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    Glycol-based method for forming a thin-film nanoporous dielectric
    42.
    发明授权
    Glycol-based method for forming a thin-film nanoporous dielectric 失效
    用于形成薄膜纳米多孔电介质的基于乙二醇的方法

    公开(公告)号：US5736425A

    公开(公告)日：1998-04-07

    申请号：US748925

    申请日：1996-11-14

    Applicant: Douglas M. Smith ,  William C. Ackerman

    Inventor： Douglas M. Smith ,  William C. Ackerman

    IPC: B01J13/00 ,  C01B33/158 ,  C03C1/00 ,  C03C17/25 ,  H01L21/314 ,  H01L21/316 ,  H01L21/00

    CPC classification number: H01L21/02126 ,  B01J13/0091 ,  C01B33/1585 ,  C03C1/008 ,  C03C17/25 ,  H01L21/02203 ,  H01L21/02216 ,  H01L21/02282 ,  H01L21/02337 ,  H01L21/31695 ,  C03C2217/213 ,  C03C2218/113

    Abstract: This invention has enabled a new, simple nanoporous dielectric fabrication method. In general, this invention uses a glycol, such as ethylene glycol, as a solvent. This new method allows both bulk and thin film aerogels to be made without supercritical drying, freeze drying, or a surface modification step before drying. Prior art aerogels have required at least one of these steps to prevent substantial pore collapse during drying. Thus, this invention allows production of nanoporous dielectrics at room temperature and atmospheric pressure, without a separate surface modification step. Although not required to prevent substantial densification, this new method does not exclude the use of supercritical drying or surface modification steps prior to drying. In general, this new method is compatible with most prior art aerogel techniques. Although this new method allows fabrication of aerogels without substantial pore collapse during drying, there may be some permanent shrinkage during aging and/or drying.

    Abstract translation: 本发明已经实现了一种新的简单的纳米多孔电介质制造方法。 通常，本发明使用乙二醇如乙二醇作为溶剂。 这种新方法允许在超临界干燥，冷冻干燥或干燥前的表面改性步骤中制造体积和薄膜气凝胶。 现有技术的气凝胶需要这些步骤中的至少一个来防止在干燥期间大量的孔隙破裂。 因此，本发明允许在室温和大气压下制备纳米多孔电介质，而无需单独的表面改性步骤。 尽管不需要防止实质致密化，但是这种新方法并不排除在干燥之前使用超临界干燥或表面改性步骤。 通常，这种新方法与大多数现有技术的气凝胶技术相兼容。 虽然这种新方法允许在干燥期间制造气凝胶而没有实质的孔隙塌陷，但在老化和/或干燥期间可能存在一些永久收缩。

    Sol gel barrier films
    43.
    发明授权
    Sol gel barrier films 失效
    溶胶凝胶屏障膜

    公开(公告)号：US5618628A

    公开(公告)日：1997-04-08

    申请号：US594080

    申请日：1996-01-30

    Applicant: Raymond A. Volpe

    Inventor： Raymond A. Volpe

    IPC: C03C1/00 ,  C08G77/02 ,  C09D183/02 ,  B01J13/00

    CPC classification number: C03C1/008 ,  C08G77/02 ,  C09D183/02

    Abstract: A relaxed sol-gel composition and a coated substrate article which is produced therefrom. A tetrafunctional alkoxide silicate is hydrolyzed in an aqueous solution together with a Lewis acid or metal chelate catalyst with optional protic acid until a viscosity of 2600-3200 cps is obtained to form a crosslinked sol-gel polymer composition. The polymer is relaxed by diluting it with water or water plus alcohol optionally containing a Lewis acid or metal chelate until a viscosity of about 1 cps is obtained while not depolymerizing the polymer. The relaxed polymer has substantially no visible polymer particles. The relaxed polymer composition is uniformly coating a substrate and dried without requiring an in-situ curing.

