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At least 19 records

Polymer precursors for SiC ceramic materials

Work on precursor polymers to SiC was performed, concentrating on polymers made from decamethyl cyclohexasilyene units. The initial approach was to synthesize mixed diphenyl decamethyl cyclohexasilane, dephenylate, and polymerize. This produced polymers which had yields of up to 50 percent SiC. (Theoretical yield is 75 percent). The present approach is to make the polymer through the intermediate trans-1,4-diphenyl decamethyl cyclohexasilane. This should produce a crystalline polymer and high strength fibers. These will be thermally decomposed to SiC fibers. This requires new chemistry which is currently being studied.

Litt, Morton H.↗

Isomeric Trisaryloxycyclotriphosphazene Polymer Precursors

Substances useful for making heat-and fire-resistant polymers. Cyclotriphosphazene-based monomers and polymer precursors led to development of high-temperature materials. Cyclotriphosphazene-derived monomers, polymer precursors, and polymers becoming important from both industrial and scientific points of view. Presence of phosphazene moiety in cyclotriphosphazene-based monomers and polymer precursors expected to impact special properties in desired high-performance materials containing inorganic backbones for aerospace applications. Useful for obtaining heat-and fire-resistant polymers for composites, adhesives, molding powders, and coating laminates. Also used in structures (e.g. secondary structures in aircraft), in construction of spacecraft, and in electronics and computer industries.

St. Clair, Terry L.↗

Ceramic fibers from Si-B-C polymer precursors

Non-oxide ceramics such as silicon carbide (SiC), silicon nitride (Si3N4), and silicon borides (SiB4, SiB6) have thermal stability, oxidation resistance, hardness, and varied electrical properties. All these materials can be prepared in a fiber form from a suitable polymer precursor. The above mentioned fibers, when tested over a temperature range from 25 to 1400 C, experience degradation at elevated temperatures. Past work in ceramic materials has shown that the strength of ceramics containing both carbides and borides is sustained at elevated temperatures, with minimum oxidation. The work presented here describes the formation of ceramic fibers containing both elements, boron and silicon, prepared via the polymer precursor route previously reported by the authors, and discusses the fiber mechanical properties that are retained over the temperature range studied.

Riccitiello, S. R.↗

Polymer precursors for ceramic matrix composites

The synthesis and characterization of a polycyclohexasilane is reported. Because of its cyclic structure, it is anticipated that this polymer might serve as a precursor to SIC having a high char yield with little rearrangement to form small, volatile cyclic silanes, and, as such, would be of interest as a precursor to SiC composite matrices and fibers, or as a binder in ceramic processing. Several approaches to the synthesis of a bifunctional cyclic monomer were attempted; the most successful of these was metal coupling of PhMeSiCl2 and Me2SiCl2. The procedure gives six-membered ring compounds with all degrees of phenyl substitution, from none to hexaphenyl. The compounds with from 0-2 groups were isolated and characterized. The fraction with degree of phenyl substitution equal to 2, a mixture of cis and trans 1,2-; 1,3-; and 1,4 isomers, was isolated in 32 percent yield. Pure 1,4 diphenyldecamethylcyclohexasilane was isolated from the mixed diphenyl compounds and characterized. Diphenyldecamethylcyclohexasilanes were dephenylated to dichlorodecamethylcyclohexasilanes by treating with H2SO4.NH4Cl in benzene. The latter were purified and polymerized by reacting with sodium in toluene. The polymers were characterized by HPGPC, elemental analysis, proton NMR, and IR. Thermogravimetric analyses were carried out on the polymers. As the yield of residual SiC was low, polymers were heat treated to increase the residual char yield. As high as 51.52 percent residual char yield was obtained in one case.

