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1. 发明授权

US08227028B2 Method for forming amorphous silica-based coating film with low dielectric constant and thus obtained amorphous silica-based coating film 有权
标题翻译：用于形成具有低介电常数的无定形二氧化硅基涂膜的方法，由此获得无定形二氧化硅基涂膜
公开(公告)号：US08227028B2
公开(公告)日：2012-07-24
申请号：US12310486
申请日：2007-07-11
申请人： Miki Egami , Akira Nakashima , Michio Komatsu
发明人： Miki Egami , Akira Nakashima , Michio Komatsu
IPC分类号： B05D3/02 , B05D3/04 , H01L29/00
CPC分类号： C09D1/00 , C09D4/00 , H01L21/316 , C08G77/04
摘要： A method of forming on a substrate an amorphous silica-based coating film having a low dielectric constant of 3.0 or below and a film strength (Young's modulus) of 3.0 GPa or more, which comprises, as a typical one, the steps of; (a) coating on the substrate a liquid composition containing hydrolysate of an organic silicon compound or compounds hydrolyzed in the presence of tetraalkylammonium hydroxide (TAAOH); (b) setting the substrate in a chamber and then drying a coating film formed on the substrate at a temperature in the range from 25 to 340° C.; (c) heating the coating film at a temperature in the range from 105 to 450° C. with introduction of a superheated steam having such a temperature into the chamber, and (d) curing the coating film at a temperature in the range from 350 to 450° C. with introduction of a nitrogen gas into the chamber.
摘要翻译：一种在基板上形成介电常数低于3.0或更低的无定形二氧化硅基涂层以及3.0GPa或更高的膜强度（杨氏模量）的方法，其中典型的步骤包括：（a）在基材上涂覆含有有机硅化合物的水解产物或在四烷基氢氧化铵（TAAOH））存在下水解的化合物的液体组合物; （b）将基板设置在室中，然后在25至340℃的温度范围内干燥形成在基板上的涂膜。（c）在105至450℃的温度范围内加热涂膜，并将具有这种温度的过热蒸汽引入室中，和（d）在350℃的温度下固化涂膜至450℃，同时将氮气引入室中。

2. 发明申请

US20060084277A1 Method of forming amorphous silica-based coating film with low dielectric constant and thus obtained silica-based coating film 有权
标题翻译：形成具有低介电常数的无定形二氧化硅基涂膜的方法，由此得到二氧化硅基涂膜
公开(公告)号：US20060084277A1
公开(公告)日：2006-04-20
申请号：US10533238
申请日：2003-10-27
申请人： Akira Nakashima , Miki Egami , Michio Komatsu , Yoshihiro Nakata , Ei Yano , Katsumi Suzuki
发明人： Akira Nakashima , Miki Egami , Michio Komatsu , Yoshihiro Nakata , Ei Yano , Katsumi Suzuki
IPC分类号： H01L21/31 , H01L21/469
CPC分类号： C09D183/02 , C08G77/08 , H01L21/02126 , H01L21/02203 , H01L21/02216 , H01L21/02282 , H01L21/02337 , H01L21/316 , H01L21/31695
摘要： The present invention relates to an amorphous silica-based coating film with a low specific dielectric constant of 2.5 or below and the Young's modulus of 6.0 GPa or more and having excellent hydrophobic property, and to a method of forming the same. A liquid composition containing a silicon compound obtained by hydrolyzing tetraalkyl ortho silicate (TAOS) and specific alkoxysilane (AS) in the presence of tetraalkyl ammonium hydroxide (TAAOH) is prepared. The liquid composition is then applied on a substrate, heated and cured to obtain a coating film. The coating film obtained as described has a smooth surface and also has specific micropores therein.
摘要翻译：本发明涉及具有2.5以下的比介电常数低，6.0GPa以上的杨氏模量和疏水性优异的无定形二氧化硅系涂膜及其形成方法。制备含有在四烷基氢氧化铵（TAAOH）存在下水解四烷基原硅酸盐（TAOS）和特定烷氧基硅烷（AS））得到的硅化合物的液体组合物。然后将液体组合物涂布在基材上，加热固化，得到涂膜。如上所述获得的涂膜具有光滑表面，并且其中也具有特定的微孔。

