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    • 1. 发明授权
    • Method and apparatus for drying wet porous bodies under subcritical
temperatures and pressures
    • 在亚临界温度和压力下干燥湿多孔体的方法和设备
    • US5875564A
    • 1999-03-02
    • US914433
    • 1997-08-19
    • Fikret KirkbirSatyabrata RaychaudhuriDouglas MeyersHideaki Murata
    • Fikret KirkbirSatyabrata RaychaudhuriDouglas MeyersHideaki Murata
    • F26B5/16F26B7/00F26B21/00F26B21/14F26B25/00F26B5/06
    • F26B25/006F26B21/14F26B7/00
    • An improved apparatus, and related method of operation, is described for rapidly drying large monoliths of glass, ceramic and/or composite material, under subcritical conditions, while minimizing the risk of cracking the monolith during the drying process. The apparatus incorporates a pressure chamber for carrying the monolith to be dried, with no significant limitation on the size of the monolith relative to the size of the chamber. The monolith is initially immersed in a suitable drying solvent, and the temperature of the pressure chamber is raised to a predetermined value below the solvent's critical temperature, which raises the pressure to a predetermined value, likewise below the solvent's critical pressure. At a selected time during the drying process the pressure chamber is connected to a diffusion chamber, to draw away and condense solvent vapor. This drawing away of solvent vapor continues until the monolith is dry, at which time the pressure chamber is purged with an inert gas and then depressurized in a controlled manner. The apparatus thereby is configured to dry the monolith at an even lower subcritical pressure than previous apparatus of this kind, leading to increased safety and reduced operating expenses.
    • 描述了一种改进的装置和相关的操作方法,用于在亚临界条件下快速干燥玻璃,陶瓷和/或复合材料的大型整料,同时最小化在干燥过程中破裂整料的风险。 该装置包括用于承载要干燥的整料的压力室,相对于室的大小对整体体的尺寸没有明显的限制。 将整料首先浸入合适的干燥溶剂中,并将压力室的温度升高到低于溶剂临界温度的预定值,将该压力提高到预定值,同样低于溶剂的临界压力。 在干燥过程中的选定时间,压力室连接到扩散室,以抽出并冷凝溶剂蒸汽。 继续抽出溶剂蒸汽直到整料干燥,此时用惰性气体吹扫压力室,然后以受控的方式进行减压。 因此,该装置被配置成以比这种类型的先前装置更低的亚临界压力干燥整料,从而增加了安全性并降低了操作费用。
    • 2. 发明授权
    • Apparatus for drying wet porous bodies under subcritical temperatures
and pressures
    • 用于在亚临界温度和压力下干燥湿多孔体的装置
    • US5966832A
    • 1999-10-19
    • US257884
    • 1999-02-25
    • Fikret KirkbirSatyabrata RaychaudhuriDouglas MeyersHideaki Murata
    • Fikret KirkbirSatyabrata RaychaudhuriDouglas MeyersHideaki Murata
    • F26B5/16F26B7/00F26B21/00F26B21/14F26B25/00F26B21/06
    • F26B25/006F26B21/14F26B7/00
    • An improved apparatus, and related method of operation, is described for rapidly drying large monoliths of glass, ceramic and/or composite material, under subcritical conditions, while minimizing the risk of cracking the monolith during the drying process. The apparatus incorporates a pressure chamber for carrying the monolith to be dried, with no significant limitation on the size of the monolith relative to the size of the chamber. The monolith is initially immersed in a suitable drying solvent, and the temperature of the pressure chamber is raised to a predetermined value below the solvent's critical temperature, which raises the pressure to a predetermined value, likewise below the solvent's critical pressure. At a selected time during the drying process the pressure chamber is connected to a diffusion chamber, to draw away and condense solvent vapor. This drawing away of solvent vapor continues until the monolith is dry, at which time the pressure chamber is purged with an inert gas and then depressurized in a controlled manner. The apparatus thereby is configured to dry the monolith at an even lower subcritical pressure than previous apparatus of this kind, leading to increased safety and reduced operating expenses.
