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Integrated High Payoff Rocket Propulsion Technology (IHPRPT) SiC Recession Model

SiC stability and recession rates were modeled in hydrogen/oxygen combustion environments for the Integrated High Payoff Rocket Propulsion Technology (IHPRPT) program. The IHPRPT program is a government and industry program to improve U.S. rocket propulsion systems. Within this program SiC-based ceramic matrix composites are being considered for transpiration cooled injector faceplates or rocket engine thrust chamber liners. Material testing under conditions representative of these environments was conducted at the NASA Glenn Research Center, Cell 22. For the study described herein, SiC degradation was modeled under these Cell 22 test conditions for comparison to actual test results: molar mixture ratio, MR (O2:H2) = 6, material temperatures to 1700 C, combustion gas pressures between 0.34 and 2.10 atm, and gas velocities between 8,000 and 12,000 fps. Recession was calculated assuming rates were controlled by volatility of thermally grown silica limited by gas boundary layer transport. Assumptions for use of this model were explored, including the presence of silica on the SiC surface, laminar gas boundary layer limited volatility, and accuracy of thermochemical data for volatile Si-O-H species. Recession rates were calculated as a function of temperature. It was found that at 1700 C, the highest temperature considered, the calculated recession rates were negligible, about 200 m/h, relative to the expected lifetime of the material. Results compared favorably to testing observations. Other mechanisms contributing to SiC recession are briefly described including consumption of underlying carbon and pitting. A simple expression for liquid flow on the material surface was developed from a one-dimensional treatment of the Navier-Stokes Equation. This relationship is useful to determine under which conditions glassy coatings or thermally grown silica would flow on the material surface, removing protective layers by shear forces. The velocity of liquid flow was found to depend on the gas velocity, the viscosity of gas and liquid, as well as the thickness of the gas boundary layer and the liquid layer. Calculated flow rates of a borosilicate glass coating compared well to flow rates observed for this coating tested on a SiC panel in Cell 22.

Opila, E. J.

Oxidation of TaSi2-Containing ZrB2-SiC Ultra-High Temperature Materials

Hot pressed coupons of composition ZrB2-20 v% SiC-5 v% TaSi2 and ZrB2-20 v% SiC-20 v% TaSi2 were oxidized in stagnant air at temperatures of 1627 and 1927C for one, five and ten 10-minute cycles. The oxidation reactions were characterized by weight change kinetics, x-ray diffraction, and SEM/EDS. Detailed WDS/microprobe quantitative analyses of the oxidation products were conducted for the ZrB2-20 v% SiC-20 v% TaSi2 sample oxidized for five 10-minute cycles at 1927C. Oxidation kinetics and product formation were compared to ZrB2-20 v% SiC with no TaSi2 additions. It was found that the 20 v% TaSi2 composition exhibited improved oxidation resistance relative to the material with no TaSi2 additions at 1627C. However, for exposures at 1927C less oxidation resistance and extensive liquid phase formation were observed compared to the material with no TaSi2 additions. Attempts to limit the liquid phase formation by reducing the TaSi2 content to 5 v% were unsuccessful. In addition, the enhanced oxidation resistance at 1627C due to 20 v% TaSi2 additions was not achieved at the 5 v% addition level. The observed oxidation product evolution is discussed in terms of thermodynamics and phase equilibria for the TaSi2-containing ZrB2-SiC material system. TaSi2-additions to ZrB2-SiC at any level are not recommended for ultra-high temperature (>1900C) applications due to excessive liquid phase formation.

Opila, Elizabeth J.