    Abstract translation: 松散的溶胶 - 凝胶组合物和由其制备的涂布的基底制品。 四官能醇盐硅酸盐在水溶液中与路易斯酸或金属螯合催化剂与任选的质子酸一起水解，直到获得2600-3200cps的粘度以形成交联的溶胶 - 凝胶聚合物组合物。 通过用水或水加醇任选地含有路易斯酸或金属螯合物来使聚合物松弛，直到达到约1cps的粘度，同时不解聚聚合物。 松散的聚合物基本上没有可见的聚合物颗粒。 松散的聚合物组合物均匀地涂覆基材并干燥而不需要原位固化。

    Ceramic composite coating
    44.
    发明授权
    Ceramic composite coating 失效
    陶瓷复合涂层

    公开(公告)号：US5595945A

    公开(公告)日：1997-01-21

    申请号：US796974

    申请日：1991-11-25

    Applicant: George G. Wicks

    Inventor： George G. Wicks

    IPC: C03C1/00 ,  C03C14/00 ,  C04B41/50 ,  C23C26/00 ,  C04C35/14

    CPC classification number: C23C26/00 ,  C03C1/008 ,  C03C14/002 ,  C03C14/004 ,  C04B41/5089 ,  C03C2214/32

    Abstract: A thin, room-temperature-curing, ceramic composite for coating and patchingetal substrates comprises a sol gel silica glass matrix filled with finely ground particles or fibers, preferably alumina. The sol gel glass is made by adding ethanol to water to form a first mixture, then separately adding ethanol to tetraethyl orthosilicate to form a second mixture, then slowly adding the first to the second mixture to make a third mixture, and making a slurry by adding the finely ground particles or fibers to the third mixture. The composite can be applied by spraying, brushing or trowelling. If applied to patch fine cracks, densification of the ceramic composite may be obtained to enhance sealing by applying heat during curing.

    Abstract translation: 用于涂覆和修补金属基材的薄的室温固化陶瓷复合材料包括填充有精细研磨的颗粒或纤维，优选氧化铝的溶胶凝胶石英玻璃基质。 溶胶凝胶玻璃是通过向水中加入乙醇形成第一混合物，然后分别将乙醇加入原硅酸四乙酯中形成第二混合物，然后缓慢加入第二混合物制成第三混合物，并通过 将细磨的颗粒或纤维加入到第三混合物中。 复合材料可以通过喷涂，刷涂或抹光涂抹。 如果应用于修补细裂纹，则可以获得陶瓷复合材料的致密化，以通过在固化期间施加热量来增强密封性。

    Process for photoinitiated control of inorganic network formation in the sol-gel process
    45.
    发明授权
    Process for photoinitiated control of inorganic network formation in the sol-gel process 失效
    溶胶 - 凝胶法中无机网络形成的光引发控制方法

    公开(公告)号：US5360834A

    公开(公告)日：1994-11-01

    申请号：US188746

    申请日：1994-01-31

    Applicant: Michael Popall ,  Jochen Schulz ,  Helmut Schmidt

    Inventor： Michael Popall ,  Jochen Schulz ,  Helmut Schmidt

    IPC: B01J13/00 ,  B01J19/12 ,  C03C1/00 ,  C03C17/02 ,  C03C17/25 ,  C08G4/00 ,  C08G77/02 ,  C08J3/28 ,  C08K3/18

    CPC classification number: B01J13/0039 ,  B01J19/123 ,  C03C1/008 ,  C03C17/02 ,  C03C17/25

    Abstract: A process is described for photoinitiated control of inorganic network fotion in the sol-gel process, which comprises eitherA) subjecting one or more hydrolytically polycondensable compounds of constituent elements of glass or ceramic, excluding silicon compounds containing polymerizable organic groups, to hydrolytic polycondensation in a liquid reaction medium to form a sol and irradiating the resulting sol in a structured or unstructured manner in the presence of a photoinitiator which can change the pH of the reaction medium on irradiation, using radiation of a wavelength range in which the photoinitiator absorbs;orB) liberating water in an anhydrous reaction medium which contains an alcohol, one or more hydrolytically polycondensable compounds of constituent elements of glass or ceramic and a photoinitiator which can liberate water by a photochemical reaction or a secondary reaction when irradiated, by structured or non-structured irradiation using radiation of a wavelength range in which the photoinitiator absorbs, and in this way effecting the hydrolytic polycondensation.

