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1. 发明授权

US07235500B2 Material for forming silica based film 有权
标题翻译：用于形成二氧化硅基膜的材料
公开(公告)号：US07235500B2
公开(公告)日：2007-06-26
申请号：US11000735
申请日：2004-12-01
申请人： Yasushi Fujii , Tatsuhiko Shibuya , Isao Sato
发明人： Yasushi Fujii , Tatsuhiko Shibuya , Isao Sato
IPC分类号： H01L21/31 , H01L21/469
CPC分类号： H01L21/02118 , H01L21/316 , H01L21/76814
摘要： A material for forming a silica based film which enables the production of a silica based film with a reduced etching rate relative to hydrofluoric acid. This material includes a solid fraction containing a film forming component capable of generating a silica based film, an organic solvent, and water, and the water content of the material, as determined by gas chromatography measurement, is within a range from 0.1 to 50% by weight.
摘要翻译：用于形成二氧化硅基膜的材料，其能够以相对于氢氟酸的蚀刻速率降低的方式制备二氧化硅基膜。该材料包括含有能够产生二氧化硅基膜，有机溶剂和水的成膜组分的固体部分，并且通过气相色谱测量确定的材料的水含量在0.1至50％的范围内，重量。

2. 发明申请

US20050136692A1 Material for forming silica based film 有权
标题翻译：用于形成二氧化硅基膜的材料
公开(公告)号：US20050136692A1
公开(公告)日：2005-06-23
申请号：US11000735
申请日：2004-12-01
申请人： Yasushi Fujii , Tatsuhiko Shibuya , Isao Sato
发明人： Yasushi Fujii , Tatsuhiko Shibuya , Isao Sato
IPC分类号： C09D183/04 , C08L83/04 , C08L83/12 , C09D5/25 , C09D183/02 , C09D183/05 , H01L21/316 , H01L21/768 , H01L21/31 , H01L21/469
CPC分类号： H01L21/02118 , H01L21/316 , H01L21/76814
摘要： A material for forming a silica based film which enables the production of a silica based film with a reduced etching rate relative to hydrofluoric acid. This material includes a solid fraction containing a film forming component capable of generating a silica based film, an organic solvent, and water, and the water content of the material, as determined by gas chromatography measurement, is within a range from 0.1 to 50% by weight.
摘要翻译：用于形成二氧化硅基膜的材料，其能够以相对于氢氟酸的蚀刻速率降低的方式制备二氧化硅基膜。该材料包括含有能够产生二氧化硅基膜，有机溶剂和水的成膜组分的固体部分，并且通过气相色谱测量确定的材料的水含量在0.1至50％的范围内，重量。

3. 发明授权

US07060361B2 Silica-based organic film and method of manufacturing the same, and base material comprising organic film 有权
公开(公告)号：US07060361B2
公开(公告)日：2006-06-13
申请号：US10616731
申请日：2003-07-10
申请人： Tatsuhiko Shibuya , Yasushi Fujii
发明人： Tatsuhiko Shibuya , Yasushi Fujii
IPC分类号： B32B9/04
CPC分类号： H01L21/02126 , H01L21/02134 , H01L21/02216 , H01L21/02282 , H01L21/02304 , H01L21/02337 , H01L21/3122 , H01L21/316 , Y10T428/31663
摘要： A film is provided which can be applied to high-temperature processes and can fill microspaces between wirings without forming voids and prevent the occurrence of side etching, and also causes less degassing due to increase of an atmospheric temperature. A coating solution containing a reaction product which is obtained by hydrolyzing at least one first alkoxysilane compound selected from the group consisting of compounds represented by general formula (I) and compounds represented by general formula (II) in an organic solvent in the presence of an acid catalyst is applied on a target material to form a coating film, and then the coating film is baked in an atmosphere having an oxygen concentration of 1000 ppm or less to form a silica-based organic film. At least one second alkoxysilane compound selected from the group consisting of compounds represented by general formula (III) may be used in combination: R12Si(OR2)2 (I) R3Si(OR4)3 (II) Si(OR5)4 (III) wherein R1 and R3 each represents an alkyl group having 1 to 4 carbon atoms or a phenyl group, R2, R4, and R5 each represents an alkyl group having 1 to 4 carbon atoms.