3. 发明申请

US20080011987A1 Coating Liquid for Forming Low Dielectric Constant Amorphous Silica-Based Coating Film, Method for Preparing the Same, and Low Dielectric Constant Amorphous Silica-Based Coating Film Obtained From the Same 审中-公开
标题翻译：用于形成低介电常数无定形二氧化硅基涂膜的涂布液，及其制备方法和从其获得的低介电常数非晶态二氧化硅基涂膜
公开(公告)号：US20080011987A1
公开(公告)日：2008-01-17
申请号：US11665746
申请日：2005-10-11
申请人： Hiroki Arao , Miki Egami , Akira Nakashima , Michio Komatsu
发明人： Hiroki Arao , Miki Egami , Akira Nakashima , Michio Komatsu
IPC分类号： H01B3/20 , C04B41/50
CPC分类号： H01L21/02216 , C08L83/08 , C09C1/30 , C09C1/3081 , C09D183/02 , C09D183/04 , C23C18/1212 , C23C18/1295 , C23C18/14 , H01L21/02126 , H01L21/02282 , H01L21/316 , C08L2666/02
摘要： Disclosed is a coating liquid for forming an amorphous silica-based coating film having a low dielectric constant of 3.0 or below and low leakage current, and a method for preparing the coating liquid. The coating liquid is a liquid composition comprising (a) silicon compound obtained by hydrolyzing tetraalkyl orthosilicate (TAOS) and alkoxysilane (AS) in the presence of tetraalkyl ammonium hydroxide (TAAOH) and water, or a silicon compound obtained by hydrolyzing or partially hydrolyzing tetraalkyl orthosilicate (TAOS) in the presence of tetraalkyl ammonium hydroxide (TAAOH) and water, mixing the hydrolyzed or partially hydrolyzed product with alkoxysilane (AS) or a hydrolyzed or partially hydrolyzed product thereof, and hydrolyzing all or a portion of the mixture, (b) an organic solvent, and (c) water. The coating liquid is characterized in that a quantity of water contained in the liquid composition is in the range from 30 to 60% by weight.
摘要翻译：公开了一种形成低介电常数为3.0以下，低漏电流的无定形二氧化硅系涂膜的涂布液及其制备方法。涂布液是一种液体组合物，其包含（a）在四烷基氢氧化铵（TAAOH）和水的存在下水解四烷基原硅酸酯（TAOS）和烷氧基硅烷（AS）而获得的硅化合物，或通过水解或部分水解四烷基在四烷基氢氧化铵（TAAOH）和水的存在下，将水解或部分水解的产物与烷氧基硅烷（AS）或其水解或部分水解产物混合，并水解所有或部分混合物，（b））有机溶剂，和（c）水。涂布液的特征在于，液体组合物中所含的水的量为30〜60重量％。

