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11. 发明授权

US07786022B2 Method for forming insulating film with low dielectric constant 失效
标题翻译：低介电常数形成绝缘膜的方法
公开(公告)号：US07786022B2
公开(公告)日：2010-08-31
申请号：US12029569
申请日：2008-02-12
申请人： Yoshitaka Hamada , Fujio Yagihashi , Takeshi Asano , Hideo Nakagawa , Masaru Sasago
发明人： Yoshitaka Hamada , Fujio Yagihashi , Takeshi Asano , Hideo Nakagawa , Masaru Sasago
IPC分类号： H01L21/31
CPC分类号： H01L21/31695 , C08G77/08 , C08L83/04 , C09D183/04 , H01B3/46 , H01L21/02126 , H01L21/02203 , H01L21/02216 , H01L21/02282 , H01L21/3122 , Y10T428/31663
摘要： In the invention, a silica sol prepared by hydrolyzing and condensing a silane compound represented by the following formula: Si(OR1)4 or R2nSi(OR3)4-n wherein R1s, R2(s) and R3(s) may be the same or different when a plurality of them are contained in the molecule and each independently represents a linear or branched C1-4 alkyl group in the presence of a hydrophilic basic catalyst and a hydrophobic basic catalyst is used for a conventional porous-film forming composition.
摘要翻译：在本发明中，通过水解和缩合由下式表示的硅烷化合物制备的硅溶胶：Si（OR1）4或R2nSi（OR3 )4-n，其中R1，R2（s）和R3（s）可以相同或者在分子中含有多个它们并且在亲水性碱性催化剂存在下各自独立地表示直链或支链C 1-4烷基，并且将疏水性碱性催化剂用于常规多孔膜形成组合物时使用。

12. 发明授权

US07754330B2 Organic silicon oxide core-shell particles and preparation method thereof, porous film-forming composition, porous film and formation method thereof, and semiconductor device 有权
标题翻译：有机氧化硅核壳颗粒及其制备方法，多孔成膜组合物，多孔膜及其形成方法以及半导体器件
公开(公告)号：US07754330B2
公开(公告)日：2010-07-13
申请号：US12472681
申请日：2009-05-27
申请人： Yoshitaka Hamada , Fujio Yagihashi , Takeshi Asano , Hideo Nakagawa , Masaru Sasago
发明人： Yoshitaka Hamada , Fujio Yagihashi , Takeshi Asano , Hideo Nakagawa , Masaru Sasago
IPC分类号： B32B5/16
CPC分类号： H01B3/10 , Y10T428/25 , Y10T428/259 , Y10T428/2991 , Y10T428/2993 , Y10T428/2995 , Y10T428/31663
摘要： Provided are organic silicon oxide fine particles which can be formed into a porous film having a dielectric constant and mechanical strength expected as a high-performance porous insulating film and having excellent chemical stability, and a preparation method thereof. Described specifically, provided are an organic silicon oxide fine particle comprising a core containing at least an inorganic silicon oxide or an organic silicon oxide and a shell containing at least an organic silicon oxide and being formed around the core by using shell-forming hydrolyzable silane in the presence of a basic catalyst; wherein of silicon atoms constituting the core or the shell, a ratio (T/Q) of a number (T) of silicon atoms having at least one bond directly attached to a carbon atom to a number (Q) of silicon atoms having all of four bonds attached to an oxygen atom is greater in the shell than in the core; and wherein the shell-forming hydrolyzable silane comprise at least a hydrolyzable silane compound having two or more hydrolyzable-group-having silicon atoms bound to each other via a carbon chain or via a carbon chain containing one silicon atom between some carbon atoms.
摘要翻译：提供可以形成具有期望作为高性能多孔绝缘膜的介电常数和机械强度并且具有优异的化学稳定性的多孔膜的有机氧化硅微粒及其制备方法。具体地说，提供了一种有机氧化硅微粒，其包含至少含有无机氧化硅或有机氧化硅的芯和至少含有有机氧化硅的壳，并且通过使用壳形成可水解硅烷在芯周围形成存在碱性催化剂; 其中构成核或壳的硅原子中，具有至少一个直接连接到碳原子上的键的硅原子数（T）与（Q）的硅原子数（Q）的比（T / Q）附着在氧原子上的四个键在壳中比在核中大; 并且其中所述成壳可水解硅烷至少包含具有两个或多个可水解基团的硅原子的可水解硅烷化合物，其通过碳链彼此结合，或通过在一些碳原子之间含有一个硅原子的碳链。

