Results for “SiC” — Page 11

DOE OSTI2025

Develop Accurate Techniques for Passive SiC Temperature Monitoring of Miniature Samples for Cross-Cutting Applications

Passive thermometry is critically important because most fuels and materials irradiation experiments are not instrumented, and it is necessary to understand the irradiation temperature to properly interpret any post-irradiation examination data, including evolving properties and/or microstructures. The standard passive thermometry approach uses continuous dilatometry to evaluate changes in the instantaneous coefficient of thermal expansion during post-irradiation thermal annealing. This approach has limitations in terms of sample size (minimum length requirements) and the maximum irradiation temperature that can be accurately determined, which is limited by the reduced swelling (and therefore recovery) following higher temperature irradiation and limitations on the furnaces used with push-rod dilatometers. This work evaluates two new proposed techniques for post-irradiation evaluation of passive SiC temperature monitors: differential scanning calorimetry (DSC) and Raman spectroscopy. DSC is an extremely sensitive technique that can be used for any specimen geometry and is capable of higher temperature operation. Raman spectroscopy is similar in that it is a surface technique capable of examining extremely small samples (submillimeter), can be used with a heated stage up to 1,500°C (planned for future work), and is capable of mapping local irradiation temperatures throughout a sample. Existing SiC samples that were previously irradiated over a wide range of temperatures were cut into multiple pieces to allow for annealing studies using multiple different techniques: dilatometry, DSC, and Raman spectroscopy. This approach mitigates the concern that samples analyzed using one technique may have a slightly different irradiation history than those analyzed using a different technique. Recovery was clearly observed during annealing using both DSC and dilatometry. In some cases, a direct comparison could not be made due to some of the DSC runs accidentally including material from multiple specimens and issues with using an alternative DSC sample holder for the highest temperature annealing studies. Nevertheless, one trend was clear: the DSC runs resulted in higher irradiation temperatures compared to those of the dilatometry runs. Part of this could be attributed to the higher temperature ramp rates used during the DSC runs, which are often preferred to reduce noise in the measurements. By comparison, dilatometry has previously been shown to produce better data at lower ramp rates. Future work should further investigate the ideal ramp rate for both techniques to produce consistent results. Additional work should evaluate the best holder material to use for DSC runs exceeding 1,000°C to provide reliable data while preventing interactions between SiC and the holder.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRSDate not supplied

Recent Progress in Extreme Environment Durable SiC JFET-R Integrated Circuit Technology

This work updates recent progress made by NASA Glenn Research Center on further advancement of its uniquely durable silicon carbide junction field effect transistor and resistor (SiC JFET-R) integrated circuit (IC) technology since HiTEC 2021. Key fabrication process improvements compared to earlier NASA Glenn IC prototype runs have been ascertained via extensive “back end of line” (BEOL) processing experiments conducted on practice wafers over the past two years. The resulting changes to the BEOL process flow employed in the fabrication of “Generation 12” SiC JFET-R wafers are described. The NASA Glenn SiC JFET-R IC prototype “Generation 12” chipset design realizes significantly higher complexity digital and analog integrated ICs aimed at flexibly implementing a broad variety of mission-enabling extreme-environment electronics demonstrations. SPICE simulations have verified circuit designs ranging from simple amplification of analog sensor signals up through long-duration Venus lander operations and microprocessor-based of electric motor drive.

Silicon Carbide↗

NASA NTRSDate not supplied

Recent Progress in Extreme Environment Durable SiC JFET-R Integrated Circuit Technology

This work updates recent progress made by NASA Glenn Research Center on further advancement of its uniquely durable silicon carbide junction field effect transistor and resistor (SiC JFET-R) integrated circuit (IC) technology since HiTEC 2021. Key fabrication process improvements compared to earlier NASA Glenn IC prototype runs have been ascertained via extensive “back end of line” (BEOL) processing experiments conducted on practice wafers over the past two years. The resulting changes to the BEOL process flow employed in the fabrication of “Generation 12” SiC JFET-R wafers are described. The NASA Glenn SiC JFET-R IC prototype “Generation 12” chipset design realizes significantly higher complexity digital and analog integrated ICs aimed at flexibly implementing a broad variety of mission-enabling extreme-environment electronics demonstrations. SPICE simulations have verified circuit designs ranging from simple amplification of analog sensor signals up through long-duration Venus lander operations and microprocessor-based of electric motor drive.

