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1. 发明授权

US06645878B2 Low volatility solvent-based method for forming thin film nanoporous aerogels on semiconductor substrates 有权
公开(公告)号：US06645878B2
公开(公告)日：2003-11-11
申请号：US10135212
申请日：2002-04-30
申请人： Douglas M. Smith , Gregory P. Johnston , William C. Ackerman , Richard A. Stoltz , Alok Maskara , Teresa Ramos , Shin-Puu Jeng , Bruce E. Gnade
发明人： Douglas M. Smith , Gregory P. Johnston , William C. Ackerman , Richard A. Stoltz , Alok Maskara , Teresa Ramos , Shin-Puu Jeng , Bruce E. Gnade
IPC分类号： H01L2131
CPC分类号： H01L21/31695 , B01J13/0091 , H01L21/02203 , H01L21/02214 , H01L21/02282 , H01L21/3105
摘要： This invention has enabled a new, simple thin film nanoporous dielectric fabrication method. In general, this invention uses glycerol, or another low volatility compound, as a solvent. This new method allows thin film aerogels/low density xerogels to be made without supercritical drying, freeze drying, or a surface modification step before drying. Thus, this invention allows production of nanoporous dielectrics at room temperature and atmospheric pressure, without a separate surface modification step. 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. This invention allows controlled porosity thin film nanoporous aerogels to be deposited, gelled, aged, and dried without atmospheric controls. In another aspect, this invention allows controlled porosity thin film nanoporous aerogels to be deposited, gelled, rapidly aged at an elevated temperature, and dried with only passive atmospheric controls, such as limiting the volume of the aging chamber.

2. 发明授权

US06319852B1 Nanoporous dielectric thin film formation using a post-deposition catalyst 有权
标题翻译：使用后沉积催化剂形成纳米孔隙介电薄膜
公开(公告)号：US06319852B1
公开(公告)日：2001-11-20
申请号：US09488185
申请日：2000-01-20
申请人： Douglas M. Smith , Gregory P. Johnston , William C. Ackerman , Shin-Puu Jeng
发明人： Douglas M. Smith , Gregory P. Johnston , William C. Ackerman , Shin-Puu Jeng
IPC分类号： H01L2131
CPC分类号： C01B33/158 , C01B33/145 , C01B33/155 , H01L21/02126 , H01L21/02203 , H01L21/02216 , H01L21/02282 , H01L21/02337 , H01L21/02343 , H01L21/02359 , H01L21/3122 , H01L21/31695 , H01L21/7682 , H01L2221/1047
摘要： This pertains generally to precursors and deposition methods suited to aerogel thin film fabrication of nanoporous dielectrics. An aerogel precursor sol is disclosed. This aerogel precursor sol contains a metal alkoxide (such as TEOS) and a solvent, but no gelation catalyst. By a method according to the present invention, such a precursor sol is applied as a nongelling thin film 14 to a semiconductor substrate 10. This substrate may contain patterned conductors 12, gaps 13, or other structures. An independent gelation catalyst (preferably, vapor phase ammonia) is added to promote rapid gelation of the thin film sol 14 at the desired time. One advantage is that it allows substantially independent control of gelation and pore fluid evaporation. This independent catalyst introduction allows additional processing steps to be performed between sol deposition and the onset of substantial gelation. One potential step is to evaporate a portion of the pore fluid solvent. Additional advantages of independent catalyst introduction are that it reduces the need for process steps requiring critical timing and provides a large increase in the pot life of the precursor sol.
摘要翻译：这通常涉及适用于纳米多孔电介质的气凝胶薄膜制造的前体和沉积方法。公开了一种气凝胶前体溶胶。该气凝胶前体溶胶含有金属醇盐（如TEOS）和溶剂，但不含凝胶化催化剂。通过根据本发明的方法，这种前体溶胶作为不合格薄膜14施加到半导体衬底10.该衬底可以包含图案化导体12，间隙13或其它结构。加入独立的凝胶化催化剂（优选气相氨）以促进薄膜溶胶14在所需时间的快速凝胶化。一个优点是它可以实质上独立地控制凝胶化和孔隙流体蒸发。这种独立的催化剂引入允许在溶胶沉积和实质凝胶化的开始之间进行额外的加工步骤。一个潜在的步骤是蒸发一部分孔隙流体溶剂。独立催化剂引入的另外的优点是减少了对需要临界时间的工艺步骤的需要，并且提供前体溶胶的适用期的大量增加。

