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At least 37 records · Page 2

New Oxide Ceramic Developed for Superior High-Temperature Wear Resistance

Ceramics, for the most part, do not have inherently good tribological properties. For example friction coefficients in excess of 0.7 have been reported for silicon nitride sliding on silicon nitride or on bearing steel (ref. 1). High friction is always accompanied by considerable wear. Despite their inherently poor tribological properties, the high strength and high toughness of silicon nitride (Si3N4) ceramics has led to their successful use in tribological applications (refs. 1 to 4). The upper temperature limit for the application of Si3N4 as wear-resistant material is limited by reaction with the tribological environment (ref. 3). Silicon nitride is known to produce a thin silicon dioxide film with easy shear capability that results in low friction and low wear in a moist environment (ref. 5). At elevated temperatures, the removal of the reaction product that acts as lubricant causes the friction coefficient to increase and, consequently, the wear performance to become poor. New materials are sought that will have wear resistance superior to that of Si3N4 at elevated temperatures and in harsh environments. A new class of oxide ceramic materials has been developed with potential for excellent high-temperature wear resistance. The new material consists of a multicomponent oxide with a two-phase microstructure, in which the wear resistance of the mixed oxide is significantly higher than that of the individual constituents. This is attributed to the strong constraining effects provided by the interlocking microstructures at different length scales, to the large aspect ratio of the phases, to the strong interphase bonding, and to the residual stresses. Fretting wear tests were conducted by rubbing the new ceramic material against boron carbide (B4C). The new ceramic material produced a wear track groove on B4C, suggesting significantly higher wear resistance for the oxide ceramic. The new material did not suffer from any microstructural degradation after the wear test. The wear rate of the new ceramic material at 600 C was determined to be on the order of 10-10 mm3/N-m, which is 3 to 5 orders of magnitude lower than that for the current state-of-theart wear-resistant materials (Si3N4and B4C). The friction coefficient of the new ceramic materials is on the order of 0.4, which is significantly lower than that of silicon nitride. This new class of oxide materials has shown considerable potential for applications requiring high wear resistance at high temperatures and in harsh environments. New understanding of the wear behavior of ceramic materials is emerging as a result of the surprisingly high wear resistance of two-phase oxide ceramics. There is excellent potential for further improvements in the wear resistance of oxide ceramics through optimizing the microstructure and altering the crystallographic properties of specific oxide materials as a second phase to reduce the coefficient of friction at elevated temperatures.

Sayir, Ali↗

Microstructural characterization of as-fabricated monolithic plates with boron carbide, aluminum boride, and zirconium boride burnable absorbers

The use of burnable absorbers can be beneficial for nuclear reactors by extending the fuel’s operational cycle, providing additional criticality control, and flattening the power profile. In this work, three burnable absorber materials (boron carbide, aluminum boride, and zirconium boride) embedded in aluminum have been fabricated into foils and clad in AA-6061 for potential use in high performance research reactors. The as-fabricated boron-containing phases were determined using transmission electron microscopy to be AlB2, B4C, and ZrB2. TEM also revealed weak bonding at the B4C-matrix interface. SEM showed a relatively uniform spatial distribution of boron-containing phases for all the candidate materials. Higher porosity was observed in the foil containing ZrB2 in its as-rolled condition. The porosity in the ZrB2 foil was reduced by hot isostatic pressing. The size and shape distributions of the boron-containing phases were analyzed on the criteria of cross-sectional area, perimeter, roundness, circularity, and aspect ratio. A method of converting the 2D burnable absorber dispersoids seen in cross-sectional microscopy images into 3D volumes was derived using both spherical and ellipsoidal geometry models. The difference in calculated burnable absorber dispersoid average volume between the two models ranges from 20% to 100%, which could impact burnable absorber burnout rates due to differences in neutron self-shielding.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

A comparison of ceramic and carbon-based reductants for vitrification of low-activity waste

Sucrose is the current baseline additive at the Hanford Waste Treatment and Immobilization Plant in Washington, USA to control foaming during waste feed to glass transitions and the redox state of the glass melt. Alternative reductants are being investigated to alleviate strain on effluent treatment from toxic acetonitrile production from incomplete combustion of sucrose. This study evaluates ceramic additive options including B4C, B6Si, SiC and VB2 in simulated low-activity waste feed, as well as coke dust, probing the feed volume expansion during melting as well as the gas evolution. All alternative reductant options examined significantly reduced acetonitrile production, however there was variability in their effectiveness as foam-reducing agents. VB2 and coke at the appropriate ratios were similarly effective as sucrose in controlling both foam volume and glass redox state, but with considerably less acetonitrile production. B4C, B6Si and SiC showed more promising foam control and very little acetonitrile production, however all of the final glasses were over reduced, i.e., Fe2+/FeT = 0.5. These alternative reductant studies provide operational flexibility to the operation of the vitrification plant, as well as options for alternative raw materials in industrial glass melting.