Silicon Carbide↗

NASA NTRS2023

Recent Progress in Extreme Environment Durable SiC JFET-R Integrated Circuit Technology

This work updates recent progress made by NASA Glenn Research Center on further advancement of its uniquely durable silicon carbide junction field effect transistor and resistor (SiC JFET-R) integrated circuit (IC) technology since HiTEC 2021. Key fabrication process improvements compared to earlier NASA Glenn IC prototype runs have been ascertained via extensive “back end of line” (BEOL) processing experiments conducted on practice wafers over the past two years. The resulting changes to the BEOL process flow employed in the fabrication of “Generation 12” SiC JFET-R wafers are described. The NASA Glenn SiC JFET-R IC prototype “Generation 12” chipset design realizes significantly higher complexity digital and analog integrated ICs aimed at flexibly implementing a broad variety of mission-enabling extreme-environment electronics demonstrations. SPICE simulations have verified circuit designs ranging from simple amplification of analog sensor signals up through long-duration Venus lander operations and microprocessor-based of electric motor drive.

Silicon Carbide↗

DOE OSTI2024

Negative thermal expansion coefficient and amorphization in defective 4H-SiC

This paper presents thermal expansion coefficient (TEC) and amorphization in 4H-SiC containing point defects at different concentrations. We considered vacancy defects, interstitial defects, and Frenkel pair defects and investigated the thermomechanical response of the lattice over a wide range of temperatures using classical molecular dynamics simulations. The results show that 4H-SiC with vacancy defects exhibits a negative TEC above a critical defect density of around 9% (irrespective of the temperature). With interstitial defects, it exhibits a positive TEC (regardless of the defect density), and with Frenkel pair defects it shows a transition from positive TEC to negative TEC for a defect density greater than 8%. The coupling between temperature-induced expansion and defect-introduced stress in the lattice forms the mechanistic basis for the observed variation in TEC. Furthermore, the specific heat decreases rapidly with an increase in defect density at room temperature, with the highest sensitivity of the lattice observed for the Frenkel pair defects followed by interstitial defects and then by vacancy defects. Finally, these findings highlight the critical implications of defects on thermal expansion behavior of 4H-SiC with applications in radiation environments.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Environmental barrier coatings on SiC without a silicon bond coating: oxidation resistance, failure modes, and future improvements

Environmental barrier coatings (EBCs) are used to mitigate chemical reactions between SiC ceramic matrix composite (CMC) components and the H 2 O in combustion gas in turbine hot sections. CMCs are currently temperature-limited by the Si-bond coating, which melts at ~ 1414 °C. This work explores EBCs where the bond coating was removed to achieve higher operating temperatures. Various versions of enhanced roughness SiC were utilized to improve EBC adhesion to the substrates prior to 1 h furnace cycle testing in steam at 1250–1425 °C. The enhanced SiC roughness resulted in short coating lifetimes as the roughness was oxidized away with SiO 2 formation. Further, isothermal furnace exposures at 1400–1600 °C showed Yb 2 Si 2 O 7 /Yb 2 SiO 5 EBC microstructural changes, resulting in premature debonding from the substrates. Finally, this work provides baseline requirements for the development of both next-generation EBCs and bond coating strategies to overcome the current limitation of the Si-bond coating melting temperature.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Influence of temperature, oxygen partial pressure, and microstructure on the high-temperature oxidation behavior of the SiC Layer of TRISO particles

