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DOE OSTI2020

Impact damage of narrow silicon carbide (SiC) ceramics with and without environmental barrier coatings (EBCs) by various foreign object debris (FOD) simulants

The leading and trailing edges of turbine airfoils are highly susceptible to impact by foreign object debris (FOD) entrained in the gas stream of turbine engines. In this study, a narrow specimen geometry is implemented to study the FOD impact behavior of low curvature airfoil edges. Silicon carbide (SiC) ceramic specimens with and without an environmental barrier coating (EBC) are used as target materials. The EBC consists of an air plasma sprayed mullite topcoat (~ 166 µm) and silicon bond coat (~ 58 µm). Spherical (∅ 1.5 mm) FOD simulants of silicon nitride (Si3N4), partially stabilized zirconia (PSZ), and steel are used as impactors. Additionally, a modified gas gun is used to generate impact damage at normal incidence and velocities ranging between 300 to 400 m/s. In situ phase contrast X-ray radiographs, which render 2D representations of the internal transient damage, are captured during the impact experiments. Impactor hardness and toughness are found to primarily influence damage in the coating. Relative to wide specimens, the narrow specimens experience a greater level of cracking and this is postulated to result from reduced self-confinement. Irrespective of specimen geometry and impactor material type, limited cracking (i.e. enhanced shielding) is observed for the coated condition.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Large-Scale Additive Manufacturing of Silicon Carbide with Process Monitoring

This report summarizes new capabilities in additive manufacturing (AM) of large-scale silicon carbide (SiC) components under the Advanced Materials and Manufacturing Technologies (AMMT) program. SiC is a promising material that is being considered for many advanced reactor designs due to its high temperature strength, radiation tolerance, minimal neutron absorption, and oxidation resistance [1-8]. One of the primary limitations to using SiC as an in-core structural material is the inability to fabricate large SiC components with complex geometries. While under the former Transformational Challenge Reactor (TCR) program, ceramic AM systems at the Oak Ridge National Laboratory (ORNL) were limited in the quantity and overall size achievable for producing ceramic AM components. To address this, ORNL has improved its infrastructure for binder jet and chemical vapor infiltration (CVI) processes with cutting-edge equipment coming online in a newly renovated laboratory space capable of producing larger components and higher throughput without compromise on part size. This report details the laboratory renovation progress, focusing specifically on the DesktopMetal (formerly ExOne) X25Pro binder jet, a large scale CVI furnace, and the added functionality of a software tool called Peregrine for quality assurance and control purposes.

36 MATERIALS SCIENCE↗

NASA NTRS1991

Silicon carbide, a semiconductor for space power electronics

After many years of promise as a high temperature semiconductor, silicon carbide (SiC) is finally emerging as a useful electronic material. Recent significant progress that has led to this emergence has been in the areas of crystal growth and device fabrication technology. High quality single-crystal SiC wafers, up to 25 mm in diameter, can now be produced routinely from boules grown by a high temperature (2700 K) sublimation process. Device fabrication processes, including chemical vapor deposition (CVD), in situ doping during CVD, reactive ion etching, oxidation, metallization, etc. have been used to fabricate p-n junction diodes and MOSFETs. The diode was operated to 870 K and the MOSFET to 770 K.

Powell, J. Anthony↗

NASA NTRS1991

Silicon carbide, a semiconductor for space power electronics

After many years of promise as a high temperature semiconductor, silicon carbide (SiC) is finally emerging as a useful electronic material. Recent significant progress that has led to this emergence has been in the area of crystal growth and device fabrication technology. High quality of single-crystal SiC wafers, up to 25 mm in diameter, can now be produced routinely from boules grown by a high temperature (2700 K) sublimation process. Device fabrication processes, including chemical vapor deposition (CVD), in situ doping during CVD, reactive ion etching, oxidation, metallization, etc. have been used to fabricate p-n junction diodes and MOSFETs. The diode was operated to 870 K and the MOSFET to 770 K.