4. 发明授权

US08062414B2 Coating liquid for forming amorphous silica-based coating film with low dielectric constant 有权
标题翻译：用于形成具有低介电常数的无定形二氧化硅基涂膜的涂布液
公开(公告)号：US08062414B2
公开(公告)日：2011-11-22
申请号：US10533302
申请日：2003-10-27
申请人： Akira Nakashima , Miki Egami , Michio Komatsu , Yoshihiro Nakata , Ei Yano , Katsumi Suzuki
发明人： Akira Nakashima , Miki Egami , Michio Komatsu , Yoshihiro Nakata , Ei Yano , Katsumi Suzuki
IPC分类号： C04B41/50 , D06M15/643 , C09D183/04
CPC分类号： H01L21/02126 , C08G77/08 , C09D183/04 , H01L21/02216 , H01L21/02282 , H01L21/3122 , H01L21/316
摘要： The present invention relates to a coating liquid for forming an amorphous silica-based coating film with a low dielectric constant of 2.5 or below and the Young's modulus of 6.0 GPa or more and having excellent hydrophobic property, and to a method of preparing the same. The coating liquid may contain a silicon compound obtained by hydrolyzing tetraalkyl ortho silicate (TAOS) and specific alkoxysilane (AS) in the presence of tetraalkyl ammonium hydroxide (TAAOH), or may contain a silicon compound obtained by hydrolyzing or partially hydrolyzing tetraalkyl ortho silicate (TAOS) in the presence of tetraalkyl ammonium hydroxide (TAAOH), mixing the reaction product with specific alkoxysilane or a hydrolysate or a partial hydrolysate thereof, and hydrolyzing all or a portion of the mixture according to the necessity. In addition, the coating liquid is prepared by mixing components described above at a specific ratio and under specific process conditions.
摘要翻译：本发明涉及一种低介电常数为2.5以下，杨氏模量为6.0GPa以上，疏水性优异的无定形二氧化硅系涂膜用涂布液及其制备方法。涂布液可以含有通过在四烷基氢氧化铵（TAAOH）的存在下水解四烷基原硅酸盐（TAOS）和特定烷氧基硅烷（AS））而获得的硅化合物，或者可以含有通过水解或部分水解原硅酸四烷基酯 TAOS）在四烷基氢氧化铵（TAAOH）的存在下，将反应产物与特定的烷氧基硅烷或其水解产物或其部分水解产物混合，并根据需要水解全部或一部分混合物。此外，通过以特定比例和特定工艺条件混合上述组分来制备涂布液。

5. 发明申请

US20100003181A1 Method For Forming Amorphous Silica-Based Coating Film With Low Dielectric Constant And Thus Obtained Amorphous Silica-Based Coating Film 有权
标题翻译：形成具有低介电常数的无定形二氧化硅基涂膜的方法，从而获得无定形二氧化硅基涂膜
公开(公告)号：US20100003181A1
公开(公告)日：2010-01-07
申请号：US12310486
申请日：2007-07-11
申请人： Miki Egami , Akira Nakashima , Michio Komatsu
发明人： Miki Egami , Akira Nakashima , Michio Komatsu
IPC分类号： C01B33/12 , H01L21/316
CPC分类号： C09D1/00 , C09D4/00 , H01L21/316 , C08G77/04
摘要： A method of forming on a substrate an amorphous silica-based coating film having a low dielectric constant of 3.0 or below and a film strength (Young's modulus) of 3.0 GPa or more, which comprises, as a typical one, the steps of; (a) coating on the substrate a liquid composition containing hydrolysate of an organic silicon compound or compounds hydrolyzed in the presence of tetraalkylammonium hydroxide (TAAOH); (b) setting the substrate in a chamber and then drying a coating film formed on the substrate at a temperature in the range from 25 to 340° C.; (c) heating the coating film at a temperature in the range from 105 to 450° C. with introduction of a superheated steam having such a temperature into the chamber, and (d) curing the coating film at a temperature in the range from 350 to 450° C. with introduction of a nitrogen gas into the chamber.
摘要翻译：一种在基板上形成介电常数低于3.0或更低的无定形二氧化硅基涂层以及3.0GPa或更高的膜强度（杨氏模量）的方法，其中典型的步骤包括：（a）在基材上涂覆含有有机硅化合物的水解产物或在四烷基氢氧化铵（TAAOH））存在下水解的化合物的液体组合物; （b）将基板设置在室中，然后在25至340℃的温度范围内干燥形成在基板上的涂膜。（c）在105至450℃的温度范围内加热涂膜，并将具有这种温度的过热蒸汽引入室中，和（d）在350℃的温度下固化涂膜至450℃，同时将氮气引入室中。

