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At least 505 records · Page 28
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Sound speed measurements in shock-compressed cemented Tungsten carbides at pressures up to 100 GPa

To gain insights into thermodynamic states attained during shock compression of cemented tungsten carbide with 3.7 wt.% cobalt binder, we present results of longitudinal sound (release wave) speed measurements and their analysis at peak stresses up to 100 GPa (volumetric compression ratio ~ 15%). The sound speeds are determined using front-surface impact and release-wave overtake plate impact experimental configurations using laser interferometry. The measured sound speed data along with estimates for bulk sound speeds obtained using the fourth-order Birch-Murnaghan EoS and thermodynamics are used to determine the longitudinal moduli and shear moduli of shocked tungsten carbide at the various peak compression states attained in the experiments. Here, the longitudinal sound speeds were found to increase linearly with volume compression ratio from 6.97 ± 0.010 km/s at ambient conditions to 8.26 ± 0.156 km/s at a volume compression ratio of ~ 15%. The corresponding longitudinal elastic moduli also increase nearly linearly with the volume compression ratio but remain consistently lower than their theoretical predictions based on continuum models with no damage. Also, the sensitivity of shear moduli to pressure, as predicted by the Steinberg-Guinan model, is reduced substantially and the shear moduli of cemented WC with 3.7 wt.% Co remains nearly constant at ~ 310 GPa at the various peak compression stress states investigated in the present study.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Silicon carbide fiber composite receiver tubes manufactured by PIP process

The performance of SiC fiber composites made by a polymer infiltration and pyrolysis (PIP) process was investigated. Two types of tubular composites were manufactured using Hi-Nicalon and Nicalon-CG silicon carbide fibers infiltrated with SMP10 silicon carbide matrix. The fiber content in both composites was about 25 vol.% with an average density of 2.39 g/cc. The tubular SiC composites showed stable solar absorptance and emittance of 0.97 and 0.91, respectively, at 800 °C. The composites were thermally shocked at 900, 1000, and 1100 °C with a waterjet simulating raindrops. As a result, the hoop tensile strength of the composites revealed no loss of mechanical strength due to the thermal shock experiments up to 1100 °C.

14 SOLAR ENERGY↗
DOE OSTI2024

Compositionally complex carbide ceramics: A perspective on irradiation damage

Extensive experimental and computational studies have demonstrated outstanding physical and chemical properties of the novel materials of compositionally complex carbides (CCCs), enabling their promising applications in advanced fission and fusion energy systems. This perspective provides a comprehensive overview of radiation damage behavior reported in the literature to understand the fundamental mechanisms related to the impact of multi-principal metal components on phase stability, irradiation-induced defect clusters, irradiation hardening, and thermal conductivity of compositionally complex carbides. Several future research directions are recommended to critically evaluate the feasibility of designing and developing new ceramic materials for extreme environments using the transformative “multi-principal component” concept. Compared to the existing materials for nuclear applications including stainless steels, nickel alloys, ZrC, SiC, and potentially high-entropy alloys, as well as certain other compositionally complex ceramic families. CCCs appear to be more resistant to amorphization, growth of irradiation defect clusters, and void swelling.

36 MATERIALS SCIENCE↗
DOE OSTI2012

SULFUR MOLECULE CHEMISTRY IN SUPERNOVA EJECTA RECORDED BY SILICON CARBIDE STARDUST

We studied about 3400 presolar silicon carbide (SiC) grains from the Murchison CM2 meteorite for C- and Si-isotopic compositions. Among these grains we identified 7 unusual or type C SiC (U/C) grains, characterized by isotopically heavy Si, and 36 supernova type X SiC grains, characterized by isotopically light Si. Selected U/C and X grains were also measured for S-, Mg-Al-, and Ca-Ti-isotopic compositions. We show that the U/C grains incorporated radioactive {sup 44}Ti, which is evidence that they formed in the ejecta of Type II supernova (SNII) explosions. Abundances of radioactive {sup 26}Al and {sup 44}Ti are compatible with those observed in X grains. U/C and X grains carry light S with enrichments in {sup 32}S of up to a factor of 2.7. The combination of heavy Si and light S observed in U/C grains is not consistent with abundance predictions of simple supernova models. The isotope data suggest preferential trapping of S from the innermost supernova zones, the production site of radioactive {sup 44}Ti, by the growing silicon carbide particles. A way to achieve this is by sulfur molecule chemistry in the still unmixed ejecta. This confirms model predictions of molecule formation in SNII ejecta and shows that sulfur molecule chemistry operates in the harsh and hot environments of stellar explosions.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2013