4. 发明授权

US5885654A Polysilazane-based coating solution for interlayer insulation 失效
标题翻译：用于层间绝缘的聚硅氮烷基涂层溶液
公开(公告)号：US5885654A
公开(公告)日：1999-03-23
申请号：US909848
申请日：1997-08-12
申请人： Yoshio Hagiwara , Tatsuhiko Shibuya
发明人： Yoshio Hagiwara , Tatsuhiko Shibuya
IPC分类号： C09D183/16 , G02F1/1333 , B05D3/02
CPC分类号： C09D183/16 , G02F1/133345
摘要： Proposed is a coating solution for the formation of an interlayer insulating film of silicon dioxide in the manufacture of various kinds of electronic devices having excellent storage stability and coating workability. The principal ingredient of the coating solution, of which the solvent is preferably a dialkyl ether, is a polysilazane compound modified with a trimethylsilylating agent such as hexamethyl disilazane to such an extent that, in the .sup.1 H-NMR spectrometric diagram, the ratio of the area of the peak assignable to SiH.sub.3 to the total area of the peaks assignable to SiH.sub.1 and SiH.sub.2 is in the range from 0.15 to 0.45. An interlayer insulating film can be formed by coating a substrate with the coating solution, drying the coating layer and baking the dried coating layer at 300.degree. to 800.degree. C. in a moisturized atmosphere. The coating solution optionally contains a trialkyl amine compound as an agent to reduce sublimation of the low molecular weight fractions of the polysilazane compound. The reaction of the trialkyl amine and the polysilazane molecules is completed by keeping the coating layer before drying at a temperature of 25.degree. to 100.degree. C. for at least 1 minute.
摘要翻译：提出了在制造具有优异的储存稳定性和涂布加工性的各种电子器件的情况下，形成二氧化硅层间绝缘膜的涂布溶液。溶剂优选为二烷基醚的涂布溶液的主要成分是用三甲基甲硅烷基化剂如六甲基二硅氮烷改性的聚硅氮烷化合物，使得在1 H-NMR光谱图中，面积比可分配给SiH 3的峰值与可分配给SiH 1和SiH 2的峰的总面积在0.15至0.45的范围内。层间绝缘膜可以通过用涂布溶液涂覆基材，干燥涂层并在300℃至800℃下在保湿的气氛中烘烤干燥的涂层而形成。涂布溶液任选地含有三烷基胺化合物作为用于降低聚硅氮烷化合物的低分子量级分的升华的试剂。三烷基胺和聚硅氮烷分子的反应通过在25℃至100℃的温度下保持涂层保持至少1分钟来完成。

5. 发明授权

US07135064B2 Silica-based coating film on substrate and coating solution therefor 有权
标题翻译：二氧化硅基涂料及其涂料溶液
公开(公告)号：US07135064B2
公开(公告)日：2006-11-14
申请号：US11067622
申请日：2005-02-28
申请人： Tatsuhiko Shibuya , Yoshio Hagiwara
发明人： Tatsuhiko Shibuya , Yoshio Hagiwara
IPC分类号： C09D183/06
CPC分类号： H01L21/31051 , C08G77/02 , C08G77/06 , C08G77/32 , C09D183/02 , C09D183/04 , H01L21/02126 , H01L21/02216 , H01L21/02282 , H01L21/3122 , H01L21/316 , Y10T428/31663
摘要： A silica-based coating film having a low dielectric constant not exceeding 2.5 can be formed on the surface of a substrate to serve as a planarizing layer or an interlayer insulating layer by coating the surface with a unique coating solution containing a hydrolysis-condensation product of a polyalkoxy silane compound such as tetraethoxy silane and monomethyl trimethoxy silane, which is formed by the hydrolysis of a polyalkoxy silane in the presence of a basic catalyst such as ammonia in an alcohol solvent in a relatively low concentration followed by replacement of the alcohol solvent with an aprotic polar solvent such as N-methyl pyrrolidone, followed by drying and baking at 350 to 800° C.
摘要翻译：可以在基板的表面上形成具有低于2.5的低介电常数的二氧化硅基涂膜，以作为平面化层或层间绝缘层，通过用含有水解缩合产物聚烷氧基硅烷化合物，例如四乙氧基硅烷和单甲基三甲氧基硅烷，其通过在碱性催化剂如氨的存在下在醇溶剂中以相对低的浓度水解而形成，随后用醇溶剂置换，非质子极性溶剂如N-甲基吡咯烷酮，然后在350至800℃下干燥和烘烤。