Packaging Technologies for 500C SiC Electronics and Sensors

Various SiC electronics and sensors are currently under development for applications in 500C high temperature environments such as hot sections of aerospace engines and the surface of Venus. In order to conduct long-term test and eventually commercialize these SiC devices, compatible packaging technologies for the SiC electronics and sensors are required. This presentation reviews packaging technologies developed for 500C SiC electronics and sensors to address both component and subsystem level packaging needs for high temperature environments. The packaging system for high temperature SiC electronics includes ceramic chip-level packages, ceramic printed circuit boards (PCBs), and edge-connectors. High temperature durable die-attach and precious metal wire-bonding are used in the chip-level packaging process. A high temperature sensor package is specifically designed to address high temperature micro-fabricated capacitive pressure sensors for high differential pressure environments. This presentation describes development of these electronics and sensor packaging technologies, including some testing results of SiC electronics and capacitive pressure sensors using these packaging technologies.

Chen, Liang-Yu

Long-Term Reliability of a Hard-Switched Boost Power Processing Unit Utilizing SiC Power MOSFETs

Silicon carbide (SiC) power devices have demonstrated many performance advantages over their silicon (Si) counterparts. As the inherent material limitations of Si devices are being swiftly realized, wide-band-gap (WBG) materials such as SiC have become increasingly attractive for high power applications. In particular, SiC power metal oxide semiconductor field effect transistors' (MOSFETs) high breakdown field tolerance, superior thermal conductivity and low-resistivity drift regions make these devices an excellent candidate for power dense, low loss, high frequency switching applications in extreme environment conditions. In this paper, a novel power processing unit (PPU) architecture is proposed utilizing commercially available 4H-SiC power MOSFETs from CREE Inc. A multiphase straight boost converter topology is implemented to supply up to 10 kilowatts full-scale. High Temperature Gate Bias (HTGB) and High Temperature Reverse Bias (HTRB) characterization is performed to evaluate the long-term reliability of both the gate oxide and the body diode of the SiC components. Finally, susceptibility of the CREE SiC MOSFETs to damaging effects from heavy-ion radiation representative of the on-orbit galactic cosmic ray environment are explored. The results provide the baseline performance metrics of operation as well as demonstrate the feasibility of a hard-switched PPU in harsh environments.

Ikpe, Stanley A.

Experimental Durability Testing of 4H SiC JFET Integrated Circuit Technology at 727 C

We have reported SiC integrated circuits (IC's) with two levels of metal interconnect that have demonstrated prolonged operation for thousands of hours at their intended peak ambient operational temperature of 500 C [1, 2]. However, it is recognized that testing of semiconductor microelectronics at temperatures above their designed operating envelope is vital to qualification. Towards this end, we previously reported operation of a 4H-SiC JFET IC ring oscillator on an initial fast thermal ramp test through 727 C [3]. However, this thermal ramp was not ended until a peak temperature of 880 C (well beyond failure) was attained. Further experiments are necessary to better understand failure mechanisms and upper temperature limit of this extreme-temperature capable 4H-SiC IC technology. Here we report on additional experimental testing of custom-packaged 4H-SiC JFET IC devices at temperatures above 500 C. In one test, the temperature was ramped and then held at 727 C, and the devices were periodically measured until electrical failure was observed. A 4H-SiC JFET on this chip electrically functioned with little change for around 25 hours at 727 C before rapid increases in device resistance caused failure. In a second test, devices from our next generation 4H-SiC JFET ICs were ramped up and then held at 700 C (which is below the maximum deposition temperature of the dielectrics). Three ring oscillators functioned for 8 hours at this temperature before degradation. In a third experiment, an alternative die attach of gold paste and package lid was used, and logic circuit operation was demonstrated for 143.5 hours at 700 C.

JFET

Experimental Durability Testing of 4H SiC JFET Integrated Circuit Technology at 727 Degrees Centigrade

