Characterization of SiC/SiNC CMC Specimens Containing Embedded SiC Disks
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Kiser, D.↗
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Low-Cost, Large C-SiC Blisk Fabrication
C-SiC composites offer unique properties for propulsion applications. However, fabrication of low-cost, thick, large scale C-SiC disk for integrally bladed disk (blisk) applications has not been established yet. MER has demonstrated a new process to address this issue. Polymer-based processing was employed for interfacial coatings, consolidation and densification. Up to 40" O.C., 2" thick C-SiC composite processing was established, yielding in excess of 1.8 g/cu cm density. Computer tomography (CT) scans on the 40" O.D., 2" thick C-SiC disk showed no visible delamination, and good density uniformity. Stress-rupture testing in air was conducted at 2200 F, 2400 F and 2550 F.
Kowbel, W.↗
Material Development of Faraday Cup Grids for the Solar Probe Plus Mission
The Solar Probe Plus mission will launch a spacecraft to the Sun to study it's outer atmosphere. One of the instruments on board will be a Faraday Cup (FC) sensor. The FC will determine solar wind properties by measuring the current produced by ions striking a metal collector plate. It will be directly exposed to the Sun and will be subject to the temperature and radiation environment that exist within 10 solar radii. Conducting grids within the FC are biased up to 10 kV and are used to selectively transmit particles based on their energy to charge ratio. We report on the development of SiC grids. Tests were done on nitrogen-doped SiC starting disks obtained from several vendors, including annealing under vacuum at 1400 C and measurement of their electrical properties. SiC grids were manufactured using a photolithographic and plasma-etching process. The grids were incorporated into a prototype FC and tested in a simulated solar wind chamber. The energy cutoffs were measured for both proton and electron fluxes and met the anticipated sensor requirements.
Volz, M. P.↗
Assessment of Readout Techniques for Passive Monitors
This fiscal year (FY) 2023 report on passive temperature sensors covers two main objectives: to demonstrate that the optical dilatometer can successfully process disc shaped silicon carbide (SiC) temperature monitors (TMs), and to demonstrate proof of concept for using the capacitance readout method to read printed melt wires. The SiC objective was successfully met by annealing and analyzing, via optical dilatometry, all eight 3-mm SiC discs provided by the Nuclear Science User Facilities (NSUF) Idaho State University (ISU) Nanostructured Steels for Enhanced Radiation Tolerance (N SERT) experiment, which was irradiated at Idaho National Laboratory (INL)’s Advanced Test Reactor (ATR). Per the ISU N SERT experiment, capsule 1 (KGT 3828 1 and KGT 3828-2) had a design temperature of 300°C +/- 50°C and an exposure of 2 dpa +/- 10%; capsule 2 (KGT 4600 and KGT 4609) had a design temperature of 300°C +/- 50°C and an exposure of 6 dpa +/- 10%; capsule 3 (KGT 4639 C and KGT 4639-D) had a design temperature of 500°C +/- 50°C and an exposure of 6 dpa +/- 10%; and capsule 4 (KGT 3841 3 and KGT 3841 4) had a design temperature of 500°C +/- 50°C and an exposure of 2 dpa +/- 10%. The target exposure rates, in dpa, are the neutron damage for various types of nanostructured steels. All but three SiC TMs (KGT 4600, KGT 4639 D, and KGT 3841 4) revealed averaged peak irradiation temperatures that fell within the design temperature ranges. The three SiC TMs that did not fall within the design temperatures ranges were at least 100°C below that target temperature. Furthermore, SiC TM KGT 3841 C revealed two irradiation regimes: one closer to the 300°C design temperature, and the other closer to the 500°C design temperature. Also, all the SiC TMs’ averaged peak irradiation temperatures came in anywhere between 20°C and 240°C below the irradiation temperatures predicted by the thermal models. This showed the optical dilatometry method to be a reliable and less time intensive process for determining averaged peak irradiation temperatures from passive SiC TMs such as rods and discs. Under the Advanced Sensors and Instrumentation (ASI) program in FY-23, Boise State University (BSU) proposed to demonstrate proof of concept for using a capacitance readout technique applicable to printed melt wires; however, they were stymied by the complexity of the capacitance readout method. In support of the BSU work, INL developed an additively manufactured (AM) ceramic package for encapsulating the new melt wires. Inks were synthesized at BSU that used new protocols rather than following previously established protocols implemented at INL, and testing of various temperatures was conducted at BSU to evaluate the melting behaviors of the printed melt wires. The result was that the capacitance readout technique showed promise but also created more challenges than originally anticipated. For example, the tin ink synthesized at BSU showed unusual melting behaviors that did nothing to enhance the performance of the final printed melt wire prototype in terms of the capacitance readout method. To make the proof of concept work when applied to the printed melt wires, the ASI program would need to invest further resources and time. Consequently, the program is not planning to continue this proof of concept work in FY-24, based on the progress and findings achieved in FY-23.
