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NASA NTRS1992

Approaches to polymer-derived CMC matrices

The use of polymeric precursors to ceramics permits the fabrication of large, complex-shaped ceramic matrix composites (CMC's) at temperatures which do not degrade the fiber. Processing equipment and techniques readily available in the resin matrix composite industry can be adapted for CMC fabrication using this approach. Criteria which influence the choice of candidate precursor polymers, the use of fillers, and the role of fiber architecture and ply layup are discussed. Three polymer systems, polycarbosilanes, polysilazanes, and polysilsesquioxanes, are compared as candidate ceramic matrix precursors.

Hurwitz, Frances I.↗

DOE OSTI2021

SNF Canister Coatings for Corrosion Prevention and Mitigation (FY21 Status Report)

This report summarizes the current actives in FY21 related to the effort by Sandia National Laboratories to identify and test coating materials for the prevention, mitigation, and repair of spent nuclear fuel dry storage canisters against potential chloride-induced stress corrosion cracking. This work follows up on the details provided in Sandia National Laboratories FY20 report on the same topic, which provided a detailed description of the specific coating properties desired for application and implementation on spent nuclear fuel canisters, as well as provided detail into several different coatings and their applicability to coat spent nuclear fuel canisters. In FY21, Sandia National Laboratories has engaged with private industry to create a Memorandum of Understanding and established a collaborative R&D program building off the analytical and laboratory capabilities at Sandia National Laboratories and the material design and synthesis capabilities of private industry. The resulting Memorandum of Understanding included four companies to date (Oxford Performance Materials, White Horse R&D, Luna Innovations, and Flora Coating) proposing six different coating technologies (polyetherketoneketone, modified polyimide/polyurea, modified phenolic resin, silane-based polyurethane hybrid with and without a Znrich primer, and a quasi-ceramic sol-gel polyurethane hybrid) to be tested, evaluated, and optimized for their potential use for this application. This report provides a detailed description of each of the coating systems proposed by the participating industry partners. It also provides a description of the planned experimental actives to be performed by Sandia National Laboratories including physical tests, electrochemical tests, and characterization methods. These analyses will be used to identify specific ways to further improve coating technologies toward their application and implementation on spent nuclear fuel canisters. In FY21, Sandia National Laboratories began baseline testing of the base metal material in according with activities of the Memorandum of Understanding. In FY22, Sandia National Laboratories will receive coated coupons from each of the participating industry partners and begin characterization, physical, and electrochemical testing following the test plan described herein.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2024

Scalable, Infiltration-Free Ceramic Matrix Composite Manufacturing

Manufacturing of ceramic matrix composites (CMCs) with carbon fiber and carbon matrix includes a time- and labor-intensive ceramic infiltration step that is responsible for more than half of the total manufacturing cost. To make CMCs cost-competitive in price-sensitive markets, like concentrated solar power, it is essential to develop a CMC manufacturing process that skips the ceramic infiltration process. In this work, we will show how a high-char-yield preceramic resin can eliminate the infiltration step while maintaining material density and evaluate the technoeconomic impact of our CMC manufacturing process. We monitor both morphology and porosity to determine the quality of CMCs made with different preceramic resins and evaluate the impact of polymer infiltration and pyrolyzing cycles.

matrix composite, polymer infiltration and pyrolys↗

DOE OSTI2024

Reinforcement induced microcracking during the conversion of polymer-derived ceramics

This study investigates the role of discontinuous reinforcement on the microcracking of a preceramic polymer matrix during polymer to ceramic conversion. The material system comprised a carbosilane-based, preceramic polymer reinforced with mullite particles. The preceramic resin slurry was formulated for photopolymerization on a digital light projection 3D printer. Micro X-ray computed tomography, using a synchrotron light source, monitored a printed composite part during pyrolysis. The conversion of the carbosilane matrix into Si(O)C generated microcracks in the matrix that radially extended from particles. The likelihood of microcrack formation positively correlated with particle size. The largest particles (>10 4 µm 3 volume or >60 µm side length) always abutted microcracks, while the matrix surrounding smaller particles (<5 µm) was free of microcracks. Numerical calculations showed the particles resist the shrinking matrix during its conversion. This created tensile stresses within the matrix. The driving force for microcrack growth was also analyzed with regard to the influence of matrix material parameters, particle form-factor and crack length. These results reveal the need to consider the form factor of discontinuous reinforcements, with regard to the material properties of the polymer-derived ceramic, in order to reduce or eliminate defects in the final part.

