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    • 2. 发明授权
    • Light-weight ceramic insulation
    • 陶瓷绝缘重量轻
    • US06339034B1
    • 2002-01-15
    • US09490677
    • 2000-01-24
    • Ming-Ta S. HsuTimothy S. Chen
    • Ming-Ta S. HsuTimothy S. Chen
    • C04B3514
    • C04B38/0045C04B2111/00982C04B35/565C04B35/56
    • 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° C. and is particularly useful as lightweight tiles for spacecraft and other high-temperature insulation applications.
    • 通过在酸性或液体介质中热解由至少一种有机二烷氧基硅烷与至少一种四氢化烷氧基硅烷的反应产生的硅氧烷凝胶来获得超高温,轻质陶瓷绝缘体。 四烷氧基硅烷和二烷氧基硅烷的反应混合物还可以含有有效量的单烷氧基硅烷或三烷氧基硅烷以获得硅氧烷凝胶。 将硅氧烷凝胶在环境压力下干燥以形成硅氧烷陶瓷前体而不显着收缩。 硅氧烷陶瓷前体随后在惰性气氛中热解,形成包含硅,碳和氧原子的黑色陶瓷绝缘体。 陶瓷绝缘体可以表征为多孔均匀的瓷砖,耐高温至1700℃的氧化作用,特别适用于航天器和其他高温绝缘应用的轻质瓦片。
    • 4. 发明授权
    • Boron-carbon-silicon polymers and the ceramic thereof
    • 硼 - 碳 - 硅聚合物及其陶瓷
    • US4987201A
    • 1991-01-22
    • US361471
    • 1989-06-05
    • Salvatore R. RiccitielloMing-ta S. HsuTimothy S. Chen
    • Salvatore R. RiccitielloMing-ta S. HsuTimothy S. Chen
    • C04B35/571C08G77/60C08G79/08
    • C08G77/60C04B35/571C08G79/08
    • The present invention relates to a process for the production of an organoborosilicon preceramic polymer of the structure: ##STR1## wherein R.sup.1 is selected from alkyl having from 1 to 10 carbon atoms or phenyl, and x is selected from 0, 1, 2 or 3;which is pyrolyzable to produce a refractory material comprising inorganic compounds of Si, C and B, which process comprises:contacting a silicon containing compound of the structure:(R.sup.1).sub.x --Si (CH.dbd.CH.sub.2).sub.4-x or (R.sup.1).sub.x Si(C.dbd.CH).sub.4-x with a boron containing compound selected from H.sub.3 B:BH.sub.3, H.sub.3 B:NH.sub.3, BH.sub.3 :N(R.sup.2).sub.3 wherein R.sup.2 is selected from methyl, ethyl, propyl, butyl or phenyl in an inert atmosphere at a temperature of between about 90.degree. and 170.degree. C. for between about 0.1 and 20 hr and recovering the prepolymer. The prepolymer is pyrolyzed to produce a ceramic article useful in high temperature (e.g., aerospace) or extreme environmental applications.
    • 本发明涉及一种制备有机硼硅前驱体聚合物的方法,其结构如下:其中R 1选自具有1至10个碳原子的烷基或苯基,x选自0,1或2, 2或3; 其可热解以制备包含Si,C和B的无机化合物的耐火材料,该方法包括:将以下结构的含硅化合物:(R1)x-Si(CH = CH2)4-x或(R1)x Si(C = CH)4-x与选自H 3 B:BH 3,H 3 B:NH 3,BH 3 :N(R 2)3的含硼化合物在惰性气氛中,其中R2选自甲基,乙基,丙基,丁基或苯基 温度在约90℃至170℃之间约0.1至20小时,并回收预聚物。 预聚物被热解以产生在高温(例如航空航天)或极端环境应用中有用的陶瓷制品。
    • 5. 发明授权
    • Boron-containing organosilane polymers and ceramic materials thereof
    • 含硼的有机硅烷聚合物及其陶瓷材料
    • US4851491A
    • 1989-07-25
    • US231027
    • 1988-08-11
    • Salvatore R. RiccitielloMing-Ta S. HsuTimothy S. Chen
    • Salvatore R. RiccitielloMing-Ta S. HsuTimothy S. Chen
    • C04B35/571C04B35/622C08G77/60
    • C08G77/60C04B35/571C04B35/62227
    • The present invention relates to a polyorganoborosilane ceramic precursor polymer comprising a plurality of repeating units of the formula: ##STR1## with the segments being linked together by second units of the formula: --[(R.sup.2)--Si--R.sup.3)--q, where R.sup.1 is lower alkyl, cycloalkyl, phenyl, or ##STR2## 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 organoborohalide of the formula R.sup.4 --B--(X.sup.1).sub.2 where R.sup.4 is selected from halogen, lower alkyl, cycloalkyl, or aryl, and an organohalosilane 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.degree. C. with in excess of four equivalents of an alkali metal, heating the reaction mixture and recovering the polyorganoborosilane. These silicon boron polymers are useful to generate high-temperature ceramic materials, such as SiC, SiB.sub.4, and B.sub.4 C, upon thermal degradation above 600.degree. C.
