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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. 发明授权

US06652612B2 Silica particles for polishing and a polishing agent 有权
标题翻译：用于抛光的二氧化硅颗粒和抛光剂
公开(公告)号：US06652612B2
公开(公告)日：2003-11-25
申请号：US10291643
申请日：2002-11-12
申请人： Kazuhiro Nakayama , Akira Nakashima , Michio Komatsu
发明人： Kazuhiro Nakayama , Akira Nakashima , Michio Komatsu
IPC分类号： C01B3312
CPC分类号： B82Y30/00 , C01P2004/62 , C01P2004/64 , C01P2004/80 , C01P2006/90 , C09C1/3081 , C09K3/1409
摘要： Silica particles for polishing have a three-dimensional polycondensation structure with an average particle diameter in a range from 5 to 300 nm. The silica particles have residual alkoxy groups therein and a carbon content in a range from 0.5 to 5 weight % retained in the residual alkoxy groups.
摘要翻译：用于抛光的二氧化硅颗粒具有平均粒径在5至300nm范围内的三维缩聚结构。二氧化硅粒子中残留有烷氧基，碳残存在残留的烷氧基中的为0.5〜5质量％。

4. 发明授权

US06455154B1 Production of short fiber silica 有权
标题翻译：生产短纤维二氧化硅
公开(公告)号：US06455154B1
公开(公告)日：2002-09-24
申请号：US09560984
申请日：2000-04-28
申请人： Akira Nakashima , Kazuaki Inoue , Ryo Muraguchi , Michio Komatsu
发明人： Akira Nakashima , Kazuaki Inoue , Ryo Muraguchi , Michio Komatsu
IPC分类号： D02G300
CPC分类号： C08G77/02 , C09D183/02 , Y10T428/2904 , Y10T428/2907 , Y10T428/2918 , Y10T428/31663
摘要： A coating liquid for forming porous silica coating, comprising a product of reaction between a short fiber silica and a hydrolyzate of an alkoxysilane of the formula XnSi(OR)4-n or a halogenated silane of the formula XnSiX′4-n (in the formula, X represents a hydrogen atom, a fluorine atom, an alkyl group having 1 to 8 carbon atoms, an aryl group or a vinyl group; R represents a hydrogen atom, an alkyl group having 1 to 8 carbon atoms, an aryl group or a vinyl group; X′ represents a chlorine atom or a bromine atom; and n is an integer of 0 to 3). A coated substrate comprising a porous silica coating film formed from the above coating liquid for forming porous silica coating. A short fiber silica having an average diameter (D) of 10 to 30 nm, a length (L) of 30 to 100 nm and an aspect ratio (L/D) of 3 to 10. The above coating liquid for forming porous silica coating enables forming an insulating film which is excellent in adherence to a substrate surface, mechanical strength, chemical resistance and crack resistance and enables flattening irregularities of a substrate surface to a high degree. The coating film of the coated substrate has the above excellent properties.
摘要翻译：一种用于形成多孔二氧化硅涂层的涂布液，包括短纤维二氧化硅和式XnSi（OR）4-n的烷氧基硅烷的水解产物或式XnSiX'4-n的卤代硅烷（在式中，X表示氢原子，氟原子，碳原子数1〜8的烷基，芳基或乙烯基; R表示氢原子，碳原子数1〜8的烷基，芳基或乙烯基; X'表示氯原子或溴原子，n表示0〜3的整数。一种涂覆基材，包括由用于形成多孔二氧化硅涂层的上述涂布液形成的多孔二氧化硅涂膜。平均直径（D）为10〜30nm，长度（L）为30〜100nm，纵横比（L / D）为3〜10的短纤维二氧化硅。上述用于形成多孔二氧化硅涂层的涂布液能够形成对基板表面的粘附性优异的机械强度，耐化学性和抗裂纹性的绝缘膜，能够高度地使基板表面变得平坦化。涂布基材的涂膜具有上述优异的性能。