36 MATERIALS SCIENCE↗

NASA NTRS2013

Testing of Advanced Conformal Ablative TPS

In support of the CA250 project, this paper details the results of a test campaign that was conducted at the Ames Arcjet Facility, wherein several novel low density thermal protection (TPS) materials were evaluated in an entry like environment. The motivation for these tests was to investigate whether novel conformal ablative TPS materials can perform under high heat flux and shear environment as a viable alternative to rigid ablators like PICA or Avcoat for missions like MSL and beyond. A conformable TPS over a rigid aeroshell has the potential to solve a number of challenges faced by traditional rigid TPS materials (such as tiled Phenolic Impregnated Carbon Ablator (PICA) system on MSL, and honeycomb-based Avcoat on the Orion Multi Purpose Crew Vehicle (MPCV)). The compliant (high strain to failure) nature of the conformable ablative materials will allow better integration of the TPS with the underlying aeroshell structure and enable monolithic-like configuration and larger segments to be used in fabrication.A novel SPRITE1 architecture, developed by the researchers at NASA Ames was used for arcjet testing. This small probe like configuration with 450 spherecone, enabled us to test the materials in a combination of high heat flux, pressure and shear environment. The heat flux near the nose were in the range of 500-1000 W/sq cm whereas in the flank section of the test article the magnitudes were about 50 of the nose, 250-500W/sq cm range. There were two candidate conformable materials under consideration for this test series. Both test materials are low density (0.28 g/cu cm) similar to Phenolic Impregnated Carbon Ablator (PICA) or Silicone Impregnated Refractory Ceramic Ablator (SIRCA) and are comprised of: A flexible carbon substrate (Carbon felt) infiltrated with an ablative resin system: phenolic (Conformal-PICA) or silicone (Conformal-SICA). The test demonstrated a successful performance of both the conformable ablators for heat flux conditions between 50-500 W/sq cm. The recession and temperature profile for these materials were comparable to PICA proving them to be viable alternatives for TPS technology development for future missions.

Gasch, Matthew↗

DOE OSTI2021

Properties of SiC-Si made via binder jet 3D printing of SiC powder, carbon addition, and silicon melt infiltration

In this work, we report the physical and mechanical properties of ceramic composite materials fabricated by binder jet 3D printing (BJ3DP) with silicon carbide (SiC) powders, followed by phenolic resin infiltration and pyrolysis (IP) to generate carbon, and a final reactive silicon melt infiltration step. After two phenolic resin infiltration and pyrolysis cycles; porosity was less than 2%, Young's modulus was close to 300 GPa, and the flexural strength was 517.6 ± 24.8 MPa. However, diminishing returns were obtained after more than two phenolic resin infiltration and pyrolysis cycles as surface pores in carbon were closed upon the formation of SiC, resulting in reaction choking and residual-free carbon and porosity. The instantaneous coefficient of thermal expansion of the composite was found to be independent of the number of phenolic IP cycles and had values of between 4.2 and 5.0 ppm/°C between 300 and 100°C, whereas the thermal conductivity was found to have a weak dependence on the number of phenolic IP cycles. While the manufacturing procedures described here yielded highly dense, gas impermeable, siliconized SiC composites with properties comparable to those of bulk siliconized silicon carbide processed according to conventional techniques, BJ3DP enables the manufacture of objects with complex shape, unlike conventional techniques.

