previous studies mixed powder feedstock was prepared by trial and error method. In this research, both modeling and experimental methods were used to prepare the bimodal powder feedstocks. Analytical packing model was introduced for irregular powders. A bimodal powder was prepared by mixing two different-sized silicon carbide powders (i.e. coarse and fine) using ball mill, and their tap densities were measured. Silicon carbide plates were printed using the coarse and bimodal powders by a commercial binder jetting system. Results showed that the modeling method could predict the tap density of bimodal powders with high accuracy. The printed parts from bimodal powder achieved higher green densities than those from the unimodal powder.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Reducing waste of the hydride-dehydride process for U-6 wt% Nb spherical powders through lower impact and targeted milling

The breakdown of solid metal into powder during the hydride-dehydride process is commercially important for the formation of titanium and other metal powders. Typically, the milling of the brittle hydride powder occurs in a ball mill, where milling media impacts powder particles to break them down. The milling media can impact particles that are larger than desired, as desired, or smaller than desired, indiscriminately making all particles smaller. In this work, we investigate how to minimize waste powder production during milling using two different milling methods, planetary ball milling and milling in a sieve shaker (sieve-milling). Both processes yielded similar amounts of 20–75 μm diameter powder (the target size range); however, sieve-milling generated a significantly smaller amount of undersized waste powder. The powders were characterized by X-ray diffraction, SEM/STEM, and magnetic susceptibility. Several differences between ball milling and sieve-milling processes are discussed. We then conclude that the decreased yield of undersized powder in sieve-milling was due to a combination of lower impact energy in sieve-milling, unreacted metallic cores in the hydride flakes, and the ability to mill target particle sizes during sieve-milling. While these results are from the milling of brittle hydride powder, similar methods may be applicable to other brittle powders, including ceramics or salts.

Chemistry↗
DOE OSTI2025

Melting point of group IV and V transition metal diborides

The environmental conical nozzle levitator system enables cooling trace experiments above 4000 K. These cooling trace experiments were used to determine the melting points through observation of thermal arrest of group IV and V transition metal diborides (TiB 2 , T m = 3313 ± 33 K; ZrB 2 , T m = 3404 ± 38 K; HfB 2 , T m = 3529 ± 33 K; and TaB 2 , T m = 3284 ± 10 K; note: mean ± 2 standard error). Temperature measurements were conducted utilizing dual single-color pyrometers at wavelengths of 0.9 and 0.65 µm. This system utilizes aerodynamic levitation and dual laser heating to achieve temperatures approaching 4000 K. The samples were synthesized from commercial powders using ceramic gel-casting to produce high-density spherical components. The measurements obtained were compared to previously reported melting temperature values and were generally found to be in agreement with most of the published values.

Materials science↗
DOE OSTI2022

Pseudo-Hot-Isostatic Pressing (P-HIP)

Researchers at Los Alamos National Laboratory developed a technology to produce high performance ceramic or metal with a combination of major key properties such as versatile-complicated shape, high density, uniform density distribution, and minimal amounts of starting material. The novel pseudo-hot-isostatic-pressing (P-HIP) uses graphite or boron nitride flakes as the stress transmission media to transmit stress instead of the conventional solid graphite punch. The graphite and boron nitride flakes are solid lubricants and can slide among one another to re-distribute the stress from high stress concentration area to the low stress concentration areas, resulting in a self-stress-relief action. This innovative P-HIP enables the manufacturing of complicated shapes with near-net-shape capability while minimizing the energy used and reducing waste. This is a revolutionary breakthrough to the ceramics and powder metallurgy industries.

36 MATERIALS SCIENCE↗