SILICON CARBIDE GRAINS OF TYPE C PROVIDE EVIDENCE FOR THE PRODUCTION OF THE UNSTABLE ISOTOPE {sup 32}Si IN SUPERNOVAE

Carbon-rich grains are observed to condense in the ejecta of recent core-collapse supernovae (SNe) within a year after the explosion. Silicon carbide grains of type X are C-rich grains with isotopic signatures of explosive SN nucleosynthesis have been found in primitive meteorites. Much rarer silicon carbide grains of type C are a special sub-group of SiC grains from SNe. They show peculiar abundance signatures for Si and S, isotopically heavy Si, and isotopically light S, which appear to be in disagreement with model predictions. We propose that C grains are formed mostly from C-rich stellar material exposed to lower SN shock temperatures than the more common type X grains. In this scenario, extreme {sup 32}S enrichments observed in C grains may be explained by the presence of short-lived {sup 32}Si ({tau}{sub 1/2} = 153 yr) in the ejecta, produced by neutron capture processes starting from the stable Si isotopes. No mixing from deeper Si-rich material and/or fractionation of Si from S due to molecular chemistry is needed to explain the {sup 32}S enrichments. The abundance of {sup 32}Si in the grains can provide constraints on the neutron density reached during the SN explosion in the C-rich He shell material. The impact of the large uncertainty of the neutron capture cross sections in the {sup 32}Si region is discussed.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2015

Hydrogen desorption from hydrogen fluoride and remote hydrogen plasma cleaned silicon carbide (0001) surfaces

Due to the extreme chemical inertness of silicon carbide (SiC), in-situ thermal desorption is commonly utilized as a means to remove surface contamination prior to initiating critical semiconductor processing steps such as epitaxy, gate dielectric formation, and contact metallization. In-situ thermal desorption and silicon sublimation has also recently become a popular method for epitaxial growth of mono and few layer graphene. Accordingly, numerous thermal desorption experiments of various processed silicon carbide surfaces have been performed, but have ignored the presence of hydrogen, which is ubiquitous throughout semiconductor processing. In this regard, the authors have performed a combined temperature programmed desorption (TPD) and x-ray photoelectron spectroscopy (XPS) investigation of the desorption of molecular hydrogen (H{sub 2}) and various other oxygen, carbon, and fluorine related species from ex-situ aqueous hydrogen fluoride (HF) and in-situ remote hydrogen plasma cleaned 6H-SiC (0001) surfaces. Using XPS, the authors observed that temperatures on the order of 700–1000 °C are needed to fully desorb C-H, C-O and Si-O species from these surfaces. However, using TPD, the authors observed H{sub 2} desorption at both lower temperatures (200–550 °C) as well as higher temperatures (>700 °C). The low temperature H{sub 2} desorption was deconvoluted into multiple desorption states that, based on similarities to H{sub 2} desorption from Si (111), were attributed to silicon mono, di, and trihydride surface species as well as hydrogen trapped by subsurface defects, steps, or dopants. The higher temperature H{sub 2} desorption was similarly attributed to H{sub 2} evolved from surface O-H groups at ∼750 °C as well as the liberation of H{sub 2} during Si-O desorption at temperatures >800 °C. These results indicate that while ex-situ aqueous HF processed 6H-SiC (0001) surfaces annealed at <700 °C remain terminated by some surface C–O and Si–O bonding, they may still exhibit significant chemical reactivity due to the creation of surface dangling bonds resulting from H{sub 2} desorption from previously undetected silicon hydride and surface hydroxide species.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Nonlinear-optical and structural properties of nanocrystalline silicon carbide films

The aim of this study is to investigate the nonlinearity of refraction in nanostructured silicon carbide films depending on their structural features (synthesis conditions for such films, substrate temperature during their deposition, concentration of the crystalline phase in the film, Si/C ratio of atomic concentrations in the film, and size of SiC nanocrystals formed in the film). The corresponding dependences are obtained, as well as the values of nonlinear-optical third-order susceptibility {chi}{sup (3)}({omega}; {omega}, -{omega}, {omega}) for various silicon polytypes (3C, 21R, and 27R) which exceed the value of {chi}{sup (3)} in bulk silicon carbide single crystals by four orders of magnitude.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Boron carbide coating deposition on tungsten and testing of tungsten layers and coating under intense plasma load

