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33 records · Page 2

Electron diffraction radial distribution function analysis of amorphous boron carbide synthesized by ion beam irradiation and chemical vapor deposition

Amorphous boron carbide (a-BxC) networks consist of light elements, and their low atomic scattering factors makes structural analysis by x-ray diffraction difficult. Electron diffraction has an advantage of detecting the light elements, because of the strong interaction between the matter and electrons. In this work, we prepared a-BxC by ion beam technologies and plasma-enhanced chemical vapor deposition, and characterized their structures via atomic pair-distribution functions derived from electron diffraction intensity profiles. It was found that a pentagonal pyramid is the most favorable cluster in a-B4C generated by ion irradiation, while C—C homonuclear bonds were formed in the deposited a-B x C thin film. X-ray photoemission spectroscopy revealed that the a-BxC thin film possesses more carbon than B 4 C, which is responsible for the formation of the homonuclear bonds.

36 MATERIALS SCIENCE↗

Laser-induced slip casting as an additive manufacturing approach for silicon carbide

Here, this work presents processing silicon carbide (SiC) with the laser-induced slip casting (LIS) additive manufacturing (AM). SiC was stabilized in water with polyethyleneimine (PEI) dispersant, and SiC slurries were made with rheology for LIS printing. High-density ceramic parts were printed, followed by single-step binder burnout and sintering. The printed parts achieved 93–95 % of theoretical density. X-ray computed tomography (XCT) revealed a small distribution of flaws exceeding 100 microns. The mechanical properties were measured in both parallel and perpendicular to the printing layers, and the orientation with layers perpendicular to the bending moment resulted in higher strength compared to the parallel direction. Porosity resulting from processing and large inclusions of boron carbide (B4C) were the root cause of failure in the measured samples. Despite these defects through this effort, this new approach demonstrates promise for green forming of SiC with densities greater than 95 % theoretical and tensile strengths above 250 MPa.

Additive Manufacturing↗

Directional amorphization of covalently-bonded solids: A generalized deformation mechanism in extreme loading

Shock compression subjects materials to a unique regime of high quasi-hydrostatic pressure and coupled shear stresses for durations on the order of 1–10 nanoseconds for laser-driven loading of samples. There is, additionally, an attendant temperature increase due to the shock and the mechanisms of plastic deformation in metals whereby dislocations, twins, and phase transitions nucleate and propagate at velocities near the sound speed. Covalently bonded materials have, by virtue of the directionality of their bonds, great difficulty in responding by conventional plastic deformation to this extreme regime of shock compression. Here, we propose that the shear from shock compression induces amorphization, as observed in Si, Ge, B4C, SiC, and olivine ((Mg, Fe) 2 SO 4 ) and that this is a general deformation mechanism in a broad class of covalently bonded materials. The crystalline structure transforms to amorphous along regions of maximum shear stress, forming nanoscale bands, and thereby relaxing the shear component of the imposed shock stress. This process is usually preceded by the emission and propagation of a critical concentration of dislocations.

36 MATERIALS SCIENCE↗

Oblique angle deposition of boron carbide films by magnetron sputtering

Many applications of boron carbide (B4C) films entail deposition on non-planar substrates, necessitating a better understanding of oblique angle deposition phenomena. Here, we systematically study the effect of substrate tilt on properties of B 4 C films with thicknesses up to 10 μm deposited by direct current magnetron sputtering. Results show that all films are amorphous and columnar with an average column width of ~100 nm, independent of substrate tilt. Column tilt angles are limited to ~20° even for substrate tilt of 80°. Film density, residual stress, and the refractive index weakly (within ≲20%) depend on substrate tilt. Furthermore, oxygen impurities bond preferentially with carbon atoms in inter-columnar regions. Substrate tilt has a major effect on mechanical properties that decrease by ~50%, suggesting weak interconnection between nano-columns. Implications of these observations for the deposition onto non-planar substrates are discussed.