36 MATERIALS SCIENCE↗
Mechanical and Thermophysical Properties of 3D-Printed SiC before and after Neutron Irradiation – FY21
This report presents the mechanical and thermophysical properties of 3D-printed SiC before and after neutron irradiation that have been evaluated to assess the fuel matrix material for the Transformational Challenge Reactor (TCR). The TCR fuel form consists of an additively-manufactured silicon carbide (SiC) matrix and uranium nitride tristructural isotropic (UN TRISO) fuel particles, which is manufactured through a newly developed processing route combining binderjet 3D printing, TRISO fuel particle loading, and chemical vapor infiltration (CVI). Because the fuel matrix is a primary component of the TCR core and its response to mechanical and thermal loads during operation is one of the most influential factors on the integrity of TCR core, testing and evaluation have focused on producing mechanical and thermophysical properties data for the binderjet/CVI SiC. Baseline mechanical and thermophysical properties were measured from the disk specimens printed for different and sizes orientations, which included equibiaxial flexural failure strength, elastic constants, thermal diffusivity and conductivity, density, and the coefficient of thermal expansion. Flexural failure strength datasets showed similar Weibull distributions regardless of sample variants including different orientations. The mean failure strengths of the 3D-printed SiC variants were in the range of 280–310 MPa, which are slightly lower than that of the chemical vapor deposition (CVD) SiC. Thermophysical test results showed that specific heat and thermal expansion are not sensitive to the build direction of SiC samples, while thermal conductivity is highly dependent on the build direction and can be correlated to the anisotropic character of the 3D-printed SiC. Neutron irradiation tests were carried out on the 3D-printed 6-mm diameter SiC disk specimens. Irradiation was carried to 2.3 dpa over a temperature range of 360–880°C. No significant degradation in strength was observed in SiC after irradiations in various conditions and with different orientations. Anisotropy that had been observed in the thermal conductivity of 3D-printed SiC prior to irradiation vanished after irradiation as the irradiation defect thermal resistivity accumulated in the material. Electron microscopy of the microstructure after neutron irradiation showed distinct defect morphologies in the heterogenous material, but no evidence for irradiation-induced cracking or degradation in the microstructure was observed.