13. 发明申请

US20080290472A1 SEMICONDUCTOR INTERLAYER-INSULATING FILM FORMING COMPOSITION, PREPARATION METHOD THEREOF, FILM FORMING METHOD, AND SEMICONDUCTOR DEVICE 审中-公开
标题翻译：半导体层间绝缘膜形成组合物，其制备方法，膜形成方法和半导体器件
公开(公告)号：US20080290472A1
公开(公告)日：2008-11-27
申请号：US12029562
申请日：2008-02-12
申请人： Fujio Yagihashi , Yoshitaka Hamada , Takeshi Asano , Tsutomu Ogihara , Motoaki Iwabuchi , Hideo Nakagawa , Masaru Sasago
发明人： Fujio Yagihashi , Yoshitaka Hamada , Takeshi Asano , Tsutomu Ogihara , Motoaki Iwabuchi , Hideo Nakagawa , Masaru Sasago
IPC分类号： H01L23/58 , C08K3/34 , C08K3/36 , B32B5/18 , H01L21/312
CPC分类号： H01L21/31695 , C08G77/16 , C08G77/70 , C08G77/80 , C08K3/36 , C08L83/04 , C09D183/04 , H01L21/02126 , H01L21/02203 , H01L21/02216 , H01L21/02282 , H01L21/3122 , H01L21/7682 , H01L2221/1047 , Y10T428/249953 , C08L83/00
摘要： Provided is a porous-film-forming composition containing silicon-oxide-based fine particles and a polysiloxane compound obtained by hydrolysis and condensation reactions, in the presence of an acid catalyst, of a hydrolyzable silane compound containing at least one tetrafunctional alkoxysilane compound represented by the following formula (1): Si(OR1)4 (1) wherein, R1s may be the same or different and each independently represents a linear or branched C1-4 alkyl group and/or at least one alkoxysilane compound represented by the following formula (2): R2nSi(OR3)4-n (2) wherein, R2(s) may be the same or different when there are plural R2s and each independently represents a linear or branched C1-8 alkyl group, R3(s) may be the same or different when there are plural R3s and each independently represents a linear or branched C1-4 alkyl group, and n is an integer from 1 to 3 in the reaction mixture containing a large excess of water.
摘要翻译：本发明提供一种多孔膜形成用组合物，其含有氧化硅系微粒和通过水解缩合反应得到的聚硅氧烷化合物，在酸催化剂的存在下，含有至少一种四官能性烷氧基硅烷化合物的水解性硅烷化合物以下公式（1）：<？in-line-formula description =“In-line formula”end =“lead”？> Si（OR1）4（1）<？in-line-formula description =“In-line 式中，R 1可以相同或不同，各自独立地表示直链或支链C 1-4烷基和/或由下式（2）表示的至少一种烷氧基硅烷化合物： in-line-formula description =“In-line Formulas”end =“lead”？> R2nSi（OR3）4-n（2）<？in-line-formula description =“In-line Formulas”end =“tail” 其中，当有多个R 2并且各自独立地表示直链或支链的C 1-8烷基时，R 2（s）可以相同或不同，R 3（s）可以相同或不同当存在多个R 3并且各自独立地表示直链或支链C 1-4烷基时，并且n是含有大量过量水的反应混合物中n是1至3的整数。