Tristructural isotropic (TRISO)-coated fuel particles are designed for use in high-temperature gas-cooled nuclear reactors, featuring a structural SiC layer that may be exposed to oxygen-rich environments over 1000 °C. Surrogate TRISO particles were tested in 0.2–20 kPa O 2 atmospheres to observe the differences in oxidation behavior. Oxide growth mechanisms remained consistent from 1200–1600 °C for each P O$_2$ , with activation energies of 228 ± 7 kJ/mol for 20 kPa O 2 and 188 ± 8 kJ/mol for 0.2 kPa O 2 . At 1600 °C, kinetic analysis revealed a change in oxide growth mechanisms between 0.2 and 6 kPa O2. In 0.2 kPa O 2 , oxidation produced raised oxide nodules on pockets with nanocrystalline SiC. Oxidation mechanisms were determined using Atom probe tomography. Active SiC oxidation occurred in C-rich grain boundaries with low P O$_2$ , leading to SiO 2 buildup in porous nodules. Here, this phenomenon was not observed at any temperature in 20 kPa O 2 environments.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2026

Influence of silicon infiltration conditions on microstructure and mechanical properties in binder jet 3D printed SiC

Atmosphere, temperature, and hold time were varied for silicon infiltrated binder jet 3D printed SiC preforms. A two-step infiltration process optimized infiltration. The first step at 1450 °C under vacuum facilitated improved wetting. The second step at elevated temperature in argon advanced infiltration while suppressing vaporization. Variation of the second-step temperature (1550–1750 °C) and hold time revealed that 1550 °C for 1 h in argon following initial vacuum treatment yielded the highest silicon uptake ratio (∼96 %) with minimal residual porosity and strengths of 150–180 MPa. Flexural strength was either stable or improved with elevated temperatures up to 1000°C. In contrast, higher temperatures or extended hold times led to increased silicon vaporization and pores. The optimized process was applied to formulations with extra carbon to enhance SiC content and interconnectedness through reaction bonding, which corresponded to increased flexural strength. These findings provide guidance for silicon infiltration in additively manufactured SiC.

Yoon, Bola [ORNL] (ORCID:0000000260875373)↗

DOE OSTI2026

Pitfalls in parameters: practical process development in chemical vapor processing of SiC

Vapor processing of high-value materials, such as silicon carbide (SiC), is of interest for many industries, including aerospace and energy production. Chemical vapor infiltration (CVI) of additively manufactured components is an especially attractive manufacturing process currently in development. Here, a novel development workflow is demonstrated with the H 2 –CH 3 SiCl 3 gas system for SiC to accelerate the process optimization of CVI SiC. A combination of calculated thermodynamics and high-throughput experimental chemical vapor deposition (CVD) coatings substantially reduced the experiments required with slow CVI processes. The computational results accurately predicted changes in the thermodynamic conditions tested, while CVD coatings – characterized by Raman spectroscopy – addressed changes in kinetic parameters. This workflow is also applicable to other vapor-processing systems, such as pyrolytic carbon, ZrC, or Si 3 N 4 .

Lamm, Benjamin W. [Oak Ridge National Laboratory (↗

DOE OSTI2024

A Low-Profile Gate Power Supply for a SiC Phase Leg with Reduced Isolation Capacitance

Gate driver power supply (GDPS) for SiC devices needs power to 5 W as the switching frequency increases to hundreds of kHz. Resonant converters with planar magnetics demand GDPS with a lower profile. Also, the isolation capacitance (Cp) needs to be minimized for SiC devices with high dv/dt. This paper proposed a planar 5 W*2, 20 V isolated gate power supply for a SiC phase leg in the EV traction inverter. Air-core magnetics with PCB windings are applied for low profile. A single-switch resonant Class-E topology is proposed with zero-voltage switching at 6.78 MHz to minimize the magnetics footprint for a 6 pF Cp. Compared with commercial power supplies with similar power, the proposed power supply reduced the profile and Cp by more than half without sacrificing its efficiency and power density.