Powell, J. A.↗

NASA NTRS2007

Silicon carbide and other films and method of deposition

A method of depositing a ceramic film, particularly a silicon carbide film, on a substrate is disclosed in which the residual stress, residual stress gradient, and resistivity are controlled. Also disclosed are substrates having a deposited film with these controlled properties and devices, particularly MEMS and NEMS devices, having substrates with films having these properties.

Mehregany, Mehran↗

NASA NTRS2011

Silicon carbide and other films and method of deposition

Mehregany, Mehran↗

NASA NTRS2012

Temperature Induced Voltage Offset Drifts in Silicon Carbide Pressure Sensors

We report the reduction of transient drifts in the zero pressure offset voltage in silicon carbide (SiC) pressure sensors when operating at 600 C. The previously observed maximum drift of +/- 10 mV of the reference offset voltage at 600 C was reduced to within +/- 5 mV. The offset voltage drifts and bridge resistance changes over time at test temperature are explained in terms of the microstructure and phase changes occurring within the contact metallization, as analyzed by Auger electron spectroscopy and field emission scanning electron microscopy. The results have helped to identify the upper temperature reliable operational limit of this particular metallization scheme to be 605 C.

Okojie, Robert S.↗

DOE OSTI2020

Fission Product Diffusion in Silicon Carbide: As Revealed by Computer Simulations and Experimental Measurements

The diffusion and release of fission products through silicon carbide in the tri-structural isotropic (TRISO) fuel particles remain unsolved for decades. The underlying mechanism is quite challenging to be determined. To help unveil the mysterious story, the current work applies molecular dynamics method to show the stability of silver, palladium, ruthenium and iodine as an interstitial and their atomic diffusion along coincident site lattice (CSL) boundary, especially ?3 grain boundary (GB). The major finding presents a much faster diffusion along GB than in bulk for all elements considered. The reasonably close estimate to experiments and simulations where available has confirmed the important role of grain boundary diffusion of Ag and Pd in SiC. However, the discrepancy addressed in Ag with measurements from fuel studies suggest a more complicated mechanism, which might be in correlation with high energy grain boundaries or the presence of crack. The subsequent characterization of Ru and I distribution in SiC-PyC-SiC diffusion couples, which have been ion irradiated at 900?C to 10 dpa and 20 dpa, has performed by secondary ion mass spectrometry (SIMS) analysis. The experiment measurements correlate well with the grain boundary diffusion by simulation, which provide further evidences that the grain boundary diffusion cannot be neglected once the fission products are accessible at the grain boundary.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS2015

Concept Demonstration of Dopant Selective Reactive Etching (DSRIE) in Silicon Carbide

Accurate quantification of combustor pressure dynamics for the primary purpose of experimental validation of computational fluid dynamics (CFD) codes requires the use of robust, reliable and sensitive pressure sensors that can resolve sub--pound-per-square-inch pressure levels in high temperature environments (i.e., combustor). The state of the art microfabricated piezoresistive silicon carbide (SiC) pressure sensors that we have developed are capable of operating reliably at 600 degrees Centigrade. This technology was used in support of the ARMD ISRP-ERA (NASA's Aeronautics Research Mission Directorate, Integrated System Research Project - Environmentally Responsible Aviation) program to quantify combustor thermoacoustic instabilities. The results showed that while the SiC pressure sensors survived the high temperature and measured instabilities, the diaphragm (force collector) was not thin enough to be sensitive in resolving sub-pound-per-square-inch pressures; 30 meters is the thinnest diaphragm achievable with conventional reactive ion etching (RIE) processes. Therefore, this precludes its use for sub-pound-per-square-inch pressure measurement with high fidelity. In order to effectively resolve sub-pound-per-square-inch pressures, a thinner more sensitive diaphragm (10 meters) is needed. To achieve this would require a new and innovative fabrication process technique.