36 MATERIALS SCIENCE↗

High-Rate Sputter Deposition of Ultrathick Boron Carbide Coatings on Rolling Spherical Substrates

Amorphous boron carbide (B 4 C) is a promising next-generation ablator material for inertial confinement fusion. However, the deposition of ultrathick B4C coatings with submicron-scale density uniformity on spherical substrates, as required for ablator shell fabrication, remains challenging. Here, in this study, we use direct current magnetron sputtering to deposit B 4 C onto 2-mm-diameter Si spheres rolling in a dish-shaped substrate holder. High deposition rates of ∼3 μm/h are achieved. Ultrathick films have a columnar microstructure, with the column width determined by the density of nodular defects. Nodular defect nucleation is dominated by the pickup of particulates from the holder during substrate rolling. We demonstrate the fabrication of a hollow B 4 C spherical shell with a wall thickness of 80 μm. Also demonstrated is the laser machining of holes in the B 4 C coating, which is necessary for both the chemical removal of the Si template and the attachment of a fusion fuel fill tube.

Inertial confinement fusion targets↗

High-Power Impulse Magnetron Sputter Deposition of Boron Carbide with Full-Face Erosion Magnetron and Mixed Ar-Ne Plasma

Boron carbide (B 4 C) is an attractive inertial confinement fusion ablator material. The fabrication of B4C ablators by magnetron sputtering requires process optimization. To increase process flexibility, here we explore high-power impulse magnetron sputter (HiPIMS) deposition of B 4 C in pure Ar and mixed Ar-Ne plasmas. Here, the results show that higher plasma discharge currents can be reached with a mixed Ar-Ne plasma in the entire working pressure range studied (5 𝑡𝑜 50 mTorr). At 45 mTorr with 10% of Ne in the Ar-Ne mix, high peak target current densities of ~1 A cm −2 were demonstrated. Films deposited with such a mixed Ar-Ne plasma with a full-face erosion magnetron source on substrates biased at −25 V exhibited higher density and improved mechanical properties, albeit with higher compressive residual stresses compared to the case of HiPIMS deposition in a pure Ar plasma. This work demonstrates additional process flexibility of the HiPIMS discharge mode for the deposition of B 4 C coatings.

Ablator capsule↗

High-entropy boride–carbide ceramics by sequential boro/carbothermal synthesis

We report a dual-phase high-entropy boride/carbide ceramic with fine grain size was synthesized by a sequential boro/carbothermal process. In the first step, a Hf-Nb-Ta-Ti-Zr-containing carbide was synthesized by carbothermal reduction of oxides followed by reaction of the carbide with B4C and ZrH2 to convert part of the carbide to boride. The resulting composition was ~29 vol% high-entropy boride with an average grain size of ~1.1 µm. Solid solution formation occurred at the densification temperature of 1900°C resulting in a relative density higher than 99%. The Vickers’ hardness was 26.5 ± 1.4 GPa. This is the first report of synthesizing dual-phase boride-carbide high-entropy ceramics from carbothermally synthesized, high-entropy carbide powders.

36 MATERIALS SCIENCE↗

Prospects for the expansion of standing wave ambient pressure photoemission spectroscopy to reactions at elevated temperatures

Standing wave ambient pressure photoemission spectroscopy (SWAPPS) is a promising method to investigate chemical and potential gradients across solid-vapor and solid-liquid interfaces under close-to-realistic environmental conditions, far away from high vacuum. Until now, these investigations have been performed only near room temperature, but for a wide range of interfacial processes, chief among them being heterogeneous catalysis, measurements at elevated temperatures are required. One concern in these investigations is the temperature stability of the multilayer mirrors, which generate the standing wave field. At elevated temperatures, degradation of the multilayer mirror due to, for example, interdiffusion between the adjacent layers, decreases the modulation of the standing wave field, thus rendering SWAPPS experiments much harder to perform. Here, we show that multilayer mirrors consisting of alternate B4C and W layers are stable at temperatures exceeding 600 °C and are, thus, promising candidates for future studies of surface and subsurface species in heterogeneous catalytic reactions using SWAPPS.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Control rods for light water reactors

A control rod for a nuclear fuel assembly is described herein that includes a neutron absorbing material having a melting point greater than 1500° C. that does not form a eutectic with a melting point less than 1500° C., and may further include a cladding material having a melting point greater than 1500° C. The cladding material is selected from the group consisting of silicon carbide, zirconium, a zirconium alloy, tungsten, and molybdenum. The absorbing material is selected from the group consisting of Gd2O3, Ir, B4C, Re, and Hf. The metal cladding or the absorbing material may be coated with an anti-oxidation coating of Cr with or without a Nb intermediate layer.