3. 发明授权

US5753305A Rapid aging technique for aerogel thin films 失效
标题翻译：气凝胶薄膜快速老化技术
公开(公告)号：US5753305A
公开(公告)日：1998-05-19
申请号：US748922
申请日：1996-11-14
申请人： Douglas M. Smith , Gregory P. Johnston , William C. Ackerman , Shin-Puu Jeng
发明人： Douglas M. Smith , Gregory P. Johnston , William C. Ackerman , Shin-Puu Jeng
IPC分类号： B01J13/00 , C01B33/158 , H01L21/314 , H01L21/316 , H01L21/768 , B05D3/04 , B05D3/00 , B05D5/00 , H01L21/00
CPC分类号： H01L21/02126 , B01J13/0091 , C01B33/1585 , H01L21/02203 , H01L21/02216 , H01L21/02282 , H01L21/02337 , H01L21/31695 , H01L21/7682 , H01L2221/1047 , Y10S438/909
摘要： This invention pertains generally to aging methods suited to aerogel thin film fabrication, and particularly to techniques for improving gel strength and/or aerogel dielectric constant by a rapid aging technique, which avoid damage or premature drying of wet gel thin films during aging. A substrate having a wet gel thin film deposited thereon is contacted with a saturated water vapor atmosphere, preferably at an elevated pressure and a temperature greater than 100.degree. C. The method may comprise a vapor-phase exchange step to remove low boiling point pore liquids such as ethanol prior to or during aging. The method may also comprise a vapor-phase exchange step to replace water in the wet gel with another pore liquid such as acetone to stop the aging process and prepare the wet gel for drying. A vapor-phase aging catalyst (e.g. ammonia) may also be used to enhance the aging process. The present invention allows aging of wet gel thin films to be completed in a few minutes instead of the days generally required for conventional bulk gel aging.
摘要翻译：本发明一般涉及适用于气凝胶薄膜制造的老化方法，特别涉及通过快速老化技术改进凝胶强度和/或气凝胶介电常数的技术，其避免了老化期间湿凝胶薄膜的损坏或过早干燥。将其上沉积有湿凝胶薄膜的基底与饱和水蒸汽气氛接触，优选在升高的压力和大于100℃的温度下进行。该方法可以包括气相交换步骤以除去低沸点孔隙液体例如在老化之前或期间的乙醇。该方法还可以包括气相交换步骤，以用另一种孔液体如丙酮代替湿凝胶中的水，以停止老化过程并制备湿凝胶进行干燥。气相老化催化剂（例如氨）也可用于增强老化过程。本发明允许在几分钟内完成湿凝胶薄膜的老化，而不是常规体积凝胶老化通常需要的时间。

4. 发明授权

US5736425A Glycol-based method for forming a thin-film nanoporous dielectric 失效
标题翻译：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
申请人： Douglas M. Smith , William C. Ackerman
发明人： Douglas M. Smith , William C. Ackerman
IPC分类号： B01J13/00 , C01B33/158 , C03C1/00 , C03C17/25 , H01L21/314 , H01L21/316 , H01L21/00
CPC分类号： H01L21/02126 , B01J13/0091 , C01B33/1585 , C03C1/008 , C03C17/25 , H01L21/02203 , H01L21/02216 , H01L21/02282 , H01L21/02337 , H01L21/31695 , C03C2217/213 , C03C2218/113
摘要： 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.
摘要翻译：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。