We have reported SiC integrated circuits (ICs) with two levels of metal interconnect that have demonstrated prolonged operation for thousands of hours at their intended peak ambient operational temperature of 500 degrees Centigrade. However, it is recognized that testing of semiconductor microelectronics at temperatures above their designed operating envelope is vital to qualification. Towards this end, we previously reported operation of a 4H-SiC JFET IC ring oscillator on an initial fast thermal ramp test through 727 degrees Centigrade. However, this thermal ramp was not ended until a peak temperature of 880 degrees Centigrade (well beyond failure) was attained. Further experiments are necessary to better understand failure mechanisms and upper temperature limit of this extreme-temperature capable 4H-SiC IC technology.Here we report on additional experimental testing of custom-packaged 4H-SiC JFET IC devices at temperatures above 500 degrees Centigrade. In one test, the temperature was ramped and then held at 727 degrees Centigrade, and the devices were periodically measured until electrical failure was observed. A 4H-SiC JFET on this chip electrically functioned with little change for around 25 hours at 727 degrees Centigrade before rapid increases in device resistance caused failure. In a second test, devices from our next generation 4H-SiC JFET ICs were ramped up and then held at 700 degrees Centigrade (which is below the maximum deposition temperature of the dielectrics). Three ring oscillators functioned for 8 hours at this temperature before degradation. In a third experiment, an alternative die attach of gold paste and package lid was used, and logic circuit operation was demonstrated for 143.5 hours at 700 degrees Centigrade.

Silicon Carbide

Practical SiC JFET-R Analog Integrated Circuit Design for Extreme Environment Applications

Silicon carbide (SiC) junction field effect transistor and SiC resistor (SiC JFET-R) integrated circuits(ICs) have uniquely demonstrated prolonged operation above 450 °C that promises significant operational improvements to a variety of NASA missions. However, the SiC epiwafers used to fabricate these ICs suffer from epi-growth process immaturity that imparts large and systematic spreads in JFET threshold voltages as a function of the device distance from the center on the wafer. Furthermore, the unprecedently wide range of intended application operating temperatures (in many cases over 600 °C wide) imparts as much as 5-fold change in JFET bias currents. This Technical Memorandum documents methods by which both temperature and radius associated JFET electrical parameter variances can be adequately eliminated, or even exploited in JFET-R circuit designs. Full analog circuit examples, including operational amplifiers, and SPICE simulations across experimentally documented SiC JFET parameter extremes are given to illustrate the efficacy of these methods. The reader may use the examples in this memorandum as either an end point, to get a desired analog signal conditioning design into hardware implemented in SiC JFET-R ICs, or as a basis point from which to derive further improvement.

Michael J Krasowski

Micro-tensile Properties of Fueled Irradiated AGR-2 TRISO-coated Particle Buffer, IPyC, and SiC Interlayer Regions

Tristructural isotropic (TRISO) coated nuclear fuel particles are proving to be a versatile fuel form for new reactor designs. Understanding the bounding strength and failure mode of each coating interface is important to both fuel quality evaluation and failure prediction. A mechanism of key significance is failure of the silicon carbide (SiC) layer to retain fission products due to incomplete tearing of the buffer layer. This is a two-step mechanism involving both mechanical failure in the buffer and inner pyrolytic carbon (IPyC) layers and degradation of the SiC layer through palladium silicides at the IPyC-SiC interface. However, the mechanical properties of TRISO particle coating layers have yet to be fully characterized due to the small dimension of TRISO fuel particles and high radioactivity. To investigate this mechanism, in situ micro-tensile properties of the buffer, IPyC, SiC, buffer-IPyC, and IPyC-SiC interlayer regions of fueled TRISO particles have been tested at both as-fabricated and irradiated conditions. Determination of the mechanical properties of these TRISO particle regions will lead to a better understanding of the SiC layer failure mechanism and enable progress towards TRISO fuel qualification.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS

Formation of carbon homonuclear bonds in β-SiC under neutron irradiation at various temperatures and neutron doses

To elucidate radiation defect processes in SiC, Raman spectroscopy was systematically applied to high-purity, polycrystalline β-SiC that was neutron irradiated at a range of temperature and dose conditions. The analysis specifically focused on formation of carbon homonuclear bonds by irradiation; these bonds were indicated by D and G bands and amorphous carbon peaks. Intensity of the carbon peaks relative to SiC peaks significantly decreased in the case of high temperature and/or high neutron dose of 500 °C to 29 displacements per atom (dpa) and about 800 °C to 1.38 and 29 dpa. The absence of carbon bond peaks under those conditions was explained by growth of stoichiometric defect clusters, consistent with previous atomistic simulations on SiC defect stability. The lack of Raman bands associated with carbon clusters under high-temperature and high-dose radiation conditions accounts for the resistance of SiC to phase separation under irradiation. The findings further suggest that material compositions and chemical properties that are inherently resistant to chemical disordering under high-dose radiation conditions are indicative of the long-term durability of ceramic compounds in radiation environments.