6. 发明授权

US07232769B2 Method of forming amorphous silica-based coating film with low dielectric constant and thus obtained silica-based coating film 有权
标题翻译：形成具有低介电常数的无定形二氧化硅基涂膜的方法，由此得到二氧化硅基涂膜
公开(公告)号：US07232769B2
公开(公告)日：2007-06-19
申请号：US10533238
申请日：2003-10-27
申请人： Akira Nakashima , Miki Egami , Michio Komatsu , Yoshihiro Nakata , Ei Yano , Katsumi Suzuki
发明人： Akira Nakashima , Miki Egami , Michio Komatsu , Yoshihiro Nakata , Ei Yano , Katsumi Suzuki
IPC分类号： H01L21/30
CPC分类号： C09D183/02 , C08G77/08 , H01L21/02126 , H01L21/02203 , H01L21/02216 , H01L21/02282 , H01L21/02337 , H01L21/316 , H01L21/31695
摘要： The present invention relates to an amorphous silica-based coating film with a low specific dielectric constant of 2.5 or below and the Young's modulus of 6.0 GPa or more and having excellent hydrophobic property, and to a method of forming the same. A liquid composition containing a silicon compound obtained by hydrolyzing tetraalkyl ortho silicate (TAOS) and specific alkoxysilane (AS) in the presence of tetraalkyl ammonium hydroxide (TAAOH) is prepared. The liquid composition is then applied on a substrate, heated and cured to obtain a coating film. The coating film obtained as described has a smooth surface and also has specific micropores therein.
摘要翻译：本发明涉及具有2.5以下的比介电常数低，6.0GPa以上的杨氏模量和疏水性优异的无定形二氧化硅系涂膜及其形成方法。制备含有在四烷基氢氧化铵（TAAOH）存在下水解四烷基原硅酸盐（TAOS）和特定烷氧基硅烷（AS））得到的硅化合物的液体组合物。然后将液体组合物涂布在基材上，加热固化，得到涂膜。如上所述获得的涂膜具有光滑表面，并且其中也具有特定的微孔。

7. 发明授权

US06451436B1 Coating liquid for forming a silica-containing film with a low-dielectric constant and substrate coated with such a film 有权
标题翻译：用于形成具有低介电常数的含二氧化硅的膜和用这种膜涂覆的基材的涂布液
公开(公告)号：US06451436B1
公开(公告)日：2002-09-17
申请号：US09577507
申请日：2000-05-24
申请人： Michio Komatsu , Akira Nakashima , Miki Egami
发明人： Michio Komatsu , Akira Nakashima , Miki Egami
IPC分类号： B32B904
CPC分类号： H01L21/3122 , C09D183/04 , H01L21/02126 , H01L21/02216 , H01L21/02282 , H01L21/02337 , Y10T428/31511 , Y10T428/31663 , Y10T428/31725 , Y10T428/31786 , Y10T428/31855 , C08L2666/02
摘要： A coating liquid for forming a silica-containing film with a low-dielectric constant, which enables the formation of a low-density film having a dielectric constant as low as 3 or less and being excellent not only in resistance of oxygen plasma and in process adaptation but also in adhesion to a substrate and in film strength, is provided. A substrate coated with the silica-containing film having the above characteristics, which is obtained by the use of the above coating liquid, is further provided. The coating liquid for forming a silica-containing film with a low-dielectric constant comprises a polymer composition mainly constituted by (i) a hydrolyzate of at least one alkoxysilane represented by the following formula (I) and/or at least one halogenated silane represented by the following formula (II), and (ii) a readily decomposable resin, XnSi(OR)4−n (I) XnSiX′4−n (II) wherein X represents a hydrogen atom, a fluorine atom, an unfluorinated or fluorinated alkyl group of 1 to 8 carbon atoms, an aryl group or a vinyl group; R represents a hydrogen atom, an alkyl group of 1 to 8 carbon atoms, an aryl group or a vinyl group; X′ represents a halogen atom; and n is an integer of 0 to 3.
摘要翻译：一种用于形成具有低介电常数的含二氧化硅的膜的涂布液，其能够形成介电常数低至3或更低的低密度膜，并且不仅具有优异的氧等离子体的电阻和过程提供适应性，但也适用于对基材的粘合性和膜强度。进一步提供了通过使用上述涂布液而获得的具有上述特性的含二氧化硅膜的基材。用于形成具有低介电常数的含二氧化硅膜的涂布液包括主要由（i）由下式（I）表示的至少一种烷氧基硅烷的水解产物和/或至少一种卤代硅烷代表的聚合物组合物通过下式（II）和（ii）易分解性树脂，其中X表示氢原子，氟原子，1至8个碳原子的未氟化或氟化烷基，芳基或乙烯基; R表示氢原子，1〜8个碳原子的烷基，芳基或乙烯基; X'表示卤原子; n为0〜3的整数。