36 MATERIALS SCIENCE↗

NASA NTRS1995

Low Cost Fabrication of Silicon Carbide Based Ceramics and Fiber Reinforced Composites

A low cost processing technique called reaction forming for the fabrication of near-net and complex shaped components of silicon carbide based ceramics and composites is presented. This process consists of the production of a microporous carbon preform and subsequent infiltration with liquid silicon or silicon-refractory metal alloys. The microporous preforms are made by the pyrolysis of a polymerized resin mixture with very good control of pore volume and pore size thereby yielding materials with tailorable microstructure and composition. Mechanical properties (elastic modulus, flexural strength, and fracture toughness) of reaction-formed silicon carbide ceramics are presented. This processing approach is suitable for various kinds of reinforcements such as whiskers, particulates, fibers (tows, weaves, and filaments), and 3-D architectures. This approach has also been used to fabricate continuous silicon carbide fiber reinforced ceramic composites (CFCC's) with silicon carbide based matrices. Strong and tough composites with tailorable matrix microstructure and composition have been obtained. Microstructure and thermomechanical properties of a silicon carbide (SCS-6) fiber reinforced reaction-formed silicon carbide matrix composites are discussed.

Singh, M.↗

NASA NTRS1961

Development of Ceramic Fibers for Reinforcement in Composite Materials

Refinements of the vertical arc fiberizing apparatus resulted in its ability to fiberize very different refractory glasses having wide ranges of properties. Although the apparatus, was originally designed as a laboratory research tool for the evaluation of many compositions daily, up to one quarter pound of fibers of a single composition could be produced in an 8-hour day. Fibers up to six and a half feet long were produced with the apparatus. Studies were conducted of two methods of fiberizing refractory glasses requiring rapid freezing from the melt. The first method consisted of fiberizing droplets of molten glass passing through an annular nozzle. The second method consisted of reconstructing the annular nozzle in. the shape of a horseshoe to achieve a shorter delay in blasting a molten droplet from the tip of a rod. Both methods were judged feasible for producing fibers of glasses requiring rapid freezing. The first method would be more amenable to volume fiber production. Studies of induction heating for fiber formation did not lead to its designation as a very efficient heating method. Problems. remain to be solved, in the design of a suitable susceptor for a higher heating rate, in protecting the susceptor from oxidation with an inert gas, in contamination of the melt from a refractory crucible, and in the protective radiation shielding of the induction concentrator coil. It is not considered practical to continue studies of this heating method. In the course of this program 151 refractory glass compositions were evaluated for fiber, forming characteristics. Of the various types of materials studied, the following showed promise in producing acceptable refractory fibers: sIlica- spinel (magnesium aluminate), silica- spinel-zirconia, silica-zirconia, silica-zinc spinel, aluminum phosphate glasses, and fluoride glasses. Compositions which did not produce acceptable fibers were high zirconia materials, barium spinels, and calcium aluminates. Improvements in the. testing apparatus for single fiber tensile strength increased the precision. of tests conducted on nine fibers. The highest mean tensile strength, a value of 295,000 pounds per square inch, was obtained with R-141 fibers. Treatment of R-74 fibers with anhydrous Linde A-1100 silane finish improved its mean fiber tensile strength by 25 percent. The lapse of time after fiber formation had no measurable effect on tensile strength. A static heating test conducted with various high melting fibers indicated that Fiberfrax and R-108 underwent no significant changes in bulk volume or resiliency on exposure to 2750 degrees Fahrenheit (1510 degrees Centigrade) in an oxidizing atmosphere. For fiber-resin composition fabrication, ten fiber materials were selected on the bases of high fiber yield, fusion temperature, and type of composition. Fiberfrax, a commercial ceramic fiber, was included for comparison. A new, more effective method of removing pellets from blown fibers was developed. The de-pelletized fibers were treated with a silane finish and felted into ten-inch diameter felts prior to resin impregnation. Composites containing 30 percent by weight of CTL 91-LD phenolic resin were molded under high pressure from the impregnated felts and post-cured to achieve optimum properties. Flexural strength, flexural modules of elasticity, and punch shear strength tests were conducted on the composite specimens. The highest average flexural strength obtained was 19,958 pounds per square inch with the R-74-fiber-resin composite. This compares very favorably with the military specification of 13,000 pounds per square inch flexural strength for randomly oriented fiber reinforced composites. The highest punch shear strength (11,509 pounds per square inch) was obtained with the R-89 fiber-resin composite. The effects of anhydrous fiber finishes on composite strength were not clearly indicated. Plasma arc tests at a heat flux of 550 British Thermal Units per square foot per second on eight composite materials indicated ablation rates generally equivalent to Fiberglas-Micarta No. 259-2. The composite reinforced with R-99 fibers had an average ablation rate of 0.008 inch per second and appears quite promising on the basis of these tests. Preliminary studies for processing fibers into yarn and fabric were conducted with R-99 fibers. The use of certain organic gums aided in 2 fabricating by hand several relatively strong yarns and a crude fabric swatch. This indicated the practicality of developing techniques for processing these fibers into yarn and fabric without significant damage to the fibers.