    • 本发明涉及一种聚有机硼硅烷陶瓷前体聚合物,其包含多个下式的重复单元:其中链段由下式的第二单元连接在一起: - [(R2)-Si-R3)-q,其中 R 1是低级烷基,环烷基,苯基或者R 3,R 2和R 3各自独立地选自氢,低级烷基,乙烯基,环烷基或芳基,n是1和100之间的整数; p是1到100之间的整数; q是1和100之间的整数。这些材料是通过将式R4-B-(X1)2的有机溴卤化物(其中R 4选自卤素,低级烷基,环烷基或芳基)和有机卤代硅烷 :R2(R3)Si(X2)2其中R2和R3各自独立地选自低级烷基,环烷基或芳基,X1和X2各自独立地选自卤素,在无水非质子溶剂中,其沸点在环境压力 不大于160℃,超过4当量碱金属,加热反应混合物并回收聚有机硼硅烷。 当在600℃以上的热降解时,这些硅硼聚合物可用于生成高温陶瓷材料,例如SiC,SiB4和B4C。
    • 6. 发明授权
    • High temperature resistant organopolysiloxane coating for protecting and
repairing rigid thermal insulation
    • 耐高温有机聚硅氧烷涂层,用于保护和修复刚性绝热
    • US5985433A
    • 1999-11-16
    • US823665
    • 1997-03-13
    • Daniel B. LeiserMing-ta S. HsuTimothy S. Chen
    • Daniel B. LeiserMing-ta S. HsuTimothy S. Chen
    • B32B18/00B32B3/26
    • B32B18/00Y10T428/249956Y10T428/249969Y10T428/249988Y10T428/24999Y10T428/31663
    • Ceramics are or 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 applied 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, oxidation resistant ceramic upon exposure to 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.
    • 陶瓷被保护或防止高温降解,包括通过施加到陶瓷表面的室温固化,水解和部分冷凝的液体聚有机硅氧烷的高温和抗氧化涂层的高温,氧化,飞行性降解。 液体聚有机硅氧烷是通过烷基三烷氧基硅烷与水或烷基三烷氧基硅烷和二烷基二烷氧基硅烷的混合物与水的水解和部分缩合形成的。 液体聚有机硅氧烷在室温下固化在陶瓷的表面上,形成硬的保护性固体涂层,其在暴露于高温环境下形成耐高温,耐氧化的陶瓷,并且还用作用于粘合修复的粘合剂 对陶瓷造成重大损害。 已经发现这对于保护和修复用于再入式太空车辆的类型的多孔刚性陶瓷是有用的。
    • 8. 发明授权
    • Boron-containing organosilane polymers and ceramic materials thereof
    • 含硼的有机硅烷聚合物及其陶瓷材料
    • US4767728A
    • 1988-08-30
    • US890577
    • 1986-07-30
    • Salvatore R. RiccitielloMing-Ta S. HsuTimothy S. Chen
    • Salvatore R. RiccitielloMing-Ta S. HsuTimothy S. Chen
    • C04B35/571C04B35/58C04B35/622C08G77/48C08G77/60C04B35/56
    • C08G77/60C04B35/571C04B35/62227
    • The present invention relates to a polyorganoborosilane ceramic precursor polymer comprising a plurality of repeating units of the formula: ##STR1## with the segments being linked together by second units of the formula: --(R.sup.2)--Si--R.sup.3)--q, where R.sup.1 is lower alkyl, cycloalkyl, phenyl, or ##STR2## 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 organoborohalide of the formula R.sup.4 -B-(X.sup.1).sub.2 where R.sup.4 is selected from halogen, lower alkyl, cycloalkyl, or aryl, and an organohalosilane 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.degree. C. with in excess of four equivalents of an alkali metal, heating the reaction mixture and recovering the polyorganoborosilane. These silicon boron polymers are useful to generate high-temperature ceramic materials, such as SiC, SiB.sub.4, and B.sub.4 C, upon thermal degradation above 600.degree. C.
    • 本发明涉及一种聚有机硼硅烷陶瓷前体聚合物,其包含多个下列重复单元:其中该链段由下式的第二单元连接在一起: - (R2)-Si-R3)-q,其中R1 是低级烷基,环烷基,苯基或者R 3,R 2和R 3各自独立地选自氢,低级烷基,乙烯基,环烷基或芳基,n是1和100之间的整数; p是1到100之间的整数; q是1和100之间的整数。这些材料是通过将式R4-B-(X1)2的有机溴卤化物(其中R 4选自卤素,低级烷基,环烷基或芳基)和有机卤代硅烷 :R2(R3)Si(X2)2其中R2和R3各自独立地选自低级烷基,环烷基或芳基,X1和X2各自独立地选自卤素,在无水非质子溶剂中,其沸点在环境压力 不大于160℃,超过4当量碱金属,加热反应混合物并回收聚有机硼硅烷。 当在600℃以上的热降解时,这些硅硼聚合物可用于生成高温陶瓷材料,例如SiC,SiB4和B4C。