8. 发明授权

US08686101B2 Coating liquid for forming low dielectric constant amorphous silica-based coating film and the coating film obtained from the same 有权
标题翻译：用于形成低介电常数无定形二氧化硅基涂膜的涂布液和由其获得的涂膜
公开(公告)号：US08686101B2
公开(公告)日：2014-04-01
申请号：US12086745
申请日：2006-12-15
申请人： Miki Egami , Hiroki Arao , Akira Nakashima , Michio Komatsu
发明人： Miki Egami , Hiroki Arao , Akira Nakashima , Michio Komatsu
IPC分类号： C08G77/08
CPC分类号： H01L21/316 , C01B33/12 , C08G77/50 , C09D183/14 , H01B3/08 , H01L21/02126 , H01L21/02216 , H01L21/02282 , H01L21/3122
摘要： A coating liquid for forming a low dielectric constant amorphous silica-based coating film with a dielectric constant of 3.0 or below and a film strength (Young's modulus) of 3.0 GPa or more, and also having a smooth surface with an excellent hydrophobicity. The coating liquid contains (1) a silicon compound obtained by hydrolyzing bis(trialkoxysilyl)alkane (BTASA) and alkoxysilane (AS) in the presence of tetraalkylammoniumhydroxide (TAAOH), or (2) a silicon compound obtained by hydrolyzing bis(trialkoxysilyl)alkane (BTASA), alkoxysilane (AS) and tetraalkylorthosilicate (TAOS) in the presence of tetraalkylammoniumhydroxide (TAAOH).
摘要翻译：一种用于形成介电常数为3.0以下，膜强度（杨氏模量）为3.0GPa以上的低介电常数无定形二氧化硅系涂膜的涂布液，并且还具有疏水性优异的光滑表面。涂布液含有（1）在四烷基氢氧化铵（TAAOH）存在下水解双（三烷氧基甲硅烷基）烷烃（BTASA）和烷氧基硅烷（AS））得到的硅化合物，或（2）通过水解双（三烷氧基甲硅烷基）烷烃获得的硅化合物（BTASA），烷氧基硅烷（AS）和四烷基原硅酸盐（TAOS）在四烷基氢氧化铵（TAAOH）存在下。