14. 发明授权

US07402621B2 Porous-film-forming composition, preparation method of the composition, porous film and semiconductor device 有权
标题翻译：多孔膜形成组合物，组合物的制备方法，多孔膜和半导体器件
公开(公告)号：US07402621B2
公开(公告)日：2008-07-22
申请号：US11041780
申请日：2005-01-24
申请人： Tsutomu Ogihara , Fujio Yagihashi , Yoshitaka Hamada , Takeshi Anaso , Motoaki Iwabuchi , Masaru Sasago , Hideo Nakagawa
发明人： Tsutomu Ogihara , Fujio Yagihashi , Yoshitaka Hamada , Takeshi Anaso , Motoaki Iwabuchi , Masaru Sasago , Hideo Nakagawa
IPC分类号： C08G77/06
CPC分类号： H01L21/02126 , C08G77/06 , C08G77/08 , C09D183/02 , C09D183/04 , H01L21/02203 , H01L21/02216 , H01L21/02282 , H01L21/31695
摘要： The invention provides a coating solution for forming a porous film having excellent mechanical strength and dielectric properties and for easily forming a film with a freely controlled film thickness in an ordinarily employed method in semiconductor process. More specifically, provided are a method for preparing a porous-film-forming composition comprising steps of preparing polysiloxane, silica or zeolite particles (Component A), imparting crosslinkability to Component A, and temporarily terminating the crosslinkability; and a porous-film-forming composition obtainable in this method. In addition, provided is a method of forming a porous film comprising steps of preparing a porous-film-forming composition by preparing Component A, imparting crosslinkability to Component A and adding a crosslinkability inhibitor to temporarily terminate the crosslinkability; applying the porous-film-forming composition onto a substrate to form a film, drying the film, crosslinking the particles along with removing the crosslinkability inhibitor by heating the dried film.
摘要翻译：本发明提供一种用于形成具有优异的机械强度和介电性能的多孔膜的涂布溶液，并且在半导体工艺中通常采用的方法容易地形成具有自由控制的膜厚度的膜。更具体地说，提供了制备多孔膜形成组合物的方法，其包括制备聚硅氧烷，二氧化硅或沸石颗粒（组分A）的步骤，赋予组分A交联性，并暂时终止交联性; 和通过该方法得到的多孔膜形成组合物。此外，提供了形成多孔膜的方法，其包括通过制备组分A制备多孔膜形成组合物，赋予组分A交联性并加入交联性抑制剂以暂时终止交联性; 将多孔膜形成组合物施加到基材上以形成膜，干燥膜，使颗粒交联，同时通过加热干燥膜除去交联性抑制剂。

15. 发明申请

US20070087124A1 COMPOSITION FOR FORMING POROUS FILM, POROUS FILM AND METHOD FOR FORMING THE SAME, INTERLEVEL INSULATOR FILM, AND SEMICONDUCTOR DEVICE 审中-公开
标题翻译：用于形成多孔膜的组合物，多孔膜及其形成方法，间隔绝缘膜和半导体器件
公开(公告)号：US20070087124A1
公开(公告)日：2007-04-19
申请号：US11537697
申请日：2006-10-02
申请人： Motoaki Iwabuchi , Fujio Yagihashi , Yoshitaka Hamada , Hideo Nakagawa , Masaru Sasago
发明人： Motoaki Iwabuchi , Fujio Yagihashi , Yoshitaka Hamada , Hideo Nakagawa , Masaru Sasago
IPC分类号： C08J9/26 , B05D3/02
CPC分类号： C08G77/16 , C08G77/04 , C08G77/08 , C08K5/235 , C09D183/04 , H01L21/02126 , H01L21/02203 , H01L21/02216 , H01L21/02282 , H01L21/31695 , C08L83/04
摘要： Provided are a composition for forming porous film which can form a porous film having practical mechanical strength in a simple and low cost process; a porous film and a method for forming the film; and an inexpensive, high-performing and highly reliable semiconductor device comprising the porous film inside. More specifically, provided is a composition for forming porous film, comprising a polymer which is obtainable by hydrolyzing and condensing one or more silane compounds represented by Formula (1), or preferably by hydrolyzing and co-condensing one or more silane compounds represented by Formula (1) and one more silane compounds represented by Formula (2), Formulas (1) and (2) being: (R1)aSi(R2)4-a (1) (R3)bSi(R4)4-b (2)Also provided is a method for forming porous film comprising a step of applying said composition on a substrate to form film and a step of transforming the film into porous film.
摘要翻译：提供一种用于形成多孔膜的组合物，其可以以简单且低成本的方法形成具有实际机械强度的多孔膜; 多孔膜和形成膜的方法; 以及包含多孔膜的便宜，高性能和高可靠性的半导体器件。更具体地说，提供了一种用于形成多孔膜的组合物，其包含通过水解和缩合一种或多种由式（1）表示的硅烷化合物，或优选通过水解和共缩合一种或多种由式（1）和另外一个由式（2），式（1）和（2）表示的硅烷化合物是：<？in-line-formula description =“In-line formula”end =“lead” （1）＆lt;＆lt; 1＆gt;＆lt; 1＆gt;＆lt; 1＆gt; “In-line Formulas”end =“tail”？> <？in-line-formula description =“In-line Formulas”end =“lead”？>（R <3> ）（2）<βin-line-formula description =“In-line Formulas”end =“tail”？ >还提供了一种形成多孔膜的方法，包括将所述组合物施加在基底上以形成膜的步骤和将膜转化为多孔膜的步骤。