Litt, M. H.↗

Processing and Characterization of Basalt Fiber Reinforced Ceramic Composites for High Temperature Applications Using Polymer Precursors

The development of high temperature structural composite materials has been very limited due to the high cost of the materials and the processing needed. Polymer Derived Ceramics (PDCs) begin as a polymer matrix, which allows a shape to be formed prior to the cure, and is then pyrolized in order to obtain a ceramic with the associated thermal and mechanical properties. The two PDCs used in this development are polysiloxane and polycarbosilane. Basalt fibers are used for the reinforcement in the composite system. The use of basalt in structural and high temperature applications has been under development for over 50 years, yet there has been little published research on the incorporation of basalt fibers as a reinforcement in composites. Continuous basalt fiber reinforced PDCs have been fabricated and tested for the applicability of this composite system as a high temperature structural composite material.

High Temperature Composites↗

Polymer precursors for ceramic composites

The fiber composite approach to reinforced ceramics provides the possibility of achieving ceramics with high fracture toughness relative to monolithics. Fabrication of ceramic composites, however, demands low processing temperatures to avoid fiber degradation. Formation of complex shapes further requires small diameter fibers as well as techniques for infiltrating the matrix between fibers. Polymers offer low temperature processability, control of rheology not available with ceramic powders, and should serve as precursors to matrix fibers. In recent years, a number of polysilanes and polysilezanes were investigated as potential presursors. A review of candidate polymers is presented, including recent studies of silsesquioxanes.

Hurwitz, Frances I.↗

Processing and Characterization of Basalt Fiber Reinforced Ceramic Composites for High Temperature Applications Using Polymer Precursors

The development of high temperature structural composite materials has been very limited due to the high cost of the materials and the processing needed. Ceramics can take much higher temperatures, but they are difficult to produce and form in bulk volumes. Polymer Derived Ceramics (PDCs) begin as a polymer matrix, allowing a shape to be formed, to be cured, and be pyrolized in order to obtain a ceramic with the associated thermal and mechanical properties. The two PDCs used in this development are polysiloxane and polycarbosilane. Polysiloxanes contain a silicon oxycarbide backbone when pyrolized up to 1000degC. Polycarbosilane, an organosilicon polymer, contain a silicon-carbon backbone; around 1200degC, -SiC begins to crystallize. The use of basalt in structural and high temperature applications has been under development for over 50 years, yet there has been little published research on the incorporation of basalt fibers as a reinforcement in composites. Basalt is a naturally occurring material found in volcanic rock. Continuous basalt fiber reinforced PDCs have been fabricated and tested for the applicability of this composite system as a high temperature structural composite material. Testing for this included thermal and mechanical testing per ASTM standard tests.

High Temperature Composites↗

Processing and Characterization of Basalt Fiber Reinforced Ceramic Composites for High Temperature Applications Using Polymer Precursors

The development of high temperature structural composite materials has been very limited due to the high cost of the materials and the processing needed. Ceramics can take much higher temperatures, but they are difficult to produce and form in bulk volumes. Polymer Derived Ceramics (PDCs) begin as a polymer matrix, allowing a shape to be formed and cured and then to be pyrolized in order to obtain a ceramic with the associated thermal and mechanical properties. The two PDCs used in this development are polysiloxane and polycarbosilane. Polysiloxanes contain a silicon oxycarbide backbone when pyrolized up to 1000C. Polycarbosilane, an organosilicon polymer, contain a silicon-carbon backbone; around 1200C, beta-SiC begins to crystallize. The use of basalt in structural and high temperature applications has been under development for over 50 years, yet there has been little published research on the incorporation of basalt fibers as a reinforcement in composites. Basalt is a naturally occurring material found in volcanic rock. Continuous basalt fiber reinforced PDCs have been fabricated and tested for the applicability of this composite system as a high temperature structural composite material. Thermal and mechanical testing includes oxyacetylene torch testing and three point bend testing.