Rigby, Jessica C. (ORCID:0000000235719977)↗

Preliminary Design of Critical Experiments Involving Commercially Available B 4 C Neutron Absorber Plates with Low-Enriched UO 2 Fuel

The International Criticality Safety Benchmark Evaluation Project (ICSBEP) is an initiative to provide high-quality benchmark data in a standardized format for criticality safety analysts to use to validate calculational tools and nuclear data. In the last released 2022 version, the ICSBEP handbook contains over 5,000 critical experiment descriptions, results, and associated models. This paper describes the critical configurations proposed and calculations performed as part of the conceptual design phase of Integral Experiment Request (IER) 554 (IER-554). The goal of IER-554 is to add to the benchmark experiments available to the criticality safety community by designing critical experiments that can analyze how adding commercially available Boralcan plates to an assembly of low-enriched UO2 fuel rods affects the effective neutron multiplication factor (k eff ). Boralcan, a neutron absorber product developed by Rio Tinto, is made of B4C in an Al 1100 matrix and is commonly used for criticality suppression in fuel storage pools. In the current version of the ICSBEP handbook, only a few dated critical experiments involve B4C materials, and none involve Boralcan in a thin plate shape. The experiments designed as part of IER-554 are intended to be performed at the Sandia Pulsed Reactor Facility/Critical Experiments (SPRF/CX) apparatus at Sandia National Laboratories. SPRF/CX is a well-characterized assembly considered trustworthy by the benchmarking community because of the numerous high-quality evaluations with very low experimental uncertainties included in the ICSBEP handbook. Figure 1 illustrates the assembly for a particular configuration from LCT-078, one of the published benchmarks in the ICSBEP handbook. The experiments will be moderated and reflected by light water at ambient atmospheric pressure. Before the plates are inserted in the critical assembly, they will be characterized with x-ray computed tomography (XCT) to identify the sizes and distribution of the B 4 C powder particles inside the plates. The preliminary design calculations were performed with SCALE 6.3.0 using the KENO V.a sequence for the criticality calculations, the CE-TSUNAMI-3D sequence for the sensitivity and uncertainty studies, and the ENDF/B-VII.1 Continuous Energy cross section library. All the calculation results presented have 10 pcm statistical uncertainties. A set of critical experiments with Boralcan plates could increase the confidence of the criticality safety community in its modeling methods when using this type of neutron absorber material. Experiments would also help validate k eff calculations, and the industry could use these validations to change the B loading credit limits from the US Nuclear Regulatory Commission standard review plan for dry cask storage of spent nuclear fuel. This paper summarizes only part of the analysis documented in the preliminary design report.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Empirical Investigation of Properties for Additive Manufactured Aluminum Metal Matrix Composites

Laser additive manufacturing with mixed powders of aluminum alloy and silicon carbide (SiC) or boron carbide (B4C) is investigated in this experiment. With various mixing ratios of SiC/Al to form metal matrix composites (MMC), their mechanical and physical properties are empirically investigated. Parameters such as laser power, scan speed, scan pattern, and hatching space are optimized to obtain the highest density for each mixing ratio of SiC/Al. The mechanical and thermal properties are systematically investigated and compared with and without heat treatment. It shows that 2 wt% of SiC obtained the highest strength and Young’s modulus. Graded composite additive manufacturing (AM) of MMC is also fabricated and characterized. Various types of MMC devices, such as heat sink using graded SiC MMC and grid type three-dimensional (3D) neutron collimators using boron carbide (B4C), were also fabricated to demonstrate their feasibility for applications.

36 MATERIALS SCIENCE↗

Friction and wear of carbon-graphite materials for high energy brakes

Caliper-type brakes simulation experiments were conducted on seven different carbon-graphite material formulations against a steel disk material and against a carbon-graphite disk material. The effects of binder level, boron carbide (B4C) additions, graphite fiber additions, and graphite cloth reinforcement on friction and wear behavior were investigated. Reductions in binder level and additions of B4C each resulted in increased wear. The wear rate was not affected by the addition of graphite fibers. Transition to severe wear and high friction was observed in the case of graphite-cloth-reinforced carbon sliding against a disk of similar composition. This transition was related to the disruption of a continuous graphite shear film that must form on the sliding surfaces if low wear is to occur. The exposure of the fiber structure of the cloth constituent is believed to play a role in the shear film disruption.