5. 发明授权

US5847443A Porous dielectric material with improved pore surface properties for electronics applications 失效
公开(公告)号：US5847443A
公开(公告)日：1998-12-08
申请号：US746689
申请日：1996-11-14
申请人： Chi-Chen Cho , Bruce E. Gnade , Douglas M. Smith , Jin Changming , William C. Ackerman , Gregory C. Johnston
发明人： Chi-Chen Cho , Bruce E. Gnade , Douglas M. Smith , Jin Changming , William C. Ackerman , Gregory C. Johnston
IPC分类号： H01L21/768 , H01L21/316 , H01L21/469 , H01L23/522 , H01L23/532 , H01L23/58
CPC分类号： H01L23/5329 , H01L21/7682 , H01L23/5222 , H01L2221/1047 , H01L2924/0002
摘要： This invention provides an improved porous structure for semiconductor devices and a process for making the same. This process may be applied to an existing porous structure 28, which may be deposited, for example, between patterned conductors 24. The method may comprise providing a substrate comprising a microelectronic circuit and a porous silica layer, the porous silica layer having an average pore diameter between 2 and 80 nm; and heating the substrate to one or more temperatures between 100 and 490 degrees C. in a substantially halogen-free atmosphere, whereby one or more dielectric properties of the porous dielectric are improved. In some embodiments, the atmosphere comprises a phenyl-containing atmosphere, such as hexaphenyldisilazane. In some embodiments, the method further comprises cooling the substrate and exposing the substrate to a substantially halogen-free atmosphere comprising either a phenyl-containing compound, such as hexaphenyldisilazane; or a methyl-containing compound, such as hexamethyldisilazane. It has been found that a porous structure treated in such a manner generally exhibits improved dielectric properties relative to an untreated sample.

6. 发明授权

US5807607A Polyol-based method for forming thin film aerogels on semiconductor substrates 失效
标题翻译：用于在半导体衬底上形成薄膜气凝胶的基于多元醇的方法
公开(公告)号：US5807607A
公开(公告)日：1998-09-15
申请号：US748926
申请日：1996-11-14
申请人： Douglas M. Smith , William C. Ackerman , Richard A. Stoltz
发明人： Douglas M. Smith , William C. Ackerman , Richard A. Stoltz
IPC分类号： B05D3/02 , H01L21/31 , H01L21/316 , H01L21/469 , B05D5/12 , H01L21/00
CPC分类号： H01L21/02126 , H01L21/02203 , H01L21/02216 , H01L21/02282 , H01L21/02337 , H01L21/02343 , H01L21/02359 , H01L21/31695
摘要： This invention has enabled a new, simple nanoporous dielectric fabrication method. In general, this invention uses a polyol, such as glycerol, 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.
摘要翻译：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，本发明使用多元醇如甘油作为溶剂。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。

7. 发明授权

US06380105B1 Low volatility solvent-based method for forming thin film nanoporous aerogels on semiconductor substrates 有权
标题翻译：在半导体衬底上形成薄膜纳米多孔气凝胶的低挥发性溶剂型方法
公开(公告)号：US06380105B1
公开(公告)日：2002-04-30
申请号：US09324370
申请日：1999-06-02
申请人： Douglas M. Smith , Gregory P. Johnston , William C. Ackerman , Richard A. Stoltz , Alok Maskara , Teresa Ramos , Shin-Puu Jeng , Bruce E. Gnade
发明人： Douglas M. Smith , Gregory P. Johnston , William C. Ackerman , Richard A. Stoltz , Alok Maskara , Teresa Ramos , Shin-Puu Jeng , Bruce E. Gnade
IPC分类号： H01L2131
CPC分类号： H01L21/31695 , B01J13/0091 , H01L21/02203 , H01L21/02214 , H01L21/02282 , H01L21/3105
摘要： This invention has enabled a new, simple thin film nanoporous dielectric fabrication method. In general, this invention uses glycerol, or another low volatility compound, as a solvent. This new method allows thin film aerogels/low density xerogels to be made without supercritical drying, freeze drying, or a surface modification step before drying. Thus, this invention allows production of nanoporous dielectrics at room temperature and atmospheric pressure, without a separate surface modification step. 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. This invention allows controlled porosity thin film nanoporous aerogels to be deposited, gelled, aged, and dried without atmospheric controls. In another aspect, this invention allows controlled porosity thin film nanoporous aerogels to be deposited, gelled, rapidly aged at an elevated temperature, and dried with only passive atmospheric controls, such as limiting the volume of the aging chamber.
摘要翻译：本发明实现了一种新的，简单的薄膜纳米多孔电介质制造方法。通常，本发明使用甘油或另一种低挥发性化合物作为溶剂。这种新方法允许在干燥之前不进行超临界干燥，冷冻干燥或表面改性步骤制备薄膜气凝胶/低密度干凝胶。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。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。本发明允许控制孔隙率薄膜纳米多孔气凝胶沉积，凝胶化，老化和干燥而无需大气控制。另一方面，本发明允许受控孔隙率的薄膜纳米多孔气凝胶沉积，凝胶化，在升高的温度下快速老化，并且仅用无源大气控制干燥，例如限制老化室的体积。