Ceramic Matrix Composites↗

Processing and Characterization of Basalt Fiber Reinforced Ceramic Composites for High Temperature Applications Using Polymer Precursors

The development of high temperature structural composite materials has been very limited due to the high cost of the materials and the processing needed. Ceramics can take much higher temperatures, but they are difficult to produce and form in bulk volumes. Polymer Derived Ceramics (PDCs) begin as a polymer matrix, allowing a shape to be formed and cured and then to be pyrolized in order to obtain a ceramic with the associated thermal and mechanical properties. The two PDCs used in this development are polysiloxane and polycarbosilane. Polysiloxanes contain a silicon oxycarbide backbone when pyrolized up to 1000 deg C. Polycarbosilane, an organosilicon polymer, contain a silicon-carbon backbone; around 1200 deg C, Beta-SiC begins to crystallize. The use of basalt in structural and high temperature applications has been under development for over 50 years, yet there has been little published research on the incorporation of basalt fibers as a reinforcement in composites. Basalt is a naturally occurring material found in volcanic rock. Continuous basalt fiber reinforced PDCs have been fabricated and tested for the applicability of this composite system as a high temperature structural composite material. Thermal and mechanical testing includes oxyacetylene torch testing and three point bend testing.

Polymer Derived Ceramics↗

Monolithic Trace-Contaminant Sorbents Fabricated from 3D-Printed Polymer Precursors

The current trace-contaminant (TC) removal technology for use in Extravehicular Activities (EVAs) involves the use of a packed bed of acid-impregnated granular charcoal, which is difficult to regenerate. In this paper, results are presented on the development of vacuum-regenerable TC sorbents for use in the Portable Life Support System (PLSS). The sorbents are derived from 3D-printed polymer monoliths (e.g., honeycomb structures), which are then carbonized and activated in order to develop porosity, and also to enhance the TC-sorption capacity. Results are presented on the following aspects of carbon-sorbent development: (1) precursor selection; (2) monolith fabrication; (3) shape retention and strength; (4) carbon surface and porosity characterization; (5) TC-sorption capacity and vacuum-regeneration; (6) pressure drop; and (7) sub-scale sorbent prototype. The use of predominantly microporous monolithic carbon is associated with the following benefits: (a) high TC-sorption capacity; (b) low pressure drop; (c) rapid vacuum (pressure-swing) desorption due to thin monolith walls and low pressure drop; (d) good thermal management (high thermal conductivity and low adsorption/desorption thermal effects associated with physisorption); and (e) good resistance to dusty environments.

Portable Life Support System (PLSS)↗

Organoborosilane Polymers And Ceramic Products

Process developed to make polyorganoborosilane polymers. Precursor polymers prepared by using alkali metal to couple boron halide with organohalosilane. In representative application, polymer drawn into fibers, then pyrolyzed to produce ceramic cloth. Ceramics exhibit high thermo-oxidative stability.

Riccitiello, Salvatore R.↗

Ceramic silicon-boron-carbon fibers from organic silicon-boron-polymers

Novel high strength ceramic fibers derived from boron, silicon, and carbon organic precursor polymers are discussed. The ceramic fibers are thermally stable up to and beyond 1200 C in air. The method of preparation of the boron-silicon-carbon fibers from a low oxygen content organosilicon boron precursor polymer of the general formula Si(R2)BR(sup 1) includes melt-spinning, crosslinking, and pyrolysis. Specifically, the crosslinked (or cured) precursor organic polymer fibers do not melt or deform during pyrolysis to form the silicon-boron-carbon ceramic fiber. These novel silicon-boron-carbon ceramic fibers are useful in high temperature applications because they retain tensile and other properties up to 1200 C, from 1200 to 1300 C, and in some cases higher than 1300 C.