    • 描述了一种改进的装置和相关的操作方法,用于在亚临界条件下快速干燥玻璃,陶瓷和/或复合材料的大型整料,同时最小化在干燥过程中破裂整料的风险。 该装置包括用于承载要干燥的整料的压力室,相对于室的大小对整体体的尺寸没有明显的限制。 将整料首先浸入合适的干燥溶剂中,并将压力室的温度升高到低于溶剂临界温度的预定值,将该压力提高到预定值,同样低于溶剂的临界压力。 在干燥过程中的选定时间,压力室连接到扩散室,以抽出并冷凝溶剂蒸汽。 继续抽出溶剂蒸汽直到整料干燥,此时用惰性气体吹扫压力室,然后以受控的方式进行减压。 因此,该装置被配置成以比这种类型的先前装置更低的亚临界压力干燥整料,从而增加了安全性并降低了操作费用。
    • 3. 发明授权
    • Process for drying sol-gel derived porous bodies at elevated subcritical
temperatures and pressures
    • 在升高的亚临界温度和压力下干燥溶胶 - 凝胶衍生的多孔体的方法
    • US5473826A
    • 1995-12-12
    • US292878
    • 1994-08-19
    • Fikret KirkbirSatyabrata Raychaudhuri
    • Fikret KirkbirSatyabrata Raychaudhuri
    • F26B3/04B01J13/00C01B33/158C03B8/02C03B19/12C03C1/00C03C3/06F26B5/00F26B7/00F26B5/04
    • F26B5/005C03C1/006C03C3/06F26B7/00C03C2203/26
    • A process is disclosed for drying sol-gel derived porous wet bodies without inducing cracks therein. The wet gel preferably is immersed in a liquid solvent before being placed inside a drying chamber capable of withstanding relatively high pressures and temperatures. After the wet gel is loaded, the chamber is sealed from the outside environment, and then is heated from outside the chamber in a controlled manner until a prescribed subcritical pressure is reached. The final temperature and pressure are always lower than the critical temperature and pressure of the drying solvent. The solvent vapor is then evacuated from the chamber in a controlled fashion to decrease the pressure until ambient pressure is reached, while preferably maintaining the temperature inside the chamber at the prescribed level. Thereafter, the inside of the chamber is purged with an inert gas for a prescribed time period, after which the chamber is cooled to ambient temperature and the dry crack-free porous gel is removed. The resulting dry gels are crack-free and monolithic.
    • 公开了一种用于干燥溶胶 - 凝胶衍生的多孔湿体而不在其中引起裂纹的方法。 湿凝胶优选在放置在能够承受相对较高的压力和温度的干燥室内之前浸入液体溶剂中。 在加载湿凝胶之后,将室从外部环境密封,然后以受控的方式从室外加热直到达到规定的亚临界压力。 最终的温度和压力总是低于干燥溶剂的临界温度和压力。 然后以受控的方式将溶剂蒸气从室抽空,以降低压力,直到达到环境压力,同时优选将室内的温度保持在规定的水平。 此后,用惰性气体吹扫室内规定的时间,之后将该室冷却至环境温度,并且除去干燥的无裂纹的多孔凝胶。 得到的干凝胶是无裂纹和整体的。
    • 5. 发明授权
    • Sol-gel process for forming a germania-doped silica glass rod
    • 用于形成掺杂氧化锗的石英玻璃棒的溶胶 - 凝胶法
    • US5254508A
    • 1993-10-19
    • US806036
    • 1991-12-12
    • Fikret KirkbirSatyabrata Raychaudhuri
    • Fikret KirkbirSatyabrata Raychaudhuri
    • G02B6/00C03B8/02C03B19/12C03B37/016C03C3/04C03C13/04
    • C03C1/006C03B19/12C03B37/016C03B2201/31C03C2201/31C03C2203/26Y02P40/57
    • A sol-gel process for forming a germania-doped silica glass rod that is suitable for use as a preform in the manufacture of high numerical aperture optical fibers. The sol is produced by mixing together prescribed quantities of alkoxides including tetraethyl orthosilicate and tetraethyl orthogermanate, deionized water, ethanol and a precipitation catalyst such as hydrofluoric acid. Premature precipitation of germania is avoided by adding ethanol and deionized water to an alkoxide solution at a controlled, drop-wise rate and by then similarly adding the catalyst at a controlled, drop-wise rate. After drying the resulting gel, sintering is performed by chlorinating the dry gel to remove residual hydroxyl groups, then oxygenating the chlorinated gel to remove the chlorine, and finally heating the oxygenated gel in helium to a temperature of about 1300.degree. C. Chlorinating and oxygenating the gel for extended time durations, and maintaining the gel above 1200.degree. C. for less than 30 minutes, ensures that the final glass rod will not bubble when subsequently raised in temperature to 1800.degree. C. during the final fiber draw step.