8. 发明授权

US06315971B1 Process for producing low density gel compositions 失效
标题翻译：生产低密度凝胶组合物的方法
公开(公告)号：US06315971B1
公开(公告)日：2001-11-13
申请号：US08826979
申请日：1997-04-09
申请人： Stephen Wallace , Douglas M. Smith , William C. Ackerman
发明人： Stephen Wallace , Douglas M. Smith , William C. Ackerman
IPC分类号： C01B33158
CPC分类号： B01J13/0056 , B01J13/0091
摘要： Disclosed are processes for producing gel composition which may be utilized to produce low density gel compositions without the need for supercritical drying, thermal treatment or surface treatment. The processes comprise drying a wet gel comprising gel solids and a drying agent to remove the drying agent while minimizing shrinkage of the gel during drying.
摘要翻译：公开了可用于生产低密度凝胶组合物而不需要超临界干燥，热处理或表面处理的凝胶组合物的方法。该方法包括干燥包含凝胶固体和干燥剂的湿凝胶以除去干燥剂，同时使干燥期间凝胶的收缩最小化。

9. 发明授权

US6130152A Aerogel thin film formation from multi-solvent systems 失效
标题翻译：从多溶剂系统形成气凝胶薄膜
公开(公告)号：US6130152A
公开(公告)日：2000-10-10
申请号：US746679
申请日：1996-11-14
申请人： Douglas M. Smith , Gregory P. Johnston , William C. Ackerman , Shin-Puu Jeng , Bruce E. Gnade
发明人： Douglas M. Smith , Gregory P. Johnston , William C. Ackerman , Shin-Puu Jeng , Bruce E. Gnade
IPC分类号： B01F3/12 , C01B33/14 , C01B33/145 , C01B33/155 , C01B33/158 , H01L21/312 , H01L21/316 , H01L21/768
CPC分类号： C01B33/158 , C01B33/145 , C01B33/155 , H01L21/02126 , H01L21/02216 , H01L21/02282 , H01L21/3122 , H01L21/7682 , H01L21/31695
摘要： This invention pertains generally to precursors and deposition methods suited to aerogel thin film fabrication. An aerogel precursor sol which contains an oligomerized metal alkoxide (such as TEOS), a high vapor pressure solvent (such as ethanol) and a low vapor pressure solvent (such as water and 1-butanol) is disclosed. By a method according to the present invention, such a precursor sol is applied as a thin film to a semiconductor wafer, and the high vapor pressure solvent is allowed to evaporate while evaporation of the low vapor pressure solvent is limited, preferably by controlling the atmosphere adjacent to the wafer. The reduced sol is then allowed to gel at a concentration determined by the ratio of metal.alkoxide to low vapor pressure solvent. One advantage of the present invention is that it provides a stable, spinnable sol for setting film thickness and providing good planarity and gap fill for patterned wafers. In addition, however, the reduced sol may be gelled rapidly from a known sol concentration keyed to the desired final density of the aerogel thin film and largely independent of film thickness and spin conditions.
摘要翻译：本发明一般涉及适用于气凝胶薄膜制造的前体和沉积方法。公开了含有低聚金属醇盐（如TEOS），高蒸气压溶剂（如乙醇）和低蒸气压溶剂（如水和1-丁醇））的气凝胶前体溶胶。通过根据本发明的方法，将这种前体溶胶作为薄膜施加到半导体晶片，并且在蒸发低蒸气压溶剂的同时，优选通过控制气氛，使高蒸气压溶剂蒸发邻近晶片。然后将还原的溶胶以由金属醇盐与低蒸气压溶剂的比例确定的浓度凝胶化。本发明的一个优点是提供了一种稳定的可纺丝溶胶，用于设定膜厚度并为图案化晶片提供良好的平面度和间隙填充。然而，此外，还原的溶胶可以从已知的溶胶浓度快速凝胶化，所述溶胶浓度与气凝胶薄膜的所需最终密度密切相关，并且在很大程度上与膜厚度和旋转条件无关。