Bill, R. C.↗

Friction and wear of carbon-graphite materials for high-energy brakes

Caliper type brake simulation experiments were conducted on seven different carbon graphite materials formulations against a steel disk material and against a carbon graphite disk material. The effects of binder level, boron carbide (B4C) additions, SiC additions, graphite fiber additions, and graphite cloth reinforcement on friction and wear behavior were investigated. Reductions in binder level, additions of B4C, and additions of SiC each resulted in increased wear. The wear rate was not affected by the addition of graphite fibers. Transition to severe wear and high friction was observed in the case of graphite-cloth-reinforced carbon sliding against a disk of similar composition. The transition was related to the disruption of a continuous graphite shear film that must form on the sliding surfaces if low wear is to occur.

Bill, R. C.↗

Effects of applied pressure on hot-pressing of Beta-SiC

The effects of applied pressure on the densification during hot pressing of beta-SiC compacts were investigated. Beta-SiC powder is Starck made and has the average particle size of about 0.7 micrometer. Hot pressing experiments were carried out in graphite dies at temperatures of 1700 deg to 2300 deg C and at the pressures up to 1000 kg/sq cm. The compacts containing 1 weight percent B4C were examined. Sintered compacts were examined for microstructure and the Rockwell A-scale hardness was measured. The B4C addition was very effective to mitigate the hot pressing conditions. It is found that densification goes with the strengthening of the bonding and does not occur in particle deformation due to concentrated stress.

Kinoshita, M.↗

Multielement mapping of alpha-SiC by scanning Auger microscopy

Fine second-phase particles, numerous in sintered alpha-SiC, were analyzed by scanning Auger microscopy and conventional techniques. The Auger analysis utilized computer-controlled data acquisition, multielement correlation diagrams, and a high spatial resolution of 100 nm. This procedure enabled construction of false color maps and the detection of fine compositional details within these particles. Carbon, silicon oxide, and boron-rich particles (qualitatively as BN or B4C) predominated. The BN particles, sometimes having a carbon core, are believed to result from reaction between B4C additives and nitrogen sintering atmospheres.

Browning, Ray↗

Development of Ceramic Matrix Composites For High Temperature Applications

The microstructure and mechanical properties of carbon fiber reinforced silicon carbide (C/SiC) composites that incorporated molecular-level oxidation inhibitors designed to increase the material s high temperature durability were characterized. The viability of a fiber-level inhibitor incorporated as part of a layered interface system as well as a molecularly-integrated matrix-level oxidation inhibitor that is co-deposited with the SiC matrix during Chemical Vapor Infiltration (CVI) was determined. It was expected that the inhibitor would act as a glass former that will getter the oxygen and form a crack sealant to reduce further ingress of oxygen into the composite. Three composites were examined. Composite A was a baseline C(sub f)/SiC(sub m) composite that incorporated a approx. 0.4 micron pyrolytic carbon (PyC) fiber coating to promote strength and toughness, and a CVI-derived SiC matrix. Composite B was a C(sub f)/SiC(sub m) composite incorporating a approx 0.4 micron pyrolytic carbon (PyC) fiber coating to promote strength and toughness, a approx. 0.6 micron B4C fiber-level oxidation barrier coating, and a CVI-derived SiC matrix. Composite C was a C(sub f) /SiC(sub m) composite that incorporated a approx. 0.4 micron pyrolytic carbon (PyC) fiber coating to promote strength and toughness, a approx. 0.6 micron B4C fiber-level oxidation barrier coating, and a BxC-SiC oxidation-inhibited matrix produced by CVI co-deposition. All composites were reinforced with 10 plies of T-300 balanced plain weave carbon fabric with 3K tows at 12.5 ends per inch.

Heimann, Paula↗

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↗

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↗

Nuclear safety considerations in the conceptual design of a fast reactor for space electric power and propulsion

Some nuclear safety aspects of a 3.2 mWt heat pipe cooled fast reactor with out-of-core thermionic converters are discussed. Safety related characteristics of the design including a thin layer of B4C surrounding the core, the use of heat pipes and BeO reflector assembly, the elimination of fuel element bowing, etc., are highlighted. Potential supercriticality hazards and countermeasures are considered. Impacts of some safety guidelines of space transportation system are also briefly discussed, since the currently developing space shuttle would be used as the primary launch vehicle for the nuclear electric propulsion spacecraft.

Hsieh, T.-M.↗