9. 发明授权

US07998567B2 Coating liquid for formation of protective film for semiconductor processing and method for preparation of the same 有权
标题翻译：用于形成半导体加工用保护膜的涂布液及其制备方法
公开(公告)号：US07998567B2
公开(公告)日：2011-08-16
申请号：US11665747
申请日：2005-10-11
申请人： Miki Egami , Hiroki Arao , Akira Nakashima , Michio Komatsu
发明人： Miki Egami , Hiroki Arao , Akira Nakashima , Michio Komatsu
IPC分类号： B32B3/26
CPC分类号： H01L21/02126 , C09D183/02 , C09D183/04 , H01L21/02203 , H01L21/02282 , H01L21/02351 , H01L21/3121 , Y10T428/249953
摘要： Disclosed is a coating liquid for forming a protective film having high film strength and a low specific dielectric constant for semiconductor processing, and a method for preparing the coating liquid. The coating liquid is a liquid composition comprising (a) silicon compound obtained by hydrolyzing tetraalkyl orthosilicate (TAOS) and alkoxysilane (AS) in the presence of tetraalkyl ammonium hydroxide (TAAOH) and water, or a silicon compound obtained by hydrolyzing or partially hydrolyzing tetraalkyl orthosilicate (TAOS) in the presence of tetraalkyl ammonium hydroxide (TAAOH) and water, mixing the hydrolyzed or partially hydrolyzed product with alkoxysilane (AS) or a hydrolyzed or partially hydrolyzed product thereof, and hydrolyzing all or a portion of the mixture, (b) an organic solvent, and (c) water. The coating liquid is characterized in that a quantity of water contained in the liquid composition is in the range from 35 to 65% by weight.
摘要翻译：公开了一种用于形成用于半导体加工的具有高膜强度和低比介电常数的保护膜的涂布液，以及一种制备涂布液的方法。涂布液是一种液体组合物，其包含（a）在四烷基氢氧化铵（TAAOH）和水的存在下水解四烷基原硅酸酯（TAOS）和烷氧基硅烷（AS）而获得的硅化合物，或通过水解或部分水解四烷基在四烷基氢氧化铵（TAAOH）和水的存在下，将水解或部分水解的产物与烷氧基硅烷（AS）或其水解或部分水解产物混合，并水解所有或部分混合物，（b））有机溶剂，和（c）水。涂布液的特征在于，液体组合物中含有的水的量在35至65重量％的范围内。

10. 发明申请

US20090061199A1 Coating liquid for formation of protective film for semiconductor processing, method for preparation of the same, and protective film for semiconductor processing made from the coating liquid 有权
标题翻译：用于形成用于半导体加工的保护膜的涂布液，其制备方法和由涂布液制成的用于半导体加工的保护膜
公开(公告)号：US20090061199A1
公开(公告)日：2009-03-05
申请号：US11665747
申请日：2005-10-11
申请人： Miki Egami , Hiroki Arao , Akira Nakashima , Michio Komatsu
发明人： Miki Egami , Hiroki Arao , Akira Nakashima , Michio Komatsu
IPC分类号： B32B3/26 , C09D7/12
CPC分类号： H01L21/02126 , C09D183/02 , C09D183/04 , H01L21/02203 , H01L21/02282 , H01L21/02351 , H01L21/3121 , Y10T428/249953
摘要： Disclosed is a coating liquid for forming a protective film having high film strength and a low specific dielectric constant for semiconductor processing, and a method for preparing the coating liquid. The coating liquid is a liquid composition comprising (a) silicon compound obtained by hydrolyzing tetraalkyl orthosilicate (TAOS) and alkoxysilane (AS) in the presence of tetraalkyl ammonium hydroxide (TAAOH) and water, or a silicon compound obtained by hydrolyzing or partially hydrolyzing tetraalkyl orthosilicate (TAOS) in the presence of tetraalkyl ammonium hydroxide (TAAOH) and water, mixing the hydrolyzed or partially hydrolyzed product with alkoxysilane (AS) or a hydrolyzed or partially hydrolyzed product thereof, and hydrolyzing all or a portion of the mixture, (b) an organic solvent, and (c) water. The coating liquid is characterized in that a quantity of water contained in the liquid composition is in the range from 35 to 65% by weight.
摘要翻译：公开了一种用于形成用于半导体加工的具有高膜强度和低比介电常数的保护膜的涂布液，以及一种制备涂布液的方法。涂布液是一种液体组合物，其包含（a）在四烷基氢氧化铵（TAAOH）和水的存在下水解四烷基原硅酸酯（TAOS）和烷氧基硅烷（AS）而获得的硅化合物，或通过水解或部分水解四烷基在四烷基氢氧化铵（TAAOH）和水的存在下，将水解或部分水解的产物与烷氧基硅烷（AS）或其水解或部分水解产物混合，并水解所有或部分混合物，（b））有机溶剂，和（c）水。涂布液的特征在于，液体组合物中含有的水的量在35至65重量％的范围内。

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