    Abstract translation: 描述了在溶胶 - 凝胶法中对无机网络形成进行光引发控制的方法，其包括A）将除了含有可聚合有机基团的硅化合物之外的玻璃或陶瓷的一种或多种水解可缩聚化合物的化合物水解缩聚 液体反应介质以形成溶胶，并且在光引发剂存在下以结构或非结构化方式照射所得溶胶，所述光引发剂可使用光引发剂吸收的波长范围的辐射在照射时改变反应介质的pH值; 或B）在含有醇，一种或多种水解可缩聚的玻璃或陶瓷组成元素的化合物和光引发剂的无水反应介质中释放水，其可以通过结构化或非结构化的光化学反应或二次反应释放水 使用光引发剂吸收的波长范围的辐射的结构化照射，并且以这种方式进行水解缩聚。

    Use of hydrogen peroxide in preparing magnesium containing silicate sols for coating and fiber formation
    47.
    发明授权
    Use of hydrogen peroxide in preparing magnesium containing silicate sols for coating and fiber formation 失效
    使用过氧化氢制备含镁硅酸盐溶胶用于涂层和纤维形成

    公开(公告)号：US5019293A

    公开(公告)日：1991-05-28

    申请号：US364106

    申请日：1989-06-12

    Applicant: James M. Burlitch

    Inventor： James M. Burlitch

    IPC: B01J13/00 ,  C03C1/00 ,  C04B35/622 ,  C09D1/00 ,  D01F11/12

    CPC classification number: C04B35/6224 ,  B01J13/0026 ,  C03C1/008 ,  C04B35/62263 ,  C09D1/00 ,  D01F11/123

    Abstract: Stable magnesium containing silicate sols are produced by preparing a solution of silicon alkoxide and of magnesium alkoxide and optionally of aluminum alkoxide in solvent wherein the atomic ratio of Mg to Si ranges from 0.3:1 to 4:1 and simultaneously reacting said alkoxides with peroxy compound or peroxy compound and water. Water presence, rate of addition of reactant, quantity of solvent and temperature of reaction are controlled to negate formation of precipitate. For a magnesium silicate sol, preferably the silicon alkoxide is tetraethylorthosilicate, the magnesium alkoxide is magnesium methoxide, the solvent is methanol and 30% H.sub.2 O.sub.2 is used as a reactant. For a magnesium aluminosilicate sol, preferably the silicon alkoxide is tetraethylorthosilicate, the magnesium alkoxide is selected from the group consisting of magnesium-s-butoxide and magnesium-2-(2'-methoxyethoxy)ethoxide, the aluminum alkoxide is aluminum isopropoxide, the solvent is sec-butanol and 2-(2'-methoxyethoxy)ethanol and 30% H.sub.2 O.sub.2 is used as a reactant. A magnesium silicate sol containing unreacted alkoxy can be reacted with HF to produce a magnesium fluoride silicate sol. The sols are used for coating by forming a layer thereof on a substrate and drying. The coating can be converted to ceramic by firing in the case of substrates which are not harmed by the firing method. The sols are used to produce fibers by a process comprising the steps of concentrating, converting to gel fibers, drying and firing.

    Abstract translation: 稳定的含镁硅酸盐溶胶通过制备硅醇盐和烷氧化镁和任选的烷氧基铝溶液在溶剂中制备，其中Mg与Si的原子比范围为0.3:1至4:1，同时使所述醇盐与过氧化合物 或过氧化合物和水。 控制水存在，反应物加入速率，溶剂量和反应温度，以消除沉淀物的形成。 对于硅酸镁溶胶，优选硅醇盐是原硅酸四乙酯，醇盐是甲醇镁，溶剂是甲醇，30％H 2 O 2用作反应物。 对于硅铝酸镁溶胶，优选烷氧基硅烷是原硅酸四乙酯，醇盐选自正丁醇镁和2-（2'-甲氧基乙氧基）乙醇镁，醇铝是异丙醇铝，溶剂 是仲丁醇，使用2-（2'-甲氧基乙氧基）乙醇和30％H 2 O 2作为反应物。 含有未反应的烷氧基的硅酸镁溶胶可与HF反应生成氟化硅硅酸盐溶胶。 该溶胶通过在基材上形成层并进行干燥而被涂覆。 在不受烧成方法伤害的基材的情况下，可以通过烧成将涂层转化为陶瓷。 溶胶用于通过包括以下步骤的方法生产纤维，所述方法是浓缩，转化成凝胶纤维，干燥和焙烧。

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