16. 发明申请

US20060289849A1 Composition for forming porous film, porous film and method for forming the same, interlevel insulator film, and semiconductor device 审中-公开
标题翻译：用于形成多孔膜的组合物，多孔膜及其形成方法，层间绝缘膜和半导体器件
公开(公告)号：US20060289849A1
公开(公告)日：2006-12-28
申请号：US11512968
申请日：2006-08-29
申请人： Fujio Yagihashi , Yoshitaka Hamada , Hideo Nakagawa , Masaru Sasago
发明人： Fujio Yagihashi , Yoshitaka Hamada , Hideo Nakagawa , Masaru Sasago
IPC分类号： H01L29/04
CPC分类号： H01L21/02126 , H01L21/02203 , H01L21/02216 , H01L21/02282 , H01L21/31695
摘要： The invention includes a semiconductor device. Specifically provided is a semiconductor device comprising a porous film therein, the porous film being formable by a composition comprising a surfactant, an aprotic polar solvent and a solution comprising a polymer formed by hydrolysis and condensation of one or more silane compounds represented by foramula (1) : RnSi(OR′)4-n. Also provided is a method for manufacturing a porous film comprising steps of applying said composition so as to form a film, drying the film and transforming the dried film to a porous film by removing said surfactant. The porous film obtained from the composition for forming porous film is further provided.
摘要翻译：本发明包括半导体器件。具体提供的是其中包含多孔膜的半导体器件，多孔膜可通过包含表面活性剂，非质子极性溶剂和包含由一个或多个由下列物质表示的硅烷化合物的水解和缩合形成的聚合物（1 ）：R n Si（OR'）4-n 还提供了一种制造多孔膜的方法，包括以下步骤：施加所述组合物以形成膜，干燥膜并通过除去所述表面活性剂将干燥的膜转化为多孔膜。进一步提供由多孔膜形成用组合物得到的多孔膜。

17. 发明授权

US07119354B2 Composition for forming porous film, porous film and method for forming the same, interlevel insulator film 失效
标题翻译：用于形成多孔膜的组合物，多孔膜及其形成方法，层间绝缘膜
公开(公告)号：US07119354B2
公开(公告)日：2006-10-10
申请号：US10810360
申请日：2004-03-26
申请人： Fujio Yagihashi , Yoshitaka Hamada , Hideo Nakagawa , Masaru Sasago
发明人： Fujio Yagihashi , Yoshitaka Hamada , Hideo Nakagawa , Masaru Sasago
IPC分类号： H01L47/00
CPC分类号： H01L21/02126 , H01L21/02203 , H01L21/02216 , H01L21/02282 , H01L21/31695
摘要： Provided is a coating liquid which can easily form a porous film having desirably controlled thickness by the method used for a usual semiconductor process, and having an excellent mesopore channel structure. Specifically provided is a composition for forming porous film comprising a surfactant, an aprotic polar solvent and a solution comprising a polymer formed by hydrolysis and condensation of one or more silane compounds represented by foramula (1): RnSi(OR′)4-n. Also provided is a method for manufacturing a porous film comprising steps of applying said composition so as to form a film, drying the film and transforming the dried film to a porous film by removing said surfactant. The porous film obtained from the composition for forming porous film is further provided.
摘要翻译：本发明提供一种可以通过通常的半导体工艺使用的方法容易地形成具有期望的控制厚度的多孔膜并具有优异的中孔通道结构的涂布液。具体地提供了一种用于形成多孔膜的组合物，其包含表面活性剂，非质子极性溶剂和包含通过水解和缩合由（1）表示的一种或多种硅烷化合物形成的聚合物的溶液：RnSi（OR'）4 -n 。还提供了一种制造多孔膜的方法，包括以下步骤：施加所述组合物以形成膜，干燥膜并通过除去所述表面活性剂将干燥的膜转化为多孔膜。进一步提供由多孔膜形成用组合物得到的多孔膜。