Li, Bo↗

DOE OSTI2025

Develop Accurate Techniques for Passive SiC Temperature Monitoring of Miniature Samples for Cross-Cutting Applications

Passive thermometry is critically important because most fuels and materials irradiation experiments are not instrumented, and it is necessary to understand the irradiation temperature to properly interpret any post-irradiation examination data, including evolving properties and/or microstructures. The standard passive thermometry approach uses continuous dilatometry to evaluate changes in the instantaneous coefficient of thermal expansion during post-irradiation thermal annealing. This approach has limitations in terms of sample size (minimum length requirements) and the maximum irradiation temperature that can be accurately determined, which is limited by the reduced swelling (and therefore recovery) following higher temperature irradiation and limitations on the furnaces used with push-rod dilatometers. This work evaluates two new proposed techniques for post-irradiation evaluation of passive SiC temperature monitors: differential scanning calorimetry (DSC) and Raman spectroscopy. DSC is an extremely sensitive technique that can be used for any specimen geometry and is capable of higher temperature operation. Raman spectroscopy is similar in that it is a surface technique capable of examining extremely small samples (submillimeter), can be used with a heated stage up to 1,500°C (planned for future work), and is capable of mapping local irradiation temperatures throughout a sample. Existing SiC samples that were previously irradiated over a wide range of temperatures were cut into multiple pieces to allow for annealing studies using multiple different techniques: dilatometry, DSC, and Raman spectroscopy. This approach mitigates the concern that samples analyzed using one technique may have a slightly different irradiation history than those analyzed using a different technique. Recovery was clearly observed during annealing using both DSC and dilatometry. In some cases, a direct comparison could not be made due to some of the DSC runs accidentally including material from multiple specimens and issues with using an alternative DSC sample holder for the highest temperature annealing studies. Nevertheless, one trend was clear: the DSC runs resulted in higher irradiation temperatures compared to those of the dilatometry runs. Part of this could be attributed to the higher temperature ramp rates used during the DSC runs, which are often preferred to reduce noise in the measurements. By comparison, dilatometry has previously been shown to produce better data at lower ramp rates. Future work should further investigate the ideal ramp rate for both techniques to produce consistent results. Additional work should evaluate the best holder material to use for DSC runs exceeding 1,000°C to provide reliable data while preventing interactions between SiC and the holder.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS1982

Microstructure and property characterization of sintered Si3N4, SiC, and SiAlON

Commercially-produced, pressureless sintered Si3N4, SiC, and SiAlON were characterized with respect to density, phases present, bend strength, and oxidation resistance. The room-temperature bend strengths of sintered Si3N4, SiC, and SiAlON are comparable. However, the room-temperature strengths are much lower (approximately 40 to 50%) than the room-temperature strength of hot-pressed Si3N4 (NC-132). The strength loss in Si3N4 and SiAlON materials at high temperature was attributed to a viscous grain-boundary phase, retained during cooling from the sintering temperature. The oxidation resistance of sintered alpha-SiC was the best of any materials tested.

Dutta, S.↗

NASA NTRS1985

Hot corrosion of sintered alpha-SiC at 1000 C

The hot corrosion of sintered alpha-SiC by thin films of Na2SO4 and Na2CO3 was studied at 1000 C in controlled gas atmospheres. Under all conditions, corrosion led to 10 to 20 times the amount of SiO2 formed in pure oxidation after a 48-h exposure. In addition, small amounts of sodium silicate formed. Melts of Na2SO4/SO3 caused uniform pitting of the SiC substrate; Na2CO3/CO2 melts caused localized pitting and grain-boundary attack. In all cases, the protective SiO2 layer dissolved to form silicate, leading to corrosion. In the sulfate case, free carbon in the SiC promotes this process. In all cases the presence of liquid films is responsible for rapid transport rates and the subsequent rapid reaction.

Jacobson, N. S.↗

NASA NTRS1985

Molten salt corrosion of SiC: Pitting mechanism

Thin films of Na2SO4 and Na2CO3 at 1000 C lead to severe pitting of sintered alpha-SiC. These pits are important as they cause a strength reduction in this material. The growth of product layers is related to pit formation for the Na2CO3 case. The early reaction stages involve repeated oxidation and dissolution to form sodium silicate. This results in severe grain boundary attack. After this a porous silica layer forms between the sodium silicate melt and the SiC. The pores in this layer appear to act as paths for the melt to reach the SiC and create larger pits.