Gates, L. E.↗

NASA NTRS1994

Development of lightweight ceramic ablators and arc-jet test results

Lightweight ceramic ablators (LCA's) were recently developed at Ames to investigate the use of low density fibrous substrates and organic resins as high temperature, high strength ablative heat shields. Unlike the traditional ablators, LCA's use porous ceramic/carbon fiber matrices as substrates for structural support, and polymeric resins as fillers. Several substrates and resins were selected for the initial studies, and the best performing candidates were further characterized. Three arcjet tests were conducted to determine the LCA's thermal performance and ablation characteristics in a high enthalpy, hypersonic flow environment. Mass loss and recession measurements were obtained for each sample at post test, and the recession rates were determined from high speed motion films. Surface temperatures were also obtained from optical pyrometers.

Tran, Huy K.↗

DOE OSTI2023

Upscaling of asymmetric hollow fiber‐supported thin film membranes for oxygen separation from air: Proof of concept

Abstract Hollow fiber membranes demonstrate various advantages for high performance oxygen separation. However, the small diameters of hollow fibers and the brittleness of ceramics limit their mechanical strength, imposing great difficulties on stack and module development. Gas‐tight sealing is another challenge for upscaling of hollow fiber membrane technology. Low temperature sealant materials of epoxy resin or silicon are typically used for hollow fiber stacks, requiring that the sealing portions be located out of hot zone. Consequently, only partial length of hollow fibers participates in oxygen permeation. In this study, upscaling of our recently developed asymmetric hollow fiber‐supported thin film membranes is conducted, where individual hollow fibers are assembled in parallel to form a stack. A reliable gas‐tight sealing is obtained by combining ceramic paste with conductive adhesive ink cohesively. Comprehensive oxygen permeation test is conducted with the sealing portions being in hot zone and compared with a single hollow fiber membrane. Fundamental mechanism is discussed to understand the performances and their differences. An accelerated long‐term test (∼320 h, 16 thermal cycles) demonstrates excellent stability and robustness of the stack and sealing. The characterization of post‐test samples further confirms excellent stability and robustness of the phases and microstructures of the stack.

36 MATERIALS SCIENCE↗

NASA NTRS1985

Fabrication of Slender Struts for Deployable Antennas

High moduli of elasticity potentially achievable. Suited for application in large diameter antennas on orbiting spacecraft. Fabrication process can accurately place dry graphite fibers and overwrap them with aluminum foil, resulting in straight, slender graphite tubes. Graphite fibers pulled out of creeled spools and fed through ceramic eyelets. Spools of aluminum foil mounted on rotating ring and capture graphite fiber as vertical winding machine carriage moves upward. Epoxy resin applied by mechanically spreading epoxy on tetrafluoroethylene mandrel by means of doctor blade attached to carriage.