18. 发明申请

US20050165197A1 Porous-film-forming composition, preparation method of the composition, porous film and semiconductor device 有权
标题翻译：多孔膜形成组合物，组合物的制备方法，多孔膜和半导体器件
公开(公告)号：US20050165197A1
公开(公告)日：2005-07-28
申请号：US11041780
申请日：2005-01-24
申请人： Tsutomu Ogihara , Fujio Yagihashi , Yoshitaka Hamada , Takeshi Anaso , Motoaki Iwabuchi , Masaru Sasago , Hideo Nakagawa
发明人： Tsutomu Ogihara , Fujio Yagihashi , Yoshitaka Hamada , Takeshi Anaso , Motoaki Iwabuchi , Masaru Sasago , Hideo Nakagawa
IPC分类号： C04B38/00 , C01B33/12 , C08G77/06 , C08G77/08 , C09D183/02 , C09D183/04 , H01L21/316 , H01L21/768 , C08G77/20
CPC分类号： H01L21/02126 , C08G77/06 , C08G77/08 , C09D183/02 , C09D183/04 , H01L21/02203 , H01L21/02216 , H01L21/02282 , H01L21/31695
摘要： The invention provides a coating solution for forming a porous film having excellent mechanical strength and dielectric properties and for easily forming a film with a freely controlled film thickness in an ordinarily employed method in semiconductor process. More specifically, provided are a method for preparing a porous-film-forming composition comprising steps of preparing polysiloxane, silica or zeolite particles (Component A), imparting crosslinkability to Component A, and temporarily terminating the crosslinkability; and a porous-film-forming composition obtainable in this method. In addition, provided is a method of forming a porous film comprising steps of preparing a porous-film-forming composition by preparing Component A, imparting crosslinkability to Component A and adding a crosslinkability inhibitor to temporarily terminate the crosslinkability; applying the porous-film-forming composition onto a substrate to form a film, drying the film, crosslinking the particles along with removing the crosslinkability inhibitor by heating the dried film.
摘要翻译：本发明提供一种用于形成具有优异的机械强度和介电性能的多孔膜的涂布溶液，并且在半导体工艺中通常采用的方法容易地形成具有自由控制的膜厚度的膜。更具体地说，提供了制备多孔膜形成组合物的方法，其包括制备聚硅氧烷，二氧化硅或沸石颗粒（组分A）的步骤，赋予组分A交联性，并暂时终止交联性; 和通过该方法得到的多孔膜形成组合物。此外，提供了形成多孔膜的方法，其包括通过制备组分A制备多孔膜形成组合物，赋予组分A交联性并添加交联性抑制剂以暂时终止交联性的步骤; 将多孔膜形成组合物施加到基材上以形成膜，干燥膜，使颗粒交联，同时通过加热干燥膜除去交联性抑制剂。