    • 一种用于形成掺杂氧化锗的石英玻璃棒的溶胶 - 凝胶法,其适用于制造高数值孔径光纤中的预制棒。 将规定量的原硅酸四乙酯和原硅酸四乙酯,去离子水,乙醇和沉淀催化剂如氢氟酸混合在一起制成溶胶。 通过以受控的滴下速率向醇盐溶液中加入乙醇和去离子水,然后以受控的滴定速率类似地加入催化剂,可以避免锗酸盐的过早沉淀。 干燥所得凝胶后,通过氯化干燥凝胶以除去残留的羟基,然后对氯化凝胶进行氧化以除去氯,并最终将氦中的氧化凝胶加热至约1300℃的温度进行烧结。氯化和加氧 凝胶延长持续时间,并将凝胶保持在1200℃以上不足30分钟,确保最后的玻璃棒在最后纤维拉伸步骤中随后在温度升高至1800℃时不会起泡。
    • 7. 发明申请
    • Photomask assembly incorporating a metal/scavenger pellicle frame
    • 包含金属/清除剂防护薄膜框架的光掩模组件
    • US20060246234A1
    • 2006-11-02
    • US11407691
    • 2006-04-19
    • Douglas MeyersRahul GanguliTroy RobinsonRobert GumpSteven ColbernFikret Kirkbir
    • Douglas MeyersRahul GanguliTroy RobinsonRobert GumpSteven ColbernFikret Kirkbir
    • G03F1/14
    • G03F1/64G03F7/70933G03F7/70983Y10T428/24793Y10T428/3154Y10T428/31544
    • A photomask assembly is disclosed having a photomask substrate and a composite pellicle frame that includes both a metallic frame component and a scavenger component. The metallic frame component has a cross-sectional thickness of at least 100 micrometers in all directions, and the volume percentage of the scavenger component relative to the overall volume of the composite frame is in the range of 0.1 to 95%. The scavenger component has a gas permeability to oxygen or nitrogen greater than about 10 ml·mm/cm2·min·MPa, an average pore size between 0.001 and 10 micrometers, and a pore surface area greater than 10 m2/g. This configuration enables the pellicle frame to have sufficient strength to withstand stresses encountered during normal use, yet also to have the capability of scavenging impurity molecules from the space adjacent to the photomask substrate. In a separate and independent feature of the invention, the scavenger component comprises at least one metal oxide selected from the group consisting of oxides of aluminum, boron, cerium, cobalt, copper, erbium, hafnium, lanthanum, neodymium, praseodymium, scandium, silicon, titanium, yttrium, zirconium, and mixtures thereof. Preferably, the metal oxide is an oxide of zirconium, yttrium, or mixtures thereof.
    • 公开了一种光掩模组件,其具有光掩模基板和包括金属框架部件和清除部件的复合防护薄膜框架。 金属框架部件在所有方向上具有至少100微米的横截面厚度,并且清除剂部件相对于复合框架的总体积的体积百分比在0.1至95%的范围内。 清除剂组分对氧气或氮气的气体渗透性大于约10毫升/厘米3·秒/秒/秒·秒·分钟·MPa,平均孔径为0.001〜10微米,孔表面积大于 10微克/克。 这种构造使得防护薄膜框架具有足够的强度以承受在正常使用期间遇到的应力,而且还具有从邻近光掩模基板的空间中清除杂质分子的能力。 在本发明的独立和独立的特征中,清除剂组分包括选自铝,硼,铈,钴,铜,铒,铪,镧,钕,镨,钪,硅的氧化物中的至少一种金属氧化物 ,钛,钇,锆及其混合物。 优选地,金属氧化物是锆,钇或其混合物的氧化物。