static↗

DOE OSTI2026

Depth-Resolved X-Ray Nanoimaging of Coherent and Incoherent Energy Transport in Silicon Carbide

Understanding lattice dynamics is crucial for optimizing the process of creating functional structures, such as laser writing of color-center defects. However, existing structural probes have difficulty measuring structural dynamics with submicrometer depth sensitivity. Here, in this study, a depth-resolved ultrafast X-ray nanodiffraction technique is developed to track the lattice dynamics of silicon carbide (SiC) in three dimensions. Upon laser excitation of an aluminum layer that acts as a heat and strain transducer, a specular Bragg peak of SiC shows an overall increase in the X-ray diffraction intensity rather than a peak shift. The relaxation dynamics of the increased intensity are significantly different when probed on and off the Bragg peak. The fast subnanosecond relaxation probed at the maximum of the Bragg peak is a result of the propagation of a coherent strain wave along the depth direction, while a slow relaxation probed at the wings of the Bragg peak reflects a localized incoherent lattice heating. To further visualize these processes, spatiotemporal maps were obtained by scanning the relative position and delay between the laser pump and X-ray probe beams, which capture the propagation of the strain wave, as well as a stationary structural distortion close to the aluminum/SiC interface. These depth-resolved structural measurements disentangle energy dissipation mechanisms in laser-excited SiC, and they open opportunities for finer control of, for example, the formation of optically addressable defect complexes central to quantum information applications.

X-ray nanodiffraction↗

DOE OSTI2025

Additive manufacturing of high‐density silicon carbide ceramics through post‐processing spark plasma sintering

This research advances the field of additive manufacturing (AM) of silicon carbide (SiC) ceramics by integrating spark plasma sintering (SPS) to enhance material density, mechanical strength, and thermal properties. Traditional AM techniques struggle to achieve the high‐density SiC required for demanding applications, such as aerospace engineering, where high thermal conductivity and mechanical strength are paramount. Here, our study addresses these challenges by incorporating SPS as a post‐processing step, achieving near‐theoretical maximum densities and significantly reducing porosity, thereby resulting in outstanding thermal conductivity in SiC ceramics. We developed a specialized SiC ink optimized for 3D printing, ensuring structural integrity after deposition through tailored rheological properties. The application of SPS facilitates rapid, uniform sintering, essential for attaining superior density, mechanical properties, and thermal performance. Our experimental results, confirmed through scanning electron microscopy analysis, demonstrate significant microstructural properties, mechanical strength, and thermal conductivity, showcasing the effectiveness of integrating SPS in AM processes. This innovative approach not only expands the capabilities of AM in producing complex, high‐density ceramic structures but also broadens the potential applications of SiC in demanding environments.

36 MATERIALS SCIENCE↗

DOE OSTI2020

High-Q suspended optical resonators in 3C silicon carbide obtained by thermal annealing

We fabricate suspended single-mode optical waveguides and ring resonators in 3C silicon carbide (SiC) that operate at telecommunication wavelength, and leverage post-fabrication thermal annealing to minimize optical propagation losses. Annealed optical resonators yield quality factors of over 41,000, which corresponds to a propagation loss of 7 dB/cm, and is a significant improvement over the 24 dB/cm in the case of the non-annealed chip. This improvement is attributed to the enhancement of SiC crystallinity and a significant reduction of waveguide surface roughness, from 2.4 nm to below 1.7 nm. The latter is attributed to surface layer oxide growth during the annealing step. We confirm that the thermo-optic coefficient, an important parameter governing high-power and temperature-dependent performance of SiC, does not vary with annealing and is comparable to that of bulk SiC. Our annealing-based approach, which is especially suitable for suspended structures, offers a straightforward way to realize high-performance 3C-SiC integrated circuits.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

NASA NTRS1985

Environmental effects on the tensile strength of chemically vapor deposited silicon carbide fibers