19. 发明授权

US07239018B2 Composition for forming a porous film prepared by hydrolysis and condensation of an alkoxysilane using a trialkylmethylammonium hydroxide catalyst 失效
标题翻译：用于形成通过使用三烷基甲基氢氧化铵催化剂水解和缩合烷氧基硅烷制备的多孔膜的组合物
公开(公告)号：US07239018B2
公开(公告)日：2007-07-03
申请号：US10796656
申请日：2004-03-09
申请人： Yoshitaka Hamada , Fujio Yagihashi , Hideo Nakagawa , Masaru Sasago
发明人： Yoshitaka Hamada , Fujio Yagihashi , Hideo Nakagawa , Masaru Sasago
IPC分类号： H01L23/52 , H01L21/473
CPC分类号： H01L23/52 , H01L21/02126 , H01L21/02216 , H01L21/02282 , H01L21/3122 , H01L21/31633 , H01L21/31695 , H01L21/7682
摘要： Provided is a composition formed by hydrolysis and condensation composition of the alkoxysilane, the composition comprising a reduced amount of metallic and halogen impurities and being applicable as electronic material. Also provided is an insulating film having low dielectric constant produced by applying the composition and sintering it. More specifically, a method for manufacturing a composition for forming a film, comprising a step of hydrolysis and condensation of alkoxysilane or a partial hydrolysis product of the alkoxysilane in an organic solvent in the presence of trialkylmethylammonium hydroxide as catalyst, wherein the alkoxysilane is selected from the groups consisting of compounds represented by formulae (1) to (4) below, and the trialkylmethylammonium hydroxide is represented by formula (5) below. Provided are a composition for forming a film obtained by the method, and a low dielectric constant film having low metallic and halogen impurities, the film produced by applying the composition for forming a film on a substrate and sintering it.
摘要翻译：提供通过烷氧基硅烷的水解和缩合组合物形成的组合物，该组合物包含减少量的金属和卤素杂质并可用作电子材料。还提供了通过施加组合物并烧结而制备的具有低介电常数的绝缘膜。更具体地说，涉及一种用于形成膜的组合物的制造方法，其特征在于，在三烷基甲基氢氧化铵作为催化剂的存在下，包括在有机溶剂中烷氧基硅烷或部分水解产物的烷氧基硅烷的水解和缩合的步骤，其中烷氧基硅烷选自由下式（1）〜（4）表示的化合物和氢氧化三烷基甲基铵组成的基团由下式（5）表示。提供了一种用于形成通过该方法获得的膜的组合物和具有低金属和卤素杂质的低介电常数膜，该膜通过将在膜上形成膜的组合物施加并烧结而制备。

20. 发明授权

US07126208B2 Composition for forming porous film, porous film and method for forming the same, interlevel insulator film, and semiconductor device 失效
标题翻译：用于形成多孔膜的组合物，多孔膜及其形成方法，层间绝缘膜和半导体器件
公开(公告)号：US07126208B2
公开(公告)日：2006-10-24
申请号：US10706863
申请日：2003-11-12
申请人： Motoaki Iwabuchi , Fujio Yagihashi , Yoshitaka Hamada , Hideo Nakagawa , Masaru Sasago
发明人： Motoaki Iwabuchi , Fujio Yagihashi , Yoshitaka Hamada , Hideo Nakagawa , Masaru Sasago
IPC分类号： H01L23/58 , H01L21/31
CPC分类号： C08G77/16 , C08G77/04 , C08G77/08 , C08K5/235 , C09D183/04 , H01L21/02126 , H01L21/02203 , H01L21/02216 , H01L21/02282 , H01L21/31695 , C08L83/04
摘要： Provided are a composition for forming porous film which can form a porous film having practical mechanical strength in a simple and low cost process; a porous film and a method for forming the film; and an inexpensive, high-performing and highly reliable semiconductor device comprising the porous film inside. More specifically, provided is a composition for forming porous film, comprising a polymer which is obtainable by hydrolyzing and condensing one or more silane compounds represented by Formula (1), or preferably by hydrolyzing and co-condensing one or more silane compounds represented by Formula (1) and one more silane compounds represented by Formula (2), Formulas (1) and (2) being: (R1)aSi(R2)4-a (1) (R3)bSi(R4)4-b (2) Also provided is a method for forming porous film comprising a step of applying said composition on a substrate to form film and a step of transforming the film into porous film.
摘要翻译：提供一种用于形成多孔膜的组合物，其可以以简单且低成本的方法形成具有实际机械强度的多孔膜; 多孔膜和形成膜的方法; 以及包含多孔膜的便宜，高性能和高可靠性的半导体器件。更具体地说，提供了一种用于形成多孔膜的组合物，其包含通过水解和缩合一种或多种由式（1）表示的硅烷化合物，或优选通过水解和共缩合一种或多种由式（1）和另外一个由式（2），式（1）和（2）表示的硅烷化合物是：<？in-line-formula description =“In-line formula”end =“lead” （1）＆lt;＆lt; 1＆gt;＆lt; 1＆gt;＆lt; 1＆gt; “In-line Formulas”end =“tail”？> <？in-line-formula description =“In-line Formulas”end =“lead”？>（R <3> ）（2）<βin-line-formula description =“In-line Formulas”end =“tail”？ >还提供了一种形成多孔膜的方法，包括将所述组合物施加在基底上以形成膜的步骤和将膜转化为多孔膜的步骤。

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