Jacobson, N. S.↗

NASA NTRS1985

Non-equilibrium phase distribution in an Al-SiC composite

The phase distribution in an Al-SiC composite has been investigated using high resolution analytical electron microscopy. Particular attention was focused on Al-SiC interfaces, matrix boundaries and impurity phases which would impede the easy glide of dislocations. Small crystallites of MgO were distributed singly and in clusters along Al-SiC interfaces in all specimens. Interfacial segregation and precipitation involving alloy species apparently affected precipitation in the matrix, where the distribution of phases was found to be very heterogeneous. Matrix phases also included unusually large constituent particles and dispersoids, a consequence of the composite processing methods. The relationship between the observed microstructure and the composite mechanical behavior reported by others is discussed. The heterogeneous distribution of matrix phases is expected to result in a wide variaiton in local yield stress and local work-hardening rate within the composite.

Nutt, S. R.↗

NASA NTRS1985

Microstructure and fracture in SiC whisker reinforced 2124 aluminum composite

The microstructures of extruded and hot-rolled 2124 Al-15 percent (by weight) SiC whisker composites have been investigated, experimentally. Among the specific factors studied were: the strength of the whisker-matrix interfaces; (2) the presence of oxides; (3) the presence of defective whiskers; (4) and the presence of distribution of intermetallic compounds, impurities in the SiC(w) powder, and microstructural inhomogeneities. Modifications in the microstructure of the SiC/AL composites due to hot rolling and extrusion are illustrated in a series of microphotographs. It was found that hot rolling along the axis of extrusion was associated with some types of whisker damage, while the whiskers still retain their original orientation. Hot-rolling perpendicular to the axis of extrusion, however, tended to rotate the whiskers and produced a nearly isotropic material. Whisker free zones were virtually eliminated or reduced in size by hot rolling. In situ Auger fractography of the composite showed that the interfacial bonding between the SiC and the Al matrix was good and that Al2O2 had no significant influence on the fracture mechanics of the composite.

Nieh, T. G.↗

NASA NTRS1985

Processing of laser formed SiC powder

Superior SiC characteristics can be achieved through the use of ideal constituent powders and careful post-synthesis processing steps. High purity SiC powders of approx. 1000 A uniform diameter, nonagglomerated and spherical were produced. This required major revision of the particle formation and growth model from one based on classical nucleation and growth to one based on collision and coalescence of Si particles followed by their carburization. Dispersions based on pure organic solvents as well as steric stabilization were investigated. Although stable dispersions were formed by both, subsequent part fabrication emphasized the pure solvents since fewer problems with drying and residuals of the high purity particles were anticipated. Test parts were made by the colloidal pressing technique; both liquid filtration and consolidation (rearrangement) stages were modeled. Green densities corresponding to a random close packed structure (approx. 63%) were achieved; this highly perfect structure has a high, uniform coordination number (greater than 11) approaching the quality of an ordered structure without introducing domain boundary effects. After drying, parts were densified at temperatures ranging from 1800 to 2100 C. Optimum densification temperatures will probably be in the 1900 to 2000 C range based on these preliminary results which showed that 2050 C samples had experienced substantial grain growth. Although overfired, the 2050 C samples exhibited excellent mechanical properties. Biaxial tensile strengths up to 714 MPa and Vickers hardness values of 2430 kg/sq mm 2 were both more typical of hot pressed than sintered SiC. Both result from the absence of large defects and the confinement of residual porosity (less than 2.5%) to small diameter, uniformly distributed pores.

Haggerty, J. S.↗

NASA NTRS1987

Thermal expansion and thermal expansion anisotropy of SiC polytypes

The principal axial coefficients of thermal expansion for the (3C), (4H), and (6H) polytypes of SiC are considered to identify the structural role of the stacking layer sequence as it affects the thermal expansion. A general equation based on the fractions of cubic and hexagonal layer stacking is developed that expresses the principal axial thermal expansion coefficients of all of the SiC polytypes. It is then applied to address the thermal expansion anisotropy of the noncubic SiC structures.

Li, Z.↗