6. 发明授权

US06875262B1 Silica-based coating film on substrate and coating solution therefor 有权
标题翻译：二氧化硅基涂料及其涂料溶液
公开(公告)号：US06875262B1
公开(公告)日：2005-04-05
申请号：US09302471
申请日：1999-04-30
申请人： Tatsuhiko Shibuya , Yoshio Hagiwara
发明人： Tatsuhiko Shibuya , Yoshio Hagiwara
IPC分类号： B32B25/20 , C08G77/02 , C08G77/06 , C08G77/32 , C09D183/02 , C09D183/04 , H01B1/00 , H01B3/00 , H01L21/3105 , H01L21/312 , H01L21/316 , H01I21/00
CPC分类号： H01L21/31051 , C08G77/02 , C08G77/06 , C08G77/32 , C09D183/02 , C09D183/04 , H01L21/02126 , H01L21/02216 , H01L21/02282 , H01L21/3122 , H01L21/316 , Y10T428/31663
摘要： A silica-based coating film having a low dielectric constant not exceeding 2.5 can be formed on the surface of a substrate to serve as a planarizing layer or an interlayer insulating layer by coating the surface with a unique coating solution containing a hydrolysis-condensation product of a polyalkoxy silane compound such as tetraethoxy silane and monomethyl trimethoxy silane, which is formed by the hydrolysis of a polyalkoxy silane in the presence of a basic catalyst such as ammonia in an alcohol solvent in a relatively low concentration followed by replacement of the alcohol solvent with an aprotic polar solvent such as N-methyl pyrrolidone, followed by drying and baking at 350 to 800° C.
摘要翻译：可以在基板的表面上形成具有低于2.5的低介电常数的二氧化硅基涂膜，以作为平面化层或层间绝缘层，通过用含有水解缩合产物聚烷氧基硅烷化合物，例如四乙氧基硅烷和单甲基三甲氧基硅烷，其通过在碱性催化剂如氨的存在下在醇溶剂中以相对低的浓度水解而形成，随后用醇溶剂置换，非质子极性溶剂如N-甲基吡咯烷酮，然后在350至800℃下干燥和烘烤。

7. 发明申请

US20050147833A1 Silica-based coating film on substrate and coating solution therefor 有权
公开(公告)号：US20050147833A1
公开(公告)日：2005-07-07
申请号：US11067622
申请日：2005-02-28
申请人： Tatsuhiko Shibuya , Yoshio Hagiwara
发明人： Tatsuhiko Shibuya , Yoshio Hagiwara
IPC分类号： B32B25/20 , C08G77/02 , C08G77/06 , C08G77/32 , C09D183/02 , C09D183/04 , H01B1/00 , H01B3/00 , H01L21/3105 , H01L21/312 , H01L21/316
CPC分类号： H01L21/31051 , C08G77/02 , C08G77/06 , C08G77/32 , C09D183/02 , C09D183/04 , H01L21/02126 , H01L21/02216 , H01L21/02282 , H01L21/3122 , H01L21/316 , Y10T428/31663
摘要： A silica-based coating film having a low dielectric constant not exceeding 2.5 can be formed on the surface of a substrate to serve as a planarizing layer or an interlayer insulating layer by coating the surface with a unique coating solution containing a hydrolysis-condensation product of a polyalkoxy silane compound such as tetraethoxy silane and monomethyl trimethoxy silane, which is formed by the hydrolysis of a polyalkoxy silane in the presence of a basic catalyst such as ammonia in an alcohol solvent in a relatively low concentration followed by replacement of the alcohol solvent with an aprotic polar solvent such as N-methyl pyrrolidone, followed by drying and baking at 350 to 800° C.

8. 发明授权

US06190788B1 Method for the formation of a siliceous coating film 失效
标题翻译：形成硅质涂膜的方法
公开(公告)号：US06190788B1
公开(公告)日：2001-02-20
申请号：US09327558
申请日：1999-06-08
申请人： Tatsuhiko Shibuya , Yoshio Hagiwara
发明人： Tatsuhiko Shibuya , Yoshio Hagiwara
IPC分类号： B21D3900
CPC分类号： H01L21/3125 , C09D183/16 , C23C18/1212 , C23C18/122 , C23C18/1283 , H01L21/02126 , H01L21/02164 , H01L21/02222 , H01L21/02282 , H01L21/02337 , Y10T428/12556
摘要： Disclosed is a method for the formation of a silica coating film having a remarkably high crack-forming thickness limit on the surface of a substrate which may be highly heat resistant, for example, having a circuit wiring layer of polycrystalline silicon to withstand a temperature higher than 500° C. without excessive diffusion of dopant through the source layer or drain layer of the semiconductor device. The method comprises the steps of: coating the substrate surface with a coating solution containing a modified polysilazane which is a reaction product of a polysilazane and a dialkyl alkanol amine, drying the coating layer, subjecting the coating layer to a first baking treatment at 350-450° C. for 10-60 minutes and subjecting the layer to a second baking treatment at 550-800° C. for 0.5-60 minutes.
摘要翻译：公开了一种形成二氧化硅涂膜的方法，该二氧化硅涂膜在基板的表面上具有非常高的耐龟裂性的极高的耐热性，例如具有多晶硅的电路布线层以承受更高的温度超过500℃，没有掺杂剂过度扩散通过半导体器件的源极层或漏极层。该方法包括以下步骤：用含有聚硅氮烷（聚硅氮烷和二烷基链烷醇胺的反应产物）的改性聚硅氮烷的涂布溶液涂布基材表面，干燥该涂层，在350℃下进行第一次烘烤处理， 450℃10-60分钟，并在550-800℃下对该层进行第二次烘烤处理0.5-60分钟。