Lahoda, Edward J.↗

Additive manufacturing of composite neutron absorbing components

Collimators and other components for use in neutron scattering experiments or to provide neutron shielding in nuclear reactors or accelerator based neutron sources are produced by additive manufacturing from multiple different types of material, such as boron carbide (B4C), steel, isotopically enriched boron carbide (10B4C), and blends thereof.

Anderson, David C.↗

Method for producing neutron collimators using additive manufacturing

Collimators and other components for use in neutron scattering experiments or to provide neutron shielding in nuclear reactors or accelerator based neutron sources are produced by additive manufacturing from neutron absorbing material, such as boron carbide (B4C) or isotopically enriched boron carbide (10B).

Anderson, David C.↗

Equation of state of boron carbide B 4 ⁢C

We present the results of recent experiments conducted on the Sandia Z machine and a new tabular equation of state for B 4 ⁢C. The equation of state was calibrated to a combination of density functional calculations reported here and fits to preexisting data. It was constructed partly to recover the effects of a shock-driven, polymorphic phase transition of unknown character beginning at particle velocities of just under 3 km/s (shock pressures of 95 GPa). Some of the Z experiments included sound speeds determined by the overtaking rarefaction method, from which we calculate the Grüneisen parameter and compare with previous experiments conducted at the OMEGA laser [Fratanduono et al ., Phys. Rev. B 94 , 184107 (2016)], our own first principles calculations, and another recent tabular equation of state [Zhang et al ., Phys. Rev. E 102 , 053203 (2020)]. We also compare our results with previous static compression, thermophysical, and melt studies, finding mixed consistency. We predict the onset and completion of shock melting at 225 and 265 GPa, respectively, and predict a melt curve that is largely flat to pressures of several hundred GPa.

36 MATERIALS SCIENCE↗

Integral Experiment Request 554 CED-1 Summary Report

This Critical Engineering Decision 1 report for the Integral Experiment Request 554 describes the effects of adding a commercially available neutron absorber material to a known light-water low-enriched uranium assembly. The assembly in question is the Seven Percent Critical Experiments at Sandia National Laboratories. The neutron absorber plates considered for the experiment are called Boralcan, which are made of boron carbide (B 4 C) particles embedded in 1100 aluminum alloy. The concentrations of B 4 C and 1100 aluminum, as well as the thickness and size of the plates, were changed, and the fuel rod configuration was adapted to ensure that the assembly would be critical in each case studied. A total of 10 critical configurations with a neutron absorber plate inserted are described in this report. No results of high-quality integral experiments involving neutron absorbers made with B 4 C and 1100 aluminum plates are currently publicly available. Sensitivity to the neutron absorber plate material definition, isotopes, and cross sections of specific regions and configurations are also analyzed. The study results indicate that these experiments are achievable with sufficiently low uncertainties and minimal modification to the assembly. The experimental uncertainty can be further decreased with an additional characterization of the plates by x-ray computerized tomography or neutron radiography methods.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

Hardness Measurements and Interface Behavior of SiC-B 4 C-Si Multiple Phase Particulate Composites Made with Melt Infiltration and Additive Manufacturing

Reaction-bonded SiC-B 4 C-Si ceramic composites were binder jet 3D-printed and subsequently pressureless-melt-infiltrated with molten Si. The addition of B 4 C aided the Si infiltration to produce a highly dense composite. The microstructures and phases of these composites were examined. The measured hardness values of each constituent with Vickers and nanoindentation matched the bulk values, and the macro-hardness values with Knoop and spherical indentation represented the bulk, composite hardness values of all three phases together, which was close to a rule of mixtures value. For particulate-based composites, this is a significant finding. The interfacial bonds of SiC and Si were imaged using scanning transmission electron microscopy to view intimacy, whereas the crack propagation was examined with carefully placed indents. This work demonstrated that pressureless melt infiltration with a reactive particle provides a method to shape non-wetting reaction-bonded ceramic composites with limited shrinkage and high density and provides insights into the mechanical behavior with numerous indentation techniques.

36 MATERIALS SCIENCE↗