Bush, H. G.↗

NASA NTRS2006

NASA Tech Briefs, June 2006

Topics covered include: Magnetic-Field-Response Measurement-Acquisition System; Platform for Testing Robotic Vehicles on Simulated Terrain; Interferometer for Low-Uncertainty Vector Metrology; Rayleigh Scattering for Measuring Flow in a Nozzle Testing Facility; "Virtual Feel" Capaciflectors; FETs Based on Doped Polyaniline/Polyethylene Oxide Fibers; Miniature Housings for Electronics With Standard Interfaces; Integrated Modeling Environment; Modified Recursive Hierarchical Segmentation of Data; Sizing Structures and Predicting Weight of a Spacecraft; Stress Testing of Data-Communication Networks; Framework for Flexible Security in Group Communications; Software for Collaborative Use of Large Interactive Displays; Microsphere Insulation Panels; Single-Wall Carbon Nanotube Anodes for Lithium Cells; Tantalum-Based Ceramics for Refractory Composites; Integral Flexure Mounts for Metal Mirrors for Cryogenic Use; Templates for Fabricating Nanowire/Nanoconduit- Based Devices; Measuring Vapors To Monitor the State of Cure of a Resin; Partial-Vacuum-Gasketed Electrochemical Corrosion Cell; Theodolite Ring Lights; Integrating Terrain Maps Into a Reactive Navigation Strategy; Reducing Centroid Error Through Model-Based Noise Reduction; Adaptive Modeling Language and Its Derivatives; Stable Satellite Orbits for Global Coverage of the Moon; and Low-Cost Propellant Launch From a Tethered Balloon

Source record↗

NASA NTRS1989

Ceramic Honeycomb Panels

Ceramic honeycomb panels serve as lightweight, heat-resistant structural members. Depending on choice of ceramic materials, panels expected to withstand temperatures as high as 1,800 degree C. Honeycomb structure made by vapor-depositing ceramic on fabric substrate woven in honeycomb pattern, then eliminating substrate by oxidizing it. Fabric made of loosely woven polymer such as polyacrylonitrile. Impregnated with organic binder such as phenolic resin for stiffness.

Cagliostro, Domenick E.↗

NASA NTRS1995

Flame-Resistant Composite Materials For Structural Members

Matrix-fiber composite materials developed for structural members occasionally exposed to hot, corrosive gases. Integral ceramic fabric surface layer essential for resistance to flames and chemicals. Endures high temperature, impedes flame from penetrating to interior, inhibits diffusion of oxygen to interior where it degrades matrix resin, resists attack by chemicals, helps resist erosion, and provides additional strength. In original intended application, composite members replace steel structural members of rocket-launching structures that deteriorate under combined influences of atmosphere, spilled propellants, and rocket exhaust. Composites also attractive for other applications in which corrosion- and fire-resistant structural members needed.

Spears, Richard K.↗

NASA NTRS2010

Multi-functional layered structure having structural and radiation shielding attributes

A cosmic and solar radiation shielding structure that also has structural attributes is comprised of three layers. The first layer is 30-42 percent by volume of ultra-high molecular weight (UHMW) polyethylene fibers, 18-30 percent by volume of graphite fibers, and a remaining percent by volume of an epoxy resin matrix. The second layer is approximately 68 percent by volume of UHMW polyethylene fibers and a remaining percent by volume of a polyethylene matrix. The third layer is a ceramic material.