10. 发明授权

US6107350A Gel compositions 失效
标题翻译：凝胶组合物
公开(公告)号：US6107350A
公开(公告)日：2000-08-22
申请号：US907722
申请日：1997-08-08
申请人： Ralph Ulrich Boes , James A. Belmont , David J. Kaul , Douglas M. Smith , William C. Ackerman
发明人： Ralph Ulrich Boes , James A. Belmont , David J. Kaul , Douglas M. Smith , William C. Ackerman
IPC分类号： C01B31/02 , B01D69/14 , B01D71/02 , B01J13/00 , B01J20/10 , B01J20/20 , B01J20/32 , B01J21/18 , C04B30/00 , C08K3/04 , C08L61/08 , C08L61/12 , C08L61/28 , C09C1/56 , C09D17/00 , C09K3/00 , F02B77/13 , C01B33/14
CPC分类号： C09K3/00 , B01D69/141 , B01D71/021 , B01J20/06 , B01J20/08 , B01J20/103 , B01J20/20 , B01J20/28047 , B01J20/3204 , B01J20/324 , B01J20/3248 , B01J20/3251 , B01J20/3253 , B01J21/18 , C04B30/00 , C09C1/56 , C09D17/005 , F02B77/13 , B01J2220/42 , B01J2220/46 , C01P2004/03 , C01P2006/10
摘要： New gel conpositions which comprise a carbonaceous component attached to a gel component. Preferably, the corbonaceous component is selected from the group consisting of: carbon blacks, carbon fibers, activated carbons and graphitic carbons; and the gel component is selected from the group consisting of: metal oxide gels and polymeric gels. Also disclosed are new gel composition comprising: a gel component and a carbon black product having attached at least one organic group, the organic group comprising: a) at least one aromatic group, and b) at least one ionic group, at least one ionizable group, or a mixture of an ionic group and an ionizable group, wherein at least one aromatic group of the organic group is directly attached to the carbon black. Further disclosed are new gel compositon comprising: a gel component and a carbon black product having attached at least one organic group, the organic group comprising: a) at least one C.sub.1 -C.sub.12 alkyl group, and b) at least one ionic group, at least one ionizable group, or a mixture of an ionic group and an ionizable group, wherein at least one alkyl group of the organic group is directly attached to the carbon black. Uses for the gel compositions are also disclosed.
摘要翻译：包含附着在凝胶组分上的碳质组分的新凝胶结构。优选地，该碳质组分选自：炭黑，碳纤维，活性炭和石墨碳; 并且凝胶组分选自：金属氧化物凝胶和聚合物凝胶。还公开了新的凝胶组合物，其包含：凝胶组分和具有连接至少一个有机基团的炭黑产物，所述有机基团包含：a）至少一个芳族基团，和b）至少一个离子基团，至少一个可离子化的基团或离子基团和可离子化基团的混合物，其中至少一个有机基团的芳族基团直接连接到炭黑上。进一步公开的是新的凝胶组合物，其包含：凝胶组分和具有连接至少一个有机基团的炭黑产物，所述有机基团包含：a）至少一个C 1 -C 12烷基和b）至少一个离子基团，至少一个可离子化基团，或离子基团和可离子化基团的混合物，其中至少一个有机基团的烷基直接附着在炭黑上。还公开了用于凝胶组合物的用途。

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