A device intended for boron carbide coating deposition and material testing under high heat loads is presented. A boron carbide coating 5 μm thick was deposited on the tungsten substrate. These samples were subjected to thermocycling loads in the temperature range of 400–1500°C. Tungsten layers deposited on tungsten substrates were tested in similar conditions. Results of the surface analysis are presented.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Electronic states in epitaxial graphene fabricated on silicon carbide

An analytical expression for the density of states of a graphene monolayer interacting with a silicon carbide surface (epitaxial graphene) is derived. The density of states of silicon carbide is described within the Haldane-Anderson model. It is shown that the graphene-substrate interaction results in a narrow gap of {approx}0.01-0.06 eV in the density of states of graphene. The graphene atom charge is estimated; it is shown that the charge transfer from the substrate is {approx}10{sup -3}-10{sup -2}e per graphene atom.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Cobalt Intercalation of Graphene on Silicon Carbide

In this paper, we studied cobalt intercalation of single-layer graphene grown on the 4H-SiC(0001) polytype. The experiments were carried out in situ under ultrahigh vacuum conditions by high energy resolution photoelectron spectroscopy using synchrotron radiation and low energy electron diffraction. The nominal thicknesses of the deposited cobalt layers varied in the range of 0.2–5 nm, while the sample temperature was varied from room temperature to 800°C. Unlike Fe films, the annealing of Co films deposited on graphene at room temperature is shown to not intercalate graphene by cobalt. The formation of the graphene–cobalt–SiC intercalation system was detected upon deposition of Co atoms on samples heated to temperatures of above ~400°C. Cobalt films with a thickness up to 2 nm under graphene are formed using this method, and they are shown to be magnetized along the surface at thicknesses of greater than 1.3 nm. Graphene intercalation by cobalt was found to be accompanied by the chemical interaction of Co atoms with silicon carbide leading to the synthesis of cobalt silicides. At temperatures of above 500°C, the growth of cobalt films under graphene is limited by the diffusion of Co atoms into the bulk of silicon carbide.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2019

On the Adsorption of Gases on Silicon Carbide: Simple Estimates

The adsorption of atomic and molecular nitrogen and ammonia on silicon carbide is considered within two physically different (solid-state and quantum-chemical) approaches. In the solid-state approach, the Haldane–Anderson model is used for the density of states of the SiC 4H and 6H polytypes to demonstrate that the energy of binding to the substrate is 6 and 3 eV for N atoms and N{sub 2} molecule, respectively. In the quantum-chemical approach, the model of a surface diatomic molecule is used to find that the binding energy of atomic nitrogen is 6 and 4 eV for adsorption on the C- and Si-edges, respectively. It has been established that the charge transfer between an adsorbate and the substrate may be neglected in all the considered cases. It has been hypothesized that the dissociation of a molecule with the further passivation of its dangling sp{sup 3}-orbitals with hydrogen atoms takes place for silicon carbide as in the case of ammonia adsorption on Si(100).

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

The Influence of the Cobalt Content on the Strength Properties of Tungsten Carbide Ceramics under Dynamic Loads

Based on the registration and analysis of the full wave profiles, the Hugoniot elastic limit and spall strength of ceramics based on tungsten carbide with different cobalt content are measured. We also study the influence of the cobalt content on the mechanical characteristics of tungsten carbide such as hardness, fracture strength, Young’s modulus, shear modulus, and sound velocity. It is shown that in the process of spalling, the failure stresses grow and the dynamic elastic limit decreases almost linearly within the scatter of their values with growing cobalt content; moreover, the value of the Hugoniot elastic limit is abruptly practically halved as the cobalt content grows from 0 to 2 wt %.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

A Vacuum-Free Method for Producing Cubic Titanium Carbide in the Plasma of Low-Voltage Direct-Current Arc Discharge

The results of a study on the production of cubic titanium carbide in direct-current arc discharge plasma initiated in open air are presented. A feature of the method is its implementation without the use of gas or liquid protective media preventing the oxidation of products and initial reagents with air oxygen. According to the X-ray diffraction data, graphite gC, hexagonal titanium α-Ti, and cubic titanium carbide TiC are identified in the composition of the powder product. The TiC particles are represented by objects with a regular characteristic cut and sizes from units to tens of micrometers.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Silicon Carbide Temperature Monitor Processing Improvements. Status Report