9. 发明授权

US06338868B1 Method for the formation of a siliceous coating film 有权
标题翻译：形成硅质涂膜的方法
公开(公告)号：US06338868B1
公开(公告)日：2002-01-15
申请号：US09733948
申请日：2000-12-12
申请人： Tatsuhiko Shibuya , Yoshio Hagiwara
发明人： Tatsuhiko Shibuya , Yoshio Hagiwara
IPC分类号： B05D302
CPC分类号： H01L21/3125 , C09D183/16 , C23C18/1212 , C23C18/122 , C23C18/1283 , H01L21/02126 , H01L21/02164 , H01L21/02222 , H01L21/02282 , H01L21/02337 , Y10T428/12556
摘要： Disclosed is a method for the formation of a silica coating film having a remarkably high crack-forming thickness limit on the surface of a substrate which may be highly heat resistant, for example, having a circuit wiring layer of polycrystalline silicon to withstand a temperature higher than 500° C. without excessive diffusion of dopant through the source layer or drain layer of the semiconductor device. The method comprises the steps of: coating the substrate surface with a coating solution containing a modified polysilazane which is a reaction product of a polysilazane and a dialkyl alkanol amine, drying the coating layer, subjecting the coating layer to a first baking treatment at 350-450° C. for 10-60 minutes and subjecting the layer to a second baking treatment at 550-800° C. for 0.5-60 minutes.
摘要翻译：公开了一种形成二氧化硅涂膜的方法，该二氧化硅涂膜在基板的表面上具有非常高的耐龟裂性的极高的耐热性，例如具有多晶硅的电路布线层以承受更高的温度超过500℃，没有掺杂剂过度扩散通过半导体器件的源极层或漏极层。该方法包括以下步骤：用含有聚硅氮烷（聚硅氮烷和二烷基链烷醇胺的反应产物）的改性聚硅氮烷的涂布溶液涂布基材表面，干燥该涂层，在350℃下进行第一次烘烤处理， 450℃10-60分钟，并在550-800℃下对该层进行第二次烘烤处理0.5-60分钟。

10. 发明授权

US5614271A Method for the formation of a silica-based coating film 失效
标题翻译：形成二氧化硅基涂膜的方法
公开(公告)号：US5614271A
公开(公告)日：1997-03-25
申请号：US692187
申请日：1996-08-05
申请人： Tatsuhiko Shibuya , Susumu Okano , Hideya Kobari , Yoshio Hagiwara , Toshimasa Nakayama
发明人： Tatsuhiko Shibuya , Susumu Okano , Hideya Kobari , Yoshio Hagiwara , Toshimasa Nakayama
IPC分类号： B05D3/06 , B05D7/00 , B05D7/24 , C04B41/50 , C09D183/00 , C09D183/16 , C23C18/12 , C23C18/14 , H01L21/316 , B29C71/02
CPC分类号： H01L21/316 , C04B41/5035 , C09D183/16 , C23C18/1212 , C23C18/122 , C23C18/1279 , C23C18/1283 , C23C18/1295 , C23C18/14 , C04B2111/00844
摘要： Proposed is an improved method for the formation of a silica-based coating film on the surface of a substrate such as a silicon wafer in the manufacture of semiconductor devices by coating the substrate surface with a polysilazane-containing coating solution followed by conversion of the coating layer of polysilazane into a silica-based coating film. The method comprises drying the coating layer of the polysilazane according to a heating schedule at a specified heating rate with continuous or stepwise increase of the temperature up to 240.degree. to 350.degree. C. followed by an irradiation treatment with far ultraviolet light at a temperature of 240.degree. to 350.degree. C. and then by a baking treatment at 350.degree. to 800.degree. C.
摘要翻译：提出了在半导体器件的制造中在硅晶片等基板的表面上形成二氧化硅类涂膜的改进方法，其中通过用含聚硅氮烷的涂布溶液涂布基板表面，随后将涂层转化聚硅氮烷层形成二氧化硅基涂膜。该方法包括以规定的加热速度按照加热方案干燥聚硅氮烷的涂层，连续或逐步升高温度至240℃至350℃，然后在远紫外光的温度下进行辐射处理 240℃至350℃，然后在350℃至800℃下进行烘烤处理。

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