Riccitiello, Salvatore R.↗

Surface modified aerogel monoliths

This invention comprises reinforced aerogel monoliths such as silica aerogels having a polymer coating on its outer geometric surface boundary, and to the method of preparing said aerogel monoliths. The polymer coatings on the aerogel monoliths are derived from polymer precursors selected from the group consisting of isocyanates as a precursor, precursors of epoxies, and precursors of polyimides. The coated aerogel monoliths can be modified further by encapsulating the aerogel with the polymer precursor reinforced with fibers such as carbon or glass fibers to obtain mechanically reinforced composite encapsulated aerogel monoliths.

Leventis, Nicholas↗

Method of Cross-Linking Aerogels Using a One-Pot Reaction Scheme

A document discusses a new, simplified method for cross-linking silica and other oxide aerogels, with a polymeric material to increase strength of such materials without adversely affecting porosity or low density. This innovation introduces the polymer precursor into the sol before gelation either as an agent, which co-reacts with the oxide gel, or as soluble polymer precursors, which do not interact with the oxide gel in any way. Subsequent exposure to heat, light, catalyst or other method of promoting polymerization causes cross-linking without any additional infiltration steps.

Meador, Ann B.↗

Forcespun Polymers as Precursors to Boron Nitride Fibers

The need for multifunctional materials in aerospace technologies is currently driving the development of new novel composite materials. Specifically, insulation materials with high thermal conductivity, high electrical resistivity, and are chemically inert are needed for high voltage power applications. Boron nitride (BN) nanomaterials fit these criteria and can be incorporated into composites for further material design. The synthesis of boron nitride through a polymer derived ceramic route allows for the morphology of the resulting BN to be tailored. This is especially beneficial since the polymers can be shaped or spun into fibers prior to the ceramic conversion. This project utilizes the Forcespinning technique to produce boron-containing polymer fibers that are converted to boron nitride through a heat treatment. The chemical compositions and fiber morphologies were studied and reported here.

Boron nitride, Fibers, Forcespinning↗

Self-Assembling, Flexible, Pre-Ceramic Composite Preforms

In this innovation, light weight, high temperature, compact aerospace structures with increased design options are made possible by using self-assembling, flexible, pre-ceramic composite materials. These materials are comprised of either ceramic or carbon fiber performs, which are infiltrated with polymer precursors that convert to ceramics upon thermal exposure. The preform architecture can vary from chopped fibers formed into blankets or felt, to continuous fibers formed into a variety of 2D or 3D weaves or braids. The matrix material can also vary considerably. For demonstration purposes, a 2D carbon weave was infiltrated with a SiC polymer precursor. The green or unfired material is fabricated into its final shape while it is still pliable. It is then folded or rolled into a much more compact shape, which will occupy a smaller space. With this approach, the part remains as one continuous piece, rather than being fabricated as multiple sections, which would require numerous seals for eventual component use. The infiltrated preform can then be deployed in-situ. The component can be assembled into its final shape by taking advantage of the elasticity of the material, which permits the structure to unfold and spring into its final form under its own stored energy. The pre-ceramic composites are converted to ceramics and rigidized immediately after deployment. The final ceramic composite yields a high-temperature, high-strength material suitable for a variety of aerospace structures. The flexibility of the material, combined with its high-temperature structural capacity after rigidization, leads to a less complex component design with an increased temperature range. The collapsibility of these structures allows for larger components to be designed and used, and also offers the potential for increased vehicle performance. For the case of collapsible nozzle extensions, a larger nozzle, and thus a larger nozzle exit plane, is possible because interference with surrounding structures can be avoided in the collapsed state. The larger exit plane leads to an increase in expansion area ratio, which has the potential to increase thrust and overall rocket performance. In general, the use of advanced ceramic materials can lead to improved engine and vehicle performance. The ceramics can run hotter, so less cooling is required. Fuel to coolant ratios can be balanced more readily to reduce weight. Engine efficiency can also be increased with hotter combustion and exhaust temperatures. In addition, the ceramic composites themselves can reduce the component weight by as much as 50 percent, which can translate into greater payload for the vehicle

Jaskowiak, Martha H.↗

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.↗