Silicon carbide (SiC) temperature monitors are used as temperature sensors in Advanced Test Reactor (ATR) irradiations at the Idaho National Laboratory (INL). Although thermocouples are typically used to provide real-time temperature indication in instrumented lead tests, other indicators, such as melt wires, are also often included in such tests as an independent technique of detecting peak temperatures incurred during irradiation. In addition, less expensive static capsule tests, which have no leads attached for real-time data transmission, often rely on melt wires as a post-irradiation technique for peak temperature indication. Melt wires are limited in that they can only detect whether a single temperature is or is not exceeded. SiC monitors are advantageous because a single monitor can be used to detect for a range of temperatures that occurred during irradiation. As part of the process initiated to make SiC temperature monitors available at the ATR, post-irradiation evaluations of these monitors have been previously completed at the High Temperature Test Laboratory (HTTL). INL selected the resistance measurement approach for determining irradiation temperature from SiC temperature monitors because it is considered to be the most accurate measurement. The current process involves the repeated annealing of the SiC monitors at incrementally increasing temperature, with resistivity measurements made between annealing steps. The process is time consuming and requires the nearly constant attention of a trained staff member. In addition to the expensive and lengthy post analysis required, the current process adds many potential sources of error in the measurement, as the sensor must be repeatedly moved from furnace to test fixture. This time-consuming post irradiation analysis is a significant portion of the total cost of using these otherwise inexpensive sensors. An additional consideration of this research is that, if the SiC post processing can be automated, it could be performed in an MFC hot cell, further reducing the time and expense of lengthy decontaminations prior to processing. Sections of this report provide a general description of resistivity techniques currently used to infer peak irradiation temperature from silicon carbide temperature monitors along with some representative data, the proposed concepts to improve the process of analyzing irradiated SiC temperature monitors, the completed efforts to prove the proposed concepts, and future activities. The efforts detailed here succeeded in designing and developing a real-time automated SiC resistivity measurement system, and performed two initial test runs. Activities carried out include the assembly and integration of the system hardware; the design and development of a preliminary monitor fixture; the design of a technique to automate the data analysis and processing; the development of the communication, coordination, and user software; and the execution and troubleshooting of test run experiments using the box furnace. Although the automation system performed as required, the designed fixture did not succeed in establishing the needed electrical contacts with the SiC monitor.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2017

Innovative coating of nanostructured vanadium carbide on the F/M cladding tube inner surface for mitigating the fuel cladding chemical interactions

Fuel cladding chemical interactions (FCCI) have been acknowledged as a critical issue in a metallic fuel/steel cladding system due to the formation of low melting intermetallic eutectic compounds between the fuel and cladding steel, resulting in reduction in cladding wall thickness as well as a formation of eutectic compounds that can initiate melting in the fuel at lower temperature. In order to mitigate FCCI, diffusion barrier coatings on the cladding inner surface have been considered. In order to generate the required coating techniques, pack cementation, electroplating, and electrophoretic deposition have been investigated. However, these methods require a high processing temperature of above 700 oC, resulting in decarburization and decomposition of the martensites in a ferritic/martensitic (F/M) cladding steel. Alternatively, organometallic chemical vapor deposition (OMCVD) can be a promising process due to its low processing temperature of below 600 oC. The aim of the project is to conduct applied and fundamental research towards the development of diffusion barrier coatings on the inner surface of F/M fuel cladding tubes. Advanced cladding steels such as T91, HT9 and NF616 have been developed and extensively studied as advanced cladding materials due to their excellent irradiation and corrosion resistance. However, the FCCI accelerated by the elevated temperature and high neutron exposure anticipated in fast reactors, can have severe detrimental effects on the cladding steels through the diffusion of Fe into fuel and lanthanides towards into the claddings. To test the functionality of developed coating layer, the diffusion couple experiments were focused on using T91 as cladding and Ce as a surrogate lanthanum fission product. By using the customized OMCVD coating equipment, thin and compact layers with a few micron between 1.5 µm and 8 µm thick and average grain size of 200 nm and 5 µm were successfully obtained at the specimen coated between 300oC and 500 oC, respectively. The coating layer contains both carbon and vanadium elements as quantified by WED, and the phases mainly consist of a mixture of V2C and VC, which was confirmed using X-ray diffraction patterns. In addition, the ratio between V and C varies with processing temperature, and it was observed that a higher temperature promotes the carbon adsorption and increases thickness of the coating. With optimized deposition conditions, we can apply the coating technique toward the actual T91 cladding materials, and provide the possibilities for the real application in sodium-cooled fast reactors (SFRs). Diffusion couple experiments were performed at both 550 oC and 690 oC, which corresponds to normal and aggressive operating temperatures, respectively. The results show that vanadium carbide coating with wider thickness (8 µm) and lower carbon concentration (27 at.%) reduced the width of the inter diffusion region, indicating that vanadium carbide coating can mitigate FCCI effectively. In specific, inter-diffusion between Fe and Ce was prohibited over most area, but Ce diffusion occurred toward the coating and the Fe substrate through thinner coating layer, which needs further optimization in terms of uniform coating thickness. Overall, it is concluded that this coating process can be successfully applied onto the inner surface of HT9 cladding tubes and the FCCI can be effectively mitigated if not totally eliminated.