36 MATERIALS SCIENCE

Time Resolution Characterization of 4H-SiC LGADs with a 90 Sr Source

This work presents timing measurements of 4H-SiC Low Gain Avalanche Detectors (4H-SiC LGADs) using beta particles from a 90Sr source. The 4H-SiC LGADs exhibit fast signal responses, and a time resolution of 61 ps was achieved, comparable to that of standard Si LGADs. The present limitation in the time resolution of 4H-SiC LGADs appears to stem from limited charge generation. Nevertheless, their higher voltage tolerance and faster carrier drift suggest that, with increased charge collection, their timing performance could approach or even surpass that of Si LGADs. Furthermore, these results demonstrate the strong potential of 4H-SiC LGADs as a robust platform for precision timing in future 4D tracking detectors, while also highlighting that signal charge is the dominant factor currently limiting their performance, indicating that further optimization of gain and drift structures will be essential for future development.

43 PARTICLE ACCELERATORS

DC Modeling of 4H-SiC JFET Gate Length Reduction at 500°C

The development of robust, high-performance integrated circuits (ICs) will enable numerous potential NASA missions of current interest, including long-duration robotic missions exploring the 460 °C surface of Venus. Currently, NASA is looking towards SiC-based devices to provide such a solution. However, the current NASA silicon carbide (SiC) JFET device with a channel length of 6μm (for recently fabricated Gen. 11 ICs) limits on mission relevant circuit capabilities [1]. In this study, we combined experiments with simulations to explore two straightforward fabrication strategies to reduce the SiC JFET channel length while maintaining turn-off behavior (Fig. 1a) needed to realize 500 °C circuit operation. The first fabrication strategy uses a shallow self-align nitrogen implant (Figure 1b) along the device's top surface but not below the gate combined with a high-dose phosphorous implant directly below the source and drain contacts. For the second fabrication strategy (Figure 1c), the high-dose phosphorous implants extended from below the contacts all the way up to the gate edges. Simulations guided gate length reductions without significant degradation in the turn-off performance. In total 12 SiC JFET variants implementing using the different fabrication strategies, gate lengths, and n-channel epilayer thickness were implemented in our simulation framework implemented in COMSOL. Since the COMSOL database does not have the material properties for 4H-SiC, these parameters were taken from the literature and implemented in COMSOL. The empirical models [2] for incomplete ionization, Auger recombination, low field mobility, and Shockley-Read-Hall recombination were implemented to account for material-specific device behavior.

4H-SiC JFET

Bulk-scale stress–strain hysteresis in layered crystalline solids: A study of graphite and Ti 3 SiC 2

Polycrystalline graphite and the MAX phase Ti 3 SiC 2 are layered crystalline solids with similar deformation mechanisms, including basal slip, ripplocation boundaries (RBs), kink boundaries (KBs), and cracking. The interplay of these mechanisms, notably in energy dissipation, has been much discussed in the past twenty-five years. This study builds upon previous work, investigating deformation with a renewed emphasis on the bulk-scale and given recent findings concerning RBs. Our investigation compares the evolution of energy dissipation, nonlinear recoverable and irrecoverable strain, and damage upon increasing stress for graphite and Ti 3 SiC 2 . Benitez et al.’s (2016) methodology of compressive cyclic loading and post-mortem electron backscatter diffraction (EBSD) to assess the prevalence of kinking based on low-angle grain boundaries (LAGBs) was used. Strains were measured with digital image correlation and EBSD was conducted on Ti 3 SiC 2 leveraging dictionary indexing, which was necessary herein to identify LAGBs accurately. The stress–strain stages of Ti 3 SiC 2 agree with literature on Ti 2 AlC. Damage and energy dissipation were more accelerated in graphite. No significant difference was observed in the fraction of LAGBs between pristine and unloaded Ti 3 SiC 2 . Trends observed and EBSD evidence that KBs were not dominant suggest that RBs are the primary dissipator of energy in both materials.