11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
Development of Ti 3 SiC 2 MAX phase tubular structures for solar receiver applications
Solar receiver tubes are key components of concentrating solar-thermal power (CSP) systems that harvest solar energy. For better efficiency, the Gen3 CSP receivers, which collect heat into a heat transfer fluid, require a temperature exceeding 700 °C during operation and need to perform under extreme conditions of high temperature and high thermal stress. Operators are seeking CSP designs using new high-temperature structural materials with high thermal conductivity and high creep resistance to achieve a design life of 30 years and thus help recover the plant capital cost sooner. MAX phase materials, which consist of an early transition metal element, an A-group element, and carbon or nitrogen, are expected to exhibit high creep resistance as well as high fracture toughness. Here, in this paper, we describe fabricating both (1) dense Ti 3 SiC 2 MAX phase disks and (2) short-length tubes using field-assisted sintering technology (FAST). First, the disk samples that we fabricated are fully dense and contain ≈90 % Ti 3 SiC 2 MAX phase materials and ≈10 % TiC phase materials. We determined a flexure strength of 519 ± 32 MPa by conducting a four-point bending test at room temperature with rectangular bar samples of ≈100 % density. The thermal conductivity of the Ti 3 SiC 2 MAX phase samples, measured by light flashing analysis, decreases linearly from a value of 41 W . m -1 . K -1 at room temperature to a value of 36 W . m -1 . K -1 at 650 °C. A solar reflectance measurement of the Ti 3 SiC 2 MAX phase revealed that, temperature increases from 400 to 1400 °C, thermal emittance increases from 0.39 to 0.49, while selectivity decreases from 1.8 to 1.4, respectively. Whereas the surface oxidized MAX phase samples after 100 h exposure to air at 1000 °C exhibit that of SiC. Next, we discuss fabrication of the crack-free Ti 3 SiC 2 MAX phase tubular structures accomplished by using FAST processing in graphite bedding. A Ti 3 SiC 2 MAX phase content of > 95 % with traceable ≈3% remaining TiC phase and ≈15 % porosity were demonstrated after high-temperature annealing. An average fracture strength of ≈250 MPa was determined with Ti 3 SiC 2 MAX phase tubes of ≈85 % density by diametral compression testing at room temperature. Our work demonstrated that using FAST processing to produce Ti 3 SiC 2 MAX phase tubular structures for CSP receiver applications is a viable approach.
14 SOLAR ENERGY↗
Deformation and fracture of single-crystal and sintered polycrystalline silicon carbide produced by cavitation
An investigation was conducted to examine the deformation and fracture behavior of single-crystal and sintered polycrystalline SiC surfaces exposed to cavitation. Cavitation erosion experiments were conducted in distilled water at 25 C by using a magnetostrictive oscillator in close proximity (1 mm) to the surface of SiC. The horn frequency was 20 kHz, and the double amplitude of the vibrating disk was 50 microns. The results of the investigation indicate that the SiC (0001) surface could be deformed in a plastic manner during cavitation. Dislocation etch pits were formed when the surface was chemically etched. The number of defects, including dislocations in the SiC (0001) surface, increased with increasing exposure time to cavitation. The presence of intrinsic defects such as voids in the surficial layers of the sintered polycrystalline SiC determined the zones at which fractured grains and fracture pits (pores) were generated. Single-crystal SiC had superior erosion resistance to that of sintered polycrystalline SiC.
Miyoshi, Kazuhisa↗
Deformation and fracture of single-crystal and sintered polycrystalline silicon carbide produced by cavitation
An investigation was conducted to examine the deformation and fracture behavior of single-crystal and sintered polycrystalline SiC surfaces exposed to cavitation. Cavitation erosion experiments were conducted in distilled water at 25 C by using a magnetostrictive oscillator in close proximity (1 mm) to the surface of SiC. The horn frequency was 20 kHz, and the double amplitude of the vibrating disk was 50 microns. The results of the investigation indicate that the SiC (0001) surface could be deformed in a plastic manner during cavitation. Dislocation etch pits were formed when the surface was chemically etched. The number of defects, including dislocations in SiC (0001) surface, increased with increasing exposure time to cavitation. The presence of intrinsic defects such as voids in the surficial layers of the sintered polycrystalline SiC determined the zones at which fractured grains and fracture pits (pores) were generated. Single-crystal SiC had superior erosion resistance to that of sintered polycrystalline SiC.