5. 发明授权

US6090446A Method of forming particle layer on substrate, method of planarizing irregular surface of substrate and particle-layer-formed substrate 失效
标题翻译：在基板上形成颗粒层的方法，平面化基板和颗粒层形成的基板的不规则表面的方法
公开(公告)号：US6090446A
公开(公告)日：2000-07-18
申请号：US624537
申请日：1996-04-12
申请人： Akira Nakashima , Michio Komatsu , Kenji Ohno , Kuniharu Teramoto , Kazuaki Inoue
发明人： Akira Nakashima , Michio Komatsu , Kenji Ohno , Kuniharu Teramoto , Kazuaki Inoue
IPC分类号： B01J19/00 , B05D1/20 , G11B5/84 , G11B7/26 , H01L21/768 , B05D5/00 , B05D1/18 , B32B3/00
CPC分类号： B05D1/20 , Y10T428/24372 , Y10T428/24893
摘要： The present invention provides a method of forming on a substrate a particle layer highly adherent to the substrate, which comprises the steps of spreading a dispersion (I) comprising a dispersing medium and, dispersed therein, solid particles being surface treated with a compound acting as a binder on a liquid (II) having a specific gravity higher than that of the dispersing medium, said liquid (II) being immiscible with the dispersing medium, subsequently removing the dispersing medium from the dispersion (I) to thereby arrange the solid particles on the liquid (II) so that a particle layer is formed on the liquid (II) and thereafter transferring the particle layer onto a substrate. Moreover, the present invention provides a method of planarizing an irregular surface of a substrate, which comprises transferring the above particle layer to an irregular surface of a substrate and removing parts of the particle layer formed on protrudent parts of the substrate to thereby planarize the irregular surface of the substrate and also provides a particle-layer-formed substrate comprising a substrate and, superimposed on a surface thereof, the particle layer obtained by each of the above methods.
摘要翻译： PCT No.PCT / JP95 / 01610 Sec。 371日期：1996年4月12日 102（e）日期1996年4月12日PCT提交1995年8月11日PCT公布。出版物WO96 / 04998 日本1996年2月22日本发明提供了在基材上形成与基材高度附着的颗粒层的方法，其包括以下步骤：将包含分散介质的分散体（I）铺展并分散在其中进行表面处理的固体颗粒在比重高于分散介质的液体（II）上作为粘合剂的化合物，所述液体（II）与分散介质不混溶，随后从分散体（I）中除去分散介质，由此将固体颗粒布置在液体（II）上，使得在液体（II）上形成颗粒层，然后将颗粒层转移到基材上。此外，本发明提供一种平面化基板的不规则表面的方法，其包括将上述颗粒层转移到基板的不规则表面，并除去形成在基板突出部分上的颗粒层的部分，从而平坦化不规则并且还提供了包含基材的颗粒层形成的基材，并且在其表面上叠加通过上述方法获得的颗粒层。