36 MATERIALS SCIENCE

Micromechanical response of SiC-OPyC layers in TRISO fuel particles

Tristructural isotropic (TRISO)–coated particle fuel is a proposed fuel for multiple advanced reactor concepts. The performance of the particle depends on whether the silicon carbide (SiC) layer remains intact to prevent the release of metallic and gaseous fission products. Mechanical fracture of the SiC layer is a potential failure mode under various fuel configurations and operating environments, including the potential transmission of matrix-originating cracks through TRISO particles. Furthermore, this study uses instrumented indentation techniques on cross-sectioned surrogate particles to examine the mechanical stability of the critical interface between SiC and the outer pyrolytic carbon (OPyC) layer. The observed behavior at the interface is rationalized by examining the radially dependent fracture behavior of the SiC layer and performing a numerical analysis to quantify the residual stresses that develop during the processing and cross-sectioning of the as-fabricated particle. Characterizing the SiC-OPyC interface of surrogate TRISO particles using nanoindentation provides unique insight into the interface's room-temperature residual stress and mechanical stability. The modeling efforts were used to investigate the experimental procedure further, and the results are presented herein to validate this fuel form's potential mechanical failure modes.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS

Methods development towards automated, physics-informed, quantitative quality control of TRISO-SiC

Tristructural-isotropic (TRISO) fuel particles have been developed as a high-performance fuel for use in high-temperature gas-cooled reactor (HTGR) systems due to their high efficiency and stability under both normal and off-normal conditions. Broader deployment of this technology in advanced nuclear applications may benefit from quantitative quality assurance and quality control (QA/QC) methods that directly link TRISO properties to downstream performance. A key TRISO property is the SiC layer microstructure, which influences fission product retention during irradiation. However, existing QA/QC for the TRISO-SiC microstructure comprises only a qualitative visual inspection; therefore, there is a clear opportunity for the development of quantitative methods for TRISO QA/QC. Here, to this end, previous work has demonstrated an image processing approach to grain boundary (GB) identification and subsequent extraction of microstructural metrics; however, extensive twinning within the SiC layer complicates such analyses because twin GBs significantly influence microstructural metrics but are not expected to contribute to fission product transport. This study presents the initial development, training, and testing of an ML-based image segmentation algorithm designed to identify and remove twin GBs from standard backscattered electron micrographs, providing an industrially applicable, quantitative, and physically meaningful QA/QC approach for the TRISO-SiC microstructure. Although pixel-wise performance metrics for the twin predictions are low, the change in grain area and the number of GB pixels after twin removal predicted by the ML workflow are within 1% of the true values calculated using crystallographic data. This suggests that the model is well capable of predicting overall twin boundary structures and grain morphology, and continued advancement of this approach could enable automated, scalable, and physics-informed QA/QC for TRISO-SiC microstructures, supporting the reliable qualification of coated particle fuels for next-generation reactor systems.