The room temperature and elevated temperature tensile strengths of commercially available chemically vapor-deposited (CVD) silicon carbide fibers were measured after 15 min heat treatment to 1600 C in various environments. These environments included oxygen, air, argon and nitrogen at one atmosphere and vacuum at 10/9 atmosphere. Two types of fibers were examined which differed in the SiC content of their carbon-rich coatings. Threshold temperature for fiber strength degradation was observed to be dependent on the as-received fiber-flaw structure, on the environment and on the coating. Fractographic analyses and flexural strength measurements indicate that tensile strength losses were caused by surface degradation. Oxidation of the surface coating is suggested as one possible degradation mechanism. The SiC fibers containing the higher percentage of SiC near the surface of the carbon-rich coating show better strength retention and higher elevated temperature strength.

Bhatt, R. T.↗

NASA NTRS1985

Sintered alpha silicon carbide ceramics for high temperature structural application - Status review and recent developments

The physical properties of sintered alpha silicon carbide are reviewed, including the effect of oxidation at high temperatures. Net shape fabricated components are described which have undergone extensive testing in heat engine applications. Properties of an SiC/TiB2 composite material, which has significantly improved fracture toughness, are presented.

Storm, R. S.↗

NASA NTRS1999

Chemical Mechanical Polishing of Silicon Carbide

The High Temperature Integrated Electronics and Sensors (HTIES) team at the NASA Lewis Research Center is developing silicon carbide (SiC) as an enabling electronic technology for many aerospace applications. The Lewis team is focusing on the chemical vapor deposition of the thin, single-crystal SiC films from which devices are fabricated. These films, which are deposited (i.e., epitaxially "grown") on commercial wafers, must consist of a single crystal with very few structural defects so that the derived devices perform satisfactorily and reliably. Working in collaboration (NASA grant) with Professor Pirouz of Case Western Reserve University, we developed a chemical-mechanical polishing (CMP) technique for removing the subsurface polishing damage prior to epitaxial growth of the single-crystal SiC films.

Powell, J. Anthony↗

DOE OSTI2025

Thermal Optimization and Experimental Demonstration of a Silicon Carbide, Half-Bridge Power Module

This paper describes modeling and experimental work to design and demonstrate a silicon carbide (SiC), single-side-cooled power module. Two SiC metal-oxide-semiconductor field-effect transistors (MOSFET) were used for each switch position and packaged on a metalized ceramic substrate. Thermal modeling was first conducted to optimize the module packaging to minimize junction-to-fluid thermal resistance and device temperature variations. This procedure identified the optimal device placement and baseplate thickness to maximize thermal performance. A heat exchanger - incorporating impinging jets of water-ethylene glycol - was designed to cool the module's baseplate to minimize thermal resistance and pumping power. The heat exchanger used relatively low fluid velocities (<1.5 m/s) to minimize erosion-corrosion effects and relatively large fluid channel sizes (>=1 mm) to prevent clogging. The power module concept was fabricated, and experiments were conducted to measure its thermal performance. Direct current was used to power the module devices, and junction temperatures were measured via device temperature-sensitive parameters. The experimental results were found to be in good agreement with model predictions (within 2%) and yielded junction-to-fluid thermal resistance values as low as about 15 mm2 K/W at relatively low pumping power values. The results demonstrate the improved performance associated with jet impingement cooling and represent an improvement over existing channel-flow-type cold plates, which can enable improvements to power density and reliability.

36 MATERIALS SCIENCE↗

NASA NTRS2000

Article and method for making complex shaped preform and silicon carbide composite by melt infiltration

Small diameter silicon carbide-containing fibers are provided in a bundle such as a fiber tow that can be formed into a structure where the radii of curvature is not limited to 10-20 inches. An aspect of this invention is directed to impregnating the bundles of fibers with the slurry composition to substantially coat the outside surface of an individual fiber within the bundle and to form a complex shaped preform with a mass of continuous fibers.

Steibel, James D.↗

NASA NTRS2001

Article and method for making complex shaped preform and silicon carbide composite by melt infiltration

Steibel, James D.↗