6. 发明授权

US6083314A Coating liquid for forming porous silica coating, coated substrate and short fiber silica 有权
标题翻译：用于形成多孔二氧化硅涂层，涂布基材和短纤维二氧化硅的涂布液
公开(公告)号：US6083314A
公开(公告)日：2000-07-04
申请号：US130043
申请日：1998-08-06
申请人： Akira Nakashima , Kazuaki Inoue , Ryo Muraguchi , Michio Komatsu
发明人： Akira Nakashima , Kazuaki Inoue , Ryo Muraguchi , Michio Komatsu
IPC分类号： C08L83/04 , C08G77/02 , C09D7/12 , C09D183/02 , C09D183/04 , C09D183/07 , C09D183/05 , C09D183/06 , C09D183/08
CPC分类号： C08G77/02 , C09D183/02 , Y10T428/2904 , Y10T428/2907 , Y10T428/2918 , Y10T428/31663
摘要： A coating liquid for forming porous silica coating, comprising a product of reaction between a short fiber silica and a hydrolyzate of an alkoxysilane of the formula X.sub.n Si(OR).sub.4-n or a halogenated silane of the formula X.sub.n SiX'.sub.4-n (in the formula, X represents a hydrogen atom, a fluorine atom, an alkyl group having 1 to 8 carbon atoms, an aryl group or a vinyl group; R represents a hydrogen atom, an alkyl group having 1 to 8 carbon atoms, an aryl group or a vinyl group; X' represents a chlorine atom or a bromine atom; and n is an integer of 0 to 3). A coated substrate comprising a porous silica coating film formed from the above coating liquid for forming porous silica coating. A short fiber silica having an average diameter (D) of 10 to 30 nm, a length (L) of 30 to 100 nm and an aspect ratio (L/D) of 3 to 10. The above coating liquid for forming porous silica coating enables forming an insulating film which is excellent in adherence to a substrate surface, mechanical strength, chemical resistance and crack resistance and enables flattening irregularities of a substrate surface to a high degree. The coating film of the coated substrate has the above excellent properties.
摘要翻译：一种用于形成多孔二氧化硅涂层的涂布液，包括短纤维二氧化硅和式XnSi（OR）4-n的烷氧基硅烷的水解产物或式XnSiX'4-n的卤代硅烷（在式中，X表示氢原子，氟原子，碳原子数1〜8的烷基，芳基或乙烯基; R表示氢原子，碳原子数1〜8的烷基，芳基或乙烯基; X'表示氯原子或溴原子，n表示0〜3的整数。一种涂覆基材，包括由用于形成多孔二氧化硅涂层的上述涂布液形成的多孔二氧化硅涂膜。平均直径（D）为10〜30nm，长度（L）为30〜100nm，纵横比（L / D）为3〜10的短纤维二氧化硅。上述用于形成多孔二氧化硅涂层的涂布液能够形成对基板表面的粘附性优异的机械强度，耐化学性和抗裂纹性的绝缘膜，能够高度地使基板表面变得平坦化。涂布基材的涂膜具有上述优异的性能。

7. 发明授权

US5204177A Process for preparing conductive fine particles and conductive coating materials containing said particles 失效
标题翻译：制备导电细颗粒和含有所述颗粒的导电涂层材料的方法
公开(公告)号：US5204177A
公开(公告)日：1993-04-20
申请号：US754208
申请日：1991-08-27
申请人： Goro Sato , Michio Komatsu , Tsuguo Koyanagi , Masayuki Matsuda , Hiroo Yoshidome , Akira Nakashima , Kazuaki Inoue
发明人： Goro Sato , Michio Komatsu , Tsuguo Koyanagi , Masayuki Matsuda , Hiroo Yoshidome , Akira Nakashima , Kazuaki Inoue
IPC分类号： C01G15/00 , C01G19/02 , C09C3/12 , C09D5/24 , H01B1/08 , H01B1/20
CPC分类号： C01G15/00 , C01G19/02 , C09C3/12 , C09D5/24 , H01B1/08 , H01B1/20 , C01P2002/52 , C01P2002/54 , Y10S428/918 , Y10T428/256
摘要： Transparent conductive coatings excellent in transparency are provided on substrates such as glass, plastics, etc. by the use of conductive coating materials obtained by maintaining aqueous solutions of hydrolyzable tin containing or indium containing compounds at pH of 8-12, and gradually hydrolyzing said compounds in the solutions to form sols containing colloidal particles, followed by drying and calcining.
摘要翻译：通过使用通过维持pH为8-12的维持含有水解性锡或含铟化合物的水溶液获得的导电涂层材料，在诸如玻璃，塑料等的基材上提供透明度优异的透明导电涂层，并逐渐水解所述化合物在形成含有胶体颗粒的溶胶的溶液中，然后干燥和煅烧。

8. 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％。

9. 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。

10. 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。

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