Kaul, Raj K.↗

NASA NTRS2008

Polymer Coats Leads on Implantable Medical Device

Langley Research Center s Soluble Imide (LaRC-SI) was discovered by accident. While researching resins and adhesives for advanced composites for high-speed aircraft, Robert Bryant, a Langley engineer, noticed that one of the polymers he was working with did not behave as predicted. After putting the compound through a two-stage controlled chemical reaction, expecting it to precipitate as a powder after the second stage, he was surprised to see that the compound remained soluble. This novel characteristic ended up making this polymer a very significant finding, eventually leading Bryant and his team to win several NASA technology awards, and an "R&D 100" award. The unique feature of this compound is the way that it lends itself to easy processing. Most polyimides (members of a group of remarkably strong and incredibly heat- and chemical-resistant polymers) require complex curing cycles before they are usable. LaRC-SI remains soluble in its final form, so no further chemical processing is required to produce final materials, like thin films and varnishes. Since producing LaRC-SI does not require complex manufacturing techniques, it has been processed into useful forms for a variety of applications, including mechanical parts, magnetic components, ceramics, adhesives, composites, flexible circuits, multilayer printed circuits, and coatings on fiber optics, wires, and metals. Bryant s team was, at the time, heavily involved with the aircraft polymer project and could not afford to further develop the polymer resin. Believing it was worth further exploration, though, he developed a plan for funding development and submitted it to Langley s chief scientist, who endorsed the experimentation. Bryant then left the high-speed civil transport project to develop LaRC-SI. The result is an extremely tough, lightweight thermoplastic that is not only solvent-resistant, but also has the ability to withstand temperature ranges from cryogenic levels to above 200 C. The thermoplastic s unique characteristics lend it to many commercial applications; uses that Bryant believed would ultimately benefit industry and the Nation. "LaRC-SI," he explains, "is a product created in a government laboratory, funded with money from the tax-paying public. What we discovered helps further the economic competitiveness of the United States, and it was our goal to initiate the technology transfer process to ensure that our work benefited the widest range of people." Several NASA centers, including Langley, have explored methods for using LaRC-SI in a number of applications from radiation shielding and as an adhesive to uses involving replacement of conventional rigid circuit boards. In the commercial realm, LaRC-SI can now be found in several commercial products, including the thin-layer composite unimorph ferroelectric driver and sensor (THUNDER) piezoelectric actuator, another "R&D 100" award winner (Spinoff 2005).

Source record↗

DOE OSTI2021

Characterization of Highly Thermally Conductive Organic Substrates for a Double-Sided Cooled Power Module

Abstract Silicon-Carbide (SiC) power devices have become a promising option for traditional Silicon (Si) due to the superior material properties. To fully take advantage of the SiC devices, a high-performance power device packaging solution is necessary. This study proposes a cost-effective double-sided cooled (DSC) 1.2 kV SiC half-bridge power module using organic epoxy-resin composite dielectric (ERCD) substrates. The high mechanical and thermal performance of the power module is achieved by the low-modulus, moderate thermal conductivity, and relatively thin (120 μm) layer of ERCD material compared with traditional metal-clad ceramic approaches. This novel organic dielectric can withstand high voltage (5 kV @ 120 μm) and operate up to 250°C continuously, which is indispensable for high power applications. The thermal modeling results show that the equivalent thermal resistance junction-to-case (Rjc_eq) of the DSC power module using dual direct bonded copper (DBC) is 17% higher than the dual ERCD configuration. Furthermore, a non-insulated DSC power module concept is proposed for maximizing thermal performance by considering thermal vias in the ERCD substrate and direct-soldered heat sink. A thought process for optimization of thermal via design is demonstrated and it shows up to 24% of improvement on thermal performance compared with the insulated DSC power module.

Double-sided cooling, epoxy-resin composite dielec↗

NASA NTRS1998

Process for making silicon carbide reinforced silicon carbide composite

A process comprising the steps of: a) providing a fiber preform comprising a non-oxide ceramic fiber with at least one coating, the coating comprising a coating element selected from the group consisting of carbon, nitrogen, aluminum and titanium, and the fiber having a degradation temperature of between 1400.degree. C. and 1450.degree. C., b) impregnating the preform with a slurry comprising silicon carbide particles and between 0.1 wt % and 3 wt % added carbon c) providing a cover mix comprising: i) an alloy comprising a metallic infiltrant and the coating element, and ii) a resin, d) placing the cover mix on at least a portion of the surface of the porous silicon carbide body, e) heating the cover mix to a temperature between 1410.degree. C. and 1450.degree. C. to melt the alloy, and f) infiltrating the fiber preform with the melted alloy for a time period of between 15 minutes and 240 minutes, to produce a ceramic fiber reinforced ceramic composite.

Lau, Sai-Kwing↗