Miyoshi, Kazuhisa↗
Friction and wear of carbon-graphite materials for high-energy brakes
Caliper type brake simulation experiments were conducted on seven different carbon graphite materials formulations against a steel disk material and against a carbon graphite disk material. The effects of binder level, boron carbide (B4C) additions, SiC additions, graphite fiber additions, and graphite cloth reinforcement on friction and wear behavior were investigated. Reductions in binder level, additions of B4C, and additions of SiC each resulted in increased wear. The wear rate was not affected by the addition of graphite fibers. Transition to severe wear and high friction was observed in the case of graphite-cloth-reinforced carbon sliding against a disk of similar composition. The transition was related to the disruption of a continuous graphite shear film that must form on the sliding surfaces if low wear is to occur.
Bill, R. C.↗
Advanced Gas Turbine (AGT) Technology Project
Engine testing, ceramic component fabrication and evaluation, component performance rig testing, and analytical studies comprised AGT 100 activities during the 1985 year. Ten experimental assemblies (builds) were evaluated using two engines. Accrued operating time was 120 hr of burning and 170 hr total, bringing cumulative total operating time to 395 hr, all devoid of major failures. Tests identified the generator seals as the primary working fluid leakage sources. Power transfer clutch operation was demonstrated. An alpha SiC gasifier rotor engine test resulted in blade tip failures. Recurring case vibration and shaft whip have limited gasifier shaft speeds to 84%. Ceramic components successfully engine tested now include the SiC scroll assembly, Si3N3 turbine rotor, combustor assembly, regenerator disk bulkhead, turbine vanes, piston rings, and couplings. A compressor shroud design change to reduce heat recirculation back to the inlet was executed. Ceramic components activity continues to focus on the development of state-of-the-art material strength characteristics in full-scale engine hardware. Fiber reinforced glass-ceramic composite turbine (inner) backplates were fabricated by Corning Glass Works. The BMAS/III material performed well in engine testing. Backplates of MAS material have not been engine tested.
Source record↗
Structural Design Parameters for Germanium
The fracture toughness and slow crack growth parameters of germanium supplied as single crystal beams and coarse grain disks were measured. Although germanium is anisotropic (A* 1.7), it is not as anisotropic as SiC, NiAl, or Cu. Thus the fracture toughness was similar on the 100, 110, and 111 planes, however, measurements associated with randomly oriented grinding cracks were 6 to 30 higher. Crack extension in ring loaded disks occurred on the 111 planes due to both the lower fracture energy and the higher stresses on stiff 111 planes. Germanium exhibits a Weibull scale effect, but does not exhibit significant slow crack growth in distilled water. (n 100), implying that design for quasi static loading can be performed with scaled strength statistics. Practical values for engineering design are a fracture toughness of 0.69 0.02 MPam (megapascals per square root meter) and a Weibull modulus of m 6 2. For well ground and reasonable handled coupons, average fracture strength should be greater than 40 megapascals. Aggregate, polycrystalline elastic constants are Epoly 131 gigapascals, vpoly 0.22.
fracture toughness↗
Zodiac II: Debris Disk Science from a Balloon
Zodiac II is a proposed balloon-borne science investigation of debris disks around nearby stars. Debris disks are analogs of the Asteroid Belt (mainly rocky) and Kuiper Belt (mainly icy) in our Solar System. Zodiac II will measure the size, shape, brightness, and color of a statistically significant sample of disks. These measurements will enable us to probe these fundamental questions: what do debris disks tell us about the evolution of planetary systems; how are debris disks produced; how are debris disks shaped by planets; what materials are debris disks made of; how much dust do debris disks make sa they grind down; and how long do debris disks live? In addition, Zodiac II will observe hot, young exoplanets as targets of opportunity. The Zodiac II instrument is a 1.1-m diameter SiC telescope and an imaging coronagraph on a gondola carried by a stratospheric balloon. Its data product is a set of images of each targeted debris disk in four broad visible wavelength bands. Zodiac II will address its science questions by taking high-resolution, multi-wavelength images of the debris disks around tens of nearby stars. Mid-latitude flights are considered: overnight test flights within the United States followed by half-global flights in the Southern Hemisphere. These longer flights are required to fully explore the set of known debris disks accessible only to Zodiac II. On these targets, it will be 100 times more sensitive than the Hubble Space Telescope's Advanced Camera for Surveys (HST/ACS); no existing telescope can match the Zodiac II contrast and resolution performance. A second objective of Zodiac II is to use the near-space environment to raise the Technology Readiness Level (TRL) of SiC mirrors, internal coronagraphs, deformable mirrors, and wavefront sensing and control, all potentially needed for a future space-based telescope for high-contrast exoplanet imaging.