36 MATERIALS SCIENCE↗
DOE OSTI2020

3D Printing with Mixed Powders of Boron Carbide and Al Alloy

Laser additive manufacturing with mixed powders of boron carbide and aluminum alloy is investigated. Parameters such as laser power, scan speed, scan pattern, and hatching space are systematically evaluated and optimized to obtain the desired density and porosity. These results show that the AM part contains 20 wt% boron carbide and 80 wt% aluminum alloy, which are well mixed and synthesized during the melting process. Its mechanical properties are close to those of aluminum. A thin-wall structure based two dimensional and three dimensional radial collimators were fabricated with well-controlled geometry for neutron scattering measurement.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Carbide-Modified Pd on ZrO2 as Active Phase for CO2-Reforming of Methane—A Model Phase Boundary Approach

Starting from subsurface Zr0-doped “inverse” Pd and bulk-intermetallic Pd0Zr0 model catalyst precursors, we investigated the dry reforming reaction of methane (DRM) using synchrotron-based near ambient pressure in-situ X-ray photoelectron spectroscopy (NAP-XPS), in-situ X-ray diffraction and catalytic testing in an ultrahigh-vacuum-compatible recirculating batch reactor cell. Both intermetallic precursors develop a Pd0–ZrO2 phase boundary under realistic DRM conditions, whereby the oxidative segregation of ZrO2 from bulk intermetallic PdxZry leads to a highly active composite layer of carbide-modified Pd0 metal nanoparticles in contact with tetragonal ZrO2. This active state exhibits reaction rates exceeding those of a conventional supported Pd–ZrO2 reference catalyst and its high activity is unambiguously linked to the fast conversion of the highly reactive carbidic/dissolved C-species inside Pd0 toward CO at the Pd/ZrO2 phase boundary, which serves the role of providing efficient CO2 activation sites. In contrast, the near-surface intermetallic precursor decomposes toward ZrO2 islands at the surface of a quasi-infinite Pd0 metal bulk. Strongly delayed Pd carbide accumulation and thus carbon resegregation under reaction conditions leads to a much less active interfacial ZrO2–Pd0 state.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Multiscale Modeling of Silicon Carbide Cladding for Nuclear Applications: Thermal Performance Modeling

The complex multiscale and anisotropic nature of silicon carbide (SiC) ceramic matrix composite (CMC) makes it difficult to accurately model its performance in nuclear applications. The existing models for nuclear grade composite SiC do not account for the microstructural features and how these features can affect the thermal and structural behavior of the cladding and its anisotropic properties. In addition to the microstructural features, the properties of individual constituents of the composites and fiber tow architecture determine the bulk properties. Models for determining the relationship between the individual constituents’ properties and the bulk properties of SiC composites for nuclear applications are absent, although empirical relationships exist in the literature. Here, a hierarchical multiscale modeling approach was presented to address this challenge. This modular approach addressed this difficulty by dividing the various aspects of the composite material into separate models at different length scales, with the evaluated property from the lower-length-scale model serving as an input to the higher-length-scale model. The multiscale model considered the properties of various individual constituents of the composite material (fiber, matrix, and interphase), the porosity in the matrix, the fiber volume fraction, the composite architecture, the tow thickness, etc. By considering inhomogeneous and anisotropic contributions intrinsically, our bottom-up multiscale modeling strategy is naturally physics-informed, bridging constitutive law from micromechanics to meso-mechanics and structural mechanics. The effects that these various physical attributes and thermo-physical properties have on the composite’s bulk thermal properties were easily evaluated and demonstrated through the various analyses presented herein. Since silicon carbide fiber-reinforced SiC CMCs are also promising thermal–structural materials with a broad range of high-end technology applications beyond nuclear applications, we envision that the multiscale modeling method we present here may prove helpful in future efforts to develop and construct reinforced CMCs and other advanced composite nuclear materials, such as MAX phase materials, that can service under harsh environments of ultrahigh temperatures, oxidation, corrosion, and/or irradiation.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