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Hsu, Ming-Ta S.

Publications and source records attributed to Hsu, Ming-Ta S..

Light-weight black ceramic insulation

Ultra-high temperature, light-weight, black ceramic insulation having a density ranging from about 0.12 g/cc. to 0.6 g/cc. such as ceramic tile is obtained by pyrolyzing siloxane gels derived from the reaction of at least one organo dialkoxy silane and at least one tetralkoxy silane in an acid or base liquid medium. The reaction mixture of the tetra- and dialkoxy silanes also may contain an effective amount of a mono- or trialkoxy silane to obtain the siloxane gels. The siloxane gels are dried at ambient temperatures and pressures to form siloxane ceramic precursors without significant shrinkage. The siloxane ceramic precursors are subsequently pyrolyzed, in an inert atmosphere, to form the black ceramic insulation comprising atoms of silicon, carbon and oxygen. The ceramic insulation can be characterized as a porous, uniform ceramic tile resistant to oxidation at temperatures ranging as high as 1700.degree. C., and particularly useful as lightweight tiles for spacecraft and other high-temperature insulation applications.

Hsu, Ming-Ta S.

Simplified Waterproofing of Aerogels

A relatively simple silanization process has been developed for waterproofing or rewaterproofing aerogels, xerogels, and aerogel/tile composites, and other, similar low-density, highly microporous materials. Such materials are potentially attractive for a variety of applications especially for thermal-insulation panels that are required to be thin and lightweight. Unfortunately, such materials are also hydrophilic and tend to collapse after adsorbing water from the air. Hence, an effective means of waterproofing is necessary to enable practical exploitation of aerogels and the like. Older processes for waterproofing aerogels are time-consuming, labor-intensive, and expensive, relative to the present process. Each of the older processes includes a number of different chemical treatment steps, and some include the use of toxic halogenated surface-modifying compounds, pressures as high as hundreds of atmospheres, and/or temperatures as high as 1,000 C.

Hsu, Ming-Ta S.

Light-weight ceramic insulation

Ultra-high temperature, light-weight, ceramic insulation such as ceramic tile is obtained by pyrolyzing a siloxane gel derived from the reaction of at least one organo dialkoxy silane and at least one tetralkoxy silane in an acid or base liquid medium. The reaction mixture of the tetra- and dialkoxy silanes may contain also an effective amount of a mono- or trialkoxy silane to obtain the siloxane gel. The siloxane gel is dried at ambient pressures to form a siloxane ceramic precursor without significant shrinkage. The siloxane ceramic precursor is subsequently pyrolyzed, in an inert atmosphere, to form the black ceramic insulation comprising atoms of silicon, carbon and oxygen. The ceramic insulation, can be characterized as a porous, uniform ceramic tile resistant to oxidation at temperatures ranging as high as 1700.degree. C. and is particularly useful as lightweight tiles for spacecraft and other high-temperature insulation applications.

Hsu, Ming-Ta S.

Refractory Oxidative-Resistant Ceramic Carbon Insulation

High-temperature, lightweight, ceramic carbon insulation is prepared by coating or impregnating a porous carbon substrate with a siloxane gel derived from the reaction of an organodialkoxy silane and an organotrialkoxy silane in an acid or base medium in the presence of the carbon substrate. The siloxane gel is subsequently dried on the carbon substrate to form a ceramic carbon precursor. The carbon precursor is pyrolyzed, in an inert atmosphere, to form the ceramic insulation containing carbon, silicon, and oxygen. The carbon insulation is characterized as a porous, fibrous, carbon ceramic tile which is particularly useful as lightweight tiles for spacecraft.

Leiser, Daniel B.

High Temperature Resistant Organopolysiloxane Coating for Protecting and Repairing Rigid Thermal Insulation

Ceramics are protected from high temperature degradation, including high temperature, oxidative, aeroconvective degradation by a high temperature and oxidation resistant coating of a room temperature curing, hydrolyzed and partially condensed liquid polyorganosiloxane to the surface of the ceramic. The liquid polyorganosiloxane is formed by the hydrolysis and partial condensation of an alkyltrialkoxysilane with water or a mixture of an alkyltrialkoxysilane and a dialkyldialkoxysilane with water. The liquid polyorganosiloxane cures at room temperature on the surface of the ceramic to form a hard, protective, solid coating which forms a high temperature environment, and is also used as an adhesive for adhering a repair plug in major damage to the ceramic. This has been found useful for protecting and repairing porous, rigid ceramics of a type used on reentry space vehicles.

Leiser, Daniel B.

Method for Waterproofing Ceramic Materials

Hygroscopic ceramic materials which are difficult to waterproof with a silane, substituted silane or silazane waterproofing agent, such as an alumina containing fibrous, flexible and porous, fibrous ceramic insulation used on a reentry space vehicle, are rendered easy to waterproof if the interior porous surface of the ceramic is first coated with a thin coating of silica. The silica coating is achieved by coating the interior surface of the ceramic with a silica precursor converting the precursor to silica either in-situ or by oxidative pyrolysis and then applying the waterproofing agent to the silica coated ceramic. The silica precursor comprises almost any suitable silicon containing material such as a silane, silicone, siloxane, silazane and the like applied by solution, vapor deposition and the like. If the waterproofing is removed by e.g., burning, the silica remains and the ceramic is easily rewaterproofed. An alumina containing TABI insulation which absorbs more that five times its weight of water, absorbs less than 10 wt. % water after being waterproofed according to the method of the invention.

Cagliostro, Domenick E.

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.