Bryden, Geoffrey↗
Zodiac II: Debris Disk Science from a Balloon
Zodiac II is a proposed balloon-borne science investigation of debris disks around nearby stars. Debris disks are analogs of the Asteroid Belt (mainly rocky) and Kuiper Belt (mainly icy) in our Solar System. Zodiac II will measure the size, shape, brightness, and color of a statistically significant sample of disks. These measurements will enable us to probe these fundamental questions: what do debris disks tell us about the evolution of planetary systems; how are debris disks produced; how are debris disks shaped by planets; what materials are debris disks made of; how much dust do debris disks make as they grind down; and how long do debris disks live? In addition, Zodiac II will observe hot, young exoplanets as targets of opportunity. The Zodiac II instrument is a 1.1-m diameter SiC (Silicone carbide) telescope and an imaging coronagraph on a gondola carried by a stratospheric balloon. Its data product is a set of images of each targeted debris disk in four broad visible-wavelength bands. Zodiac II will address its science questions by taking high-resolution, multi-wavelength images of the debris disks around tens of nearby stars. Mid-latitude flights are considered: overnight test flights in the US followed by half-global flights in the Southern Hemisphere. These longer flights are required to fully explore the set of known debris disks accessible only to Zodiac II. On these targets, it will be 100 times more sensitive than the Hubble Space Telescope's Advanced Camera for Surveys (HST/ACS); no existing telescope can match the Zodiac II contrast and resolution performance. A second objective of Zodiac II is to use the near-space environment to raise the Technology Readiness Level (TRL) of SiC mirrors, internal coronagraphs, deformable mirrors, and wavefront sensing and control, all potentially needed for a future space-based telescope for high-contrast exoplanet imaging.
suborbital↗
Sliding wear of self-mated Al2O3-SiC whisker reinforced composites at 23-1200 C
Microstructural changes occurring during sliding wear of self-mated Al2O3-SiC whisker reinforced composites were studied using optical, scanning electron microscopy, and transmission electron microscopy. Pin-on-disk specimens were slid in air at 2.7 m/sec sliding velocity under a 26.5 N load for 1 hr. Wear tests were conducted at 23, 600, 800, and 1200 C. Mild wear with a wear factor of 2.4 times 10(exp -7) to 1.5 times 10(exp -6) cu mm/Nm was experienced at all test temperatures. The composite shows evidence of wear by fatigue mechanisms at 800 C and below. Tribochemical reaction (SiC oxidation and reaction of SiO2 and Al2O3) leads to intergranular failure at 1200 C. Distinct microstructural differences existing at each test temperature are reported.
Farmer, Serene C.↗
Slow Crack Growth of Germanium
The fracture toughness and slow crack growth parameters of germanium supplied as single crystal beams and coarse grain disks were measured. Although germanium is anisotropic (A=1.7), it is not as anisotropic as SiC, NiAl, or Cu, as evidence by consistent fracture toughness on the 100, 110, and 111 planes. Germanium does not exhibit significant slow crack growth in distilled water. (n=100). Practical values for engineering design are a fracture toughness of 0.7 MPam and a Weibull modulus of m=6+/-2. For well ground and reasonable handled coupons, fracture strength should be greater than 30 MPa.
