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    Process for producing low density gel compositions
    1.
    发明授权
    Process for producing low density gel compositions 失效
    生产低密度凝胶组合物的方法

    公开(公告)号：US06172120B2

    公开(公告)日：2001-01-09

    申请号：US08826982

    申请日：1997-04-09

    申请人： Douglas M. Smith ,  William C. Ackerman ,  Stephen Wallace ,  Elsbeth R. Lokey

    发明人： Douglas M. Smith ,  William C. Ackerman ,  Stephen Wallace ,  Elsbeth R. Lokey

    IPC分类号： B01J1300

    CPC分类号： B01J13/0052 ,  B01J13/0091

    摘要： Processes for producing gel compositions comprising: esterifying a portion of the surface of a gel composition sufficient to produce a gel composition having a rod density of less than or equal to 0.15 g/cc, and/or a tap density of less than or equal to 0.2 g/cc through contact with at least one esterification agent and at least one catalyst. The processes may be utilized to produce low density gel compositions without the need for a supercritical drying step or thermal treatment.

    摘要翻译： 用于生产凝胶组合物的方法，包括：将足以产生棒密度小于或等于0.15g / cc的凝胶组合物的一部分表面凝胶化，和/或振实密度小于或等于 通过与至少一种酯化剂和至少一种催化剂接触来制备0.2g / cc。 该方法可用于生产低密度凝胶组合物，而不需要超临界干燥步骤或热处理。

    Process for producing low density gel compositions
    3.
    发明授权
    Process for producing low density gel compositions 失效
    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。

    Nanoporous dielectric thin film formation using a post-deposition catalyst
    6.
    发明授权
    Nanoporous dielectric thin film formation using a post-deposition catalyst 有权
    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。

    Rapid aging technique for aerogel thin films
    7.
    发明授权
    Rapid aging technique for aerogel thin films 失效
    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。

    Glycol-based method for forming a thin-film nanoporous dielectric
    8.
    发明授权
    Glycol-based method for forming a thin-film nanoporous dielectric 失效
    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。

    Nanoporous dielectric thin film surface modification
    9.
    发明授权
    Nanoporous dielectric thin film surface modification 失效
    纳米介电薄膜表面改性

    公开(公告)号：US6063714A

    公开(公告)日：2000-05-16

    申请号：US749186

    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： H01L21/314 ,  H01L21/316 ,  H01L21/768 ,  H01L21/00 ,  B05D3/04

    CPC分类号： H01L21/02126 ,  H01L21/02203 ,  H01L21/02216 ,  H01L21/02282 ,  H01L21/02337 ,  H01L21/02343 ,  H01L21/31695 ,  H01L21/76801

    摘要： This pertains generally to precursors and deposition methods suited to aerogel thin film fabrication of nanoporous dielectrics. A method of forming a nanoporous dielectric on a semiconductor substrate is disclosed. By a method according to the present invention, 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, and/or other structures. A portion of the solvent is evaporated from the thin film 14 to produce a reduced thickness film 18. Film 18 is gelled and may be aged. A surface modification agent is introduced to the reaction atmosphere in a vaporish form, e.g., a vapor, mist, aerosol, or similar form. The surface modifier can then diffuse into, condense onto, and/or settle onto the wet gel and then diffuse throughout the thin film. This vaporish introduction of the surface modification agent ensures that there are no strong fluid flows across the wafer that might damage the wet gel. It can also be compatible with standard processing equipment and can potentially be used with other reaction atmosphere controls that reduce premature drying of the gel.

    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。 公开了一种在半导体衬底上形成纳米多孔电介质的方法。 通过根据本发明的方法，将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和/或其它结构。 溶剂的一部分从薄膜14蒸发以产生厚度减薄的薄膜18.薄膜18胶凝并且可以老化。 将表面改性剂以蒸气形式，例如蒸汽，雾，气溶胶或类似形式引入反应气氛中。 然后，表面改性剂可以扩散进入，冷凝到和/或沉降到湿凝胶上，然后在整个薄膜中扩散。 表面改性剂的蒸发引入确保了晶片上没有强大的流体流动，这可能会损坏湿凝胶。 它也可以与标准的加工设备兼容，并且可以与其他反应气氛控制器一起使用，以减少凝胶的过早干燥。

    Low volatility solvent-based method for forming thin film nanoporous aerogels on semiconductor substrates
    10.
    发明授权
    Low volatility solvent-based method for forming thin film nanoporous aerogels on semiconductor substrates 有权
    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。