Boron-carbon-silicon polymers and the ceramic thereof

The present invention relates to a process for the production of an organoborosilicon preceramic polymer. The prepolymer is pyrolyzed to produce a ceramic article useful in high temperature (e.g., aerospace) or extreme environmental applications.

Riccitiello, Salvatore R.

Boron-containing organosilane polymers and ceramic materials thereof

The present invention relates to a polyorgano borosilane ceramic precursor polymer comprising a plurality of repeating units of the formula: (R(sup 1) single bond B)(sub p) being linked together at B by second units of the formula: single bond (R sup 2) single bond (Si single bond R sup 3) single bond (sub q), where R(sup 1) is a lower alkyl, cycloalkyl, phenyl, or (R(sup 2)R(sup 3) single bond Si single bond B single bond)(sub n) and R(sup 2) and R(sup 3) are each independently selected from hydrogen, lower alkyl, vinyl, cycloalkyl, or aryl, n is an integer between 1 and 100; p is an integer between 1 and 100; and q is an integer between 1 and 100. These materials are prepared by combining an organo borohalide of the formula R(sup 4) single bond B single bond (X sup 1) (sub 2) where R(sup 4) is selected from halogen, lower alkyl, cycloalkyl, or aryl, and an organo halosilane of the formula: R(sup 2)(R sup 3)Si(X sup 2)(sub 2) where R(sup 2) and R (sup 3) are each independently selected from lower alkyl, cycloalkyl, or aryl, and X(sup 1) and X(sup 2) are each independently selected from halogen, in an anhydrous aprotic solvent having a boiling point at ambient pressure of not greater than 160 C with in excess of four equivalents of an alkali metal, heating the reaction mixture and recovering the polyorgano borosilane. These silicon boron polymers are useful to generate high-temperature ceramic materials, such as SiC, SiB4, and B4C, upon thermal degradation above 600 C.

Riccitiello, Salvatore R.

Composites of vinyl polystyrylpyridine/bismaleimide-aliphatic ether copolymers

An aliphatic ether bismaleimide was prepared and coreacted with a polyvinylstyrylpyridine (VPSP) oligomer. Studies showed that a controlled ratio of aliphatic to aromatic units in the polymer backbone improved both processibility and interlaminar shear properties for the carbon-fiber composite system. This modified resin was readily soluble in tetrahydrofuran, allowing for better fiber impregnation and thus enhancing adhesive properties and reproducibility. DSC studies have shown a lower cure temperature for the copolymer than for the neat aliphatic bismaleimide, and a glass transition temperature of 260 C, which is more than adequate for most applications. Limited measurements indicated an improvement in toughness (impact resistance).

Heimbuch, Alvin H.

Boron-containing organosilane polymers and ceramic materials thereof

The present invention relates to organic silicon-boron polymers which upon pyrolysis produce high-temperature ceramic materials. More particularly, it relates to the polyorganoborosilanes containing -Si-B- bonds which generate high-temperature ceramic materials (e.g., SiC, SiB4, B4C) upon thermal degradation. The process for preparing these organic silicon-boron polymer precursors are also part of the invention.

Riccitiello, Salvatore R.

Synthesis Of B, B', B"-Trichloroborazine

Simplified, relatively safe, and economical synthesis of B, B', B"-trichloroborazine easily practiced in standard organic-chemistry laboratory. Yield is 20 to 30 percent, fairly acceptable value in view of inherent difficulty of synthesizing borazines. New synthesis has potential use in industry.

Riccitiello, Salvatore R.

Bismaleimide Copolymer Matrix Resins

Graphite composites, prepared from 1:1 copolymer of two new bismaleimides based on N,N'-m-phenylene-bis(m-amino-benzamide) structure have mechanical properties superior to those prepared from other bismaleimide-type resins. New heat-resistant composites replace metal in some structural applications. Monomers used to form copolymers with superior mechanical properties prepared by reaction of MMAB with maleic or citraconic anhydride.

Parker, John A.

Preparation of B-trichloroborazine

The present invention relates to a method of preparing B-trichloroborazine. Generally, the method includes the combination of gaseous boron trichloride in an anhydrous aprotic organic solvent followed by addition of excess gaseous ammonia at ambient temperature or below. The reaction mixture is heated to about 100 to 140 C followed by cooling, removal of the solid ammonium chloride at ambient temperature, distillation of the solvent under vacuum if necessary at a temperature of up to about 112 C, and recovery of the B-trichloroborazine. Solvents include toluene, benzene, xylene, chlorinated hydrocarbons, chlorinated aromatic compounds, or mixtures thereof. Toluene is a preferred solvent. The process provides a convenient synthesis of a material which often decomposes on standing. B-trichloroborazine is useful in a number of chemical reactions, and particularly in the formation of high temperature inorganic polymers and polymer precursors.

Riccitiello, Salvatore R.

Structural panels

Vinyl pyridines including vinyl stilbazole materials and vinyl styrylpyridine oligomer materials are disclosed. These vinylpyridines form copolymers with bismaleimides which copolymers have good fire retardancy and decreased brittleness. The cure temperatures of the copolymers are substantially below the cure temperatures of the bismaleimides alone. Reinforced composites made from the cured copolymers are disclosed as well.

Parker, John A.

Vinyl stilbazoles

Vinyl pyridines including vinyl stilbazole materials and vinyl styrylpyridine oligomer materials are disclosed. These vinylpyridines form copolymers with bismaleimides which copolymers have good fire retardancy and decreased brittleness. The cure temperatures of the copolymers are substantially below the cure temperatures of the bismaleimides alone. Reinforced composites made from the cured copolymers are disclosed as well.

Parker, John A.