Stress Corrosion Susceptibility↗
Processing and properties of SiC composites made via binder jet 3D printing and infiltration and pyrolysis of preceramic polymer
The effect of polymer infiltration and pyrolysis (PIP) cycles with polycarbosiloxane on the microstructure, air leak rate, and properties of SiC composites manufactured by a combination of binder jet 3D printing and PIP are reported. The density, Young’s modulus and flexural strength of disk-shaped components increased with the number of PIP cycles. In the case of density, it increased from 2.05 g/cm 3 in one PIP cycle to 2.33 g/cm 3 after three PIP cycles, while values of flexural strength and Young’s modulus at room temperature after three PIP cycles reached 66.8 ± 2.5 MPa and 69.5 ± 2.8 GPa, respectively. Conversely, the air leak rate was found to decrease with number of PIP cycles, and it reached a value of 4 mbar-liter/s after three cycles. The instantaneous coefficient of thermal expansion of the composite was found to change minimally with the number of PIP cycles and had a value of 4 ± 1.2 ppm/°C between 200°C and 1,000°C. Thermal conductivity was found to increase with number of PIP cycles and to decrease with temperature. For example, after 3 PIP cycles it was found to change from 6.72 ± 0.08 to 6.98 ± 0.08 W/mK at 25°C and 7.36 ± 0.08 to 7.96 ± 0.08 W/mK at 300°C. These values were lower than those of crystalline SiC because of the amorphous nature of the matrix and the presence of pores and cracks.
36 MATERIALS SCIENCE↗
Comparison of NDE techniques for sintered-SiC components
High frequency, bulk-wave ultrasonics detected defects in manufactured SiC components. In addition, gas-turbine blades and vanes were examined by scanning laser acoustic microscopy (SLAM). Comparative results obtained on simple shapes such as disks and bars by microfocus X-ray radiography, ultrasonics, scanning photoacoustic spectroscopy, and SLAM are discussed.
Srinivasan, M.↗
NASA Tech Briefs, July 2004
Topics: Optoelectronic Sensor System for Guidance in Docking; Hybrid Piezoelectric/Fiber-Optic Sensor Sheets; Multisensor Arrays for Greater Reliability and Accuracy; Integrated-Optic Oxygen Sensors; Ka-Band Autonomous Formation Flying Sensor; CMOS VLSI Active-Pixel Sensor for Tracking; Lightweight, Self-Deploying Foam Antenna Structures; Electrically Small Microstrip Quarter-Wave Monopole Antennas; A 2-to-28-MHz Phase-Locked Loop; Portable Electromyograph; Open-Source Software for Modeling of Nanoelectronic Devices; Software for Generating Strip Maps from SAR Data; Calibration Software for use with Jurassicprok; Software for Probabilistic Risk Reduction; Software Processes SAR Motion-Measurement Data; Improved Method of Purifying Carbon Nanotubes; Patterned Growth of Carbon Nanotubes or Nanofibers; Lightweight, Rack-Mountable Composite Cold Plate/Shelves; SiC-Based Miniature High-Temperature Cantilever Anemometer; Inlet Housing for a Partial-Admission Turbine; Lightweight Thermoformed Structural Components and Optics; Growing High-Quality InAs Quantum Dots for Infrared Lasers; Selected Papers on Protoplanetary Disks; Module for Oxygenating Water without Generating Bubbles; Coastal Research Imaging Spectrometer; Rapid Switching and Modulation by use of Coupled VCSELs; Laser-Induced-Fluorescence Photogrammetry and Videogrammetry; Laboratory Apparatus Generates Dual-Species Cold Atomic Beam; Laser Ablation of Materials for Propulsion of Spacecraft; Small Active Radiation Monitor; Hybrid Image-Plane/Stereo Manipulation; Partitioning a Gridded Rectangle into Smaller Rectangles; Digital Radar-Signal Processors Implemented in FPGAs; Part 1 of a Computational Study of a Drop-Laden Mixing Layer; and Some Improvements in Signal-Conditioning Circuits.
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