Computer vision

Screening and qualification methodology for SiC end plug processing methods

Deployment of SiC-ceramic-based fuel cladding for light water reactors requires a hermetic end plug–to–cladding joint that can withstand neutron irradiation during normal operation and maintain integrity during design-basis accidents. Reactor experiments have shown that some SiC composite tubes with SiC end plugs can retain hermeticity after irradiation. However, achieving consistent joint performance under irradiation remains a key challenge. Resolving this issue is essential to enable integral irradiation testing and to demonstrate fuel integrity under commercial-reactor irradiation conditions. This report aims to: (1) provide guidance for designing radiation-tolerant end plug joints for SiC cladding; (2) demonstrate experimental methods to detect processing defects that are unstable under neutron irradiation at light-water-reactor-relevant temperatures and doses; and (3) outline a step-by-step approach for designing and conducting reactor experiments to screen joining methods. The resulting data will be used to improve joint processing and to define critical defect types and sizes that must be detected and eliminated through non-destructive evaluation for quality assurance. Based on prior irradiation experiments at the High Flux Isotope Reactor, differential swelling among the cladding, bonding layer, and end plug was identified as an underlying mechanism for irradiation-induced joint degradation. Accordingly, this effect must be considered in the design of radiation-tolerant joining techniques. In this work, miniature SiC end plug joint specimens irradiated during the previous project were analyzed using X-ray computed tomography to characterize the joint microstructure. Digital volume correlation of the tomography data quantified radiation-induced microstructural changes and enabled evaluation of defect-related risks. Finally, ongoing neutron irradiation efforts using larger specimen volumes are presented. These efforts aim to statistically assess joint performance and to build a microstructure–performance (e.g., leak-tightness) dataset to inform processing improvements and quality control.

22 GENERAL STUDIES OF NUCLEAR REACTORS

High-Temperature SiC Cladding End Plug Irradiation Design and HFIR Readiness

This report documents the design of a High Flux Isotope Reactor (HFIR) irradiation experiment intended to evaluate irradiation effects on the hermeticity of silicon carbide (SiC) end plug specimens under a radial fast neutron flux gradient at representative light-water reactor (LWR) temperatures of approximately 300 °C. The overarching goal of this work is to statistically evaluate SiC end plug hermeticity and mechanical properties following irradiation using the high-throughput irradiation capability discussed here. Each specimen consists of a short section of SiC fiber–reinforced SiC (SiC/SiC) tube with a single monolithic SiC end plug joined to one end. The experiment allows up to 66 specimens to be irradiated in six different stacks within a dry, sealed irradiation capsule derived from the previously developed high-temperature SiC/SiC cladding bowing experiment. The neutronics basis, thermal analysis, and HFIR readiness of the experiment are discussed in this report for two possible design cases. The first design case is based on existing approval documentation and components that are on hand and approved for use, so the experiment insertion would require only specimen receipt, specimen pre-irradiation characterization, experiment assembly, and final fabrication package approval. The second design case provides improved thermal robustness and the preferred end plug geometry but requires fabrication of a modified holder and revisions to the HFIR approval documentation, in addition to the other activities required for the first design case, before insertion.

Hott, Daniel [Oak Ridge National Laboratory (ORNL)

Bubble formation in oxide scales on SiC

The oxidation of alpha-SiC single crystals and sintered alphaand beta-SiC polycrystals has been investigated at elevated temperatures. Bubble formation is commonly observed in oxide scales on polycrystalline SiC, but is rarely found on single-crystal scales; bubbles result from the preferential oxidation of C inclusions, which are abundant in SiC polycrystals. The absence of bubbles on single crystals, in fact, implies that diffusion of the gaseous species formed on oxidation, CO (or possibly SiO), controls the rate of oxidation of SiC.

Mieskowski, D. M.

Raman scattering studies of chemical-vapor-deposited cubic SiC films of (100)Si

Raman scattering studies for a series of CVD-grown cubic SiC single-crystal films with film thickness from 600 A to 17 microns are discussed. The results suggest that the crystalline orientations of the Si substrate and the 3C-SiC film are the same. It is found that the Si 522/cm phonon from a Si wafer is enhanced in intensity by a factor of 2-3 due to a CVD overlayer of cubic SiC, and that the 3C-SiC longitudinal optical phonon at the Gamma point from SiC/Si samples is enhanced by a factor of two or three following the removal of the Si substrate. The variation of the Raman spectrum with incident power is investigated, and a method for determining the Raman cross section for 3 C-SiC is proposed.

Feng, Z. C.