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1. 发明授权

US06518539B2 Method for producing damage resistant optics 失效
公开(公告)号：US06518539B2
公开(公告)日：2003-02-11
申请号：US09948444
申请日：2001-09-07
申请人： Lloyd A. Hackel , Alan K. Burnham , Bernardino M. Penetrante , Raymond M. Brusasco , Paul J. Wegner , Lawrence W. Hrubesh , Mark R. Kozlowski , Michael D. Feit
发明人： Lloyd A. Hackel , Alan K. Burnham , Bernardino M. Penetrante , Raymond M. Brusasco , Paul J. Wegner , Lawrence W. Hrubesh , Mark R. Kozlowski , Michael D. Feit
IPC分类号： B23K2600
CPC分类号： C03C23/002 , C03C15/00 , C03C23/0025
摘要： The present invention provides a system that mitigates the growth of surface damage in an optic. Damage to the optic is minimally initiated. In an embodiment of the invention, damage sites in the optic are initiated, located, and then treated to stop the growth of the damage sites. The step of initiating damage sites in the optic includes a scan of the optic using a laser to initiate defects. The exact positions of the initiated sites are identified. A mitigation process is performed that locally or globally removes the cause of subsequent growth of the damaged sites.

2. 发明授权

US07211605B2 Super-hydrophobic fluorine containing aerogels 失效
标题翻译：超疏水氟气凝胶
公开(公告)号：US07211605B2
公开(公告)日：2007-05-01
申请号：US10794847
申请日：2004-03-04
申请人： Paul R. Coronado , John F. Poco , Lawrence W. Hrubesh
发明人： Paul R. Coronado , John F. Poco , Lawrence W. Hrubesh
IPC分类号： C08J3/02 , C03C3/00 , B01J13/00
CPC分类号： C09C1/3081 , B01J13/0091 , C01B33/159 , C01P2006/10 , C01P2006/12 , C08J2205/026 , Y10T428/2995
摘要： An aerogel material with surfaces containing fluorine atoms which exhibits exceptional hydrophobicity, or the ability to repel liquid water. Hydrophobic aerogels are efficient absorbers of solvents from water. Solvents miscible with water are separated from it because the solvents are more volatile than water and they enter the porous aerogel as a vapor across the liquid water/solid interface. Solvents that are immisicble with water are separated from it by selectively wetting the aerogel. The hydrophobic property is achieved by formulating the aerogel using fluorine containing molecules either directly by addition in the sol-gel process, or by treating a standard dried aerogel using the vapor of fluorine containing molecules.
摘要翻译：具有表现出优异疏水性的氟原子表面的气凝胶材料，或排斥液态水的能力。疏水性气凝胶是水中有效的溶剂吸收剂。与水混溶的溶剂与其分离，因为溶剂比水更易挥发，并且它们作为蒸汽进入多孔气凝胶，穿过液态水/固体界面。与水不溶的溶剂通过选择性润湿气凝胶与其分离。通过使用含氟分子直接通过在溶胶 - 凝胶法中添加来配制气凝胶，或通过使用含氟分子的蒸气处理标准干燥气凝胶来实现疏水性。

3. 发明授权

US5275796A Method for producing metal oxide aerogels having densities less than 0.02 g/cc 失效
标题翻译：密度小于0.02g / cc的金属氧化物气凝胶的制造方法
公开(公告)号：US5275796A
公开(公告)日：1994-01-04
申请号：US754349
申请日：1991-09-05
申请人： Thomas M. Tillotson , John F. Poco , Lawrence W. Hrubesh , Ian M. Thomas
发明人： Thomas M. Tillotson , John F. Poco , Lawrence W. Hrubesh , Ian M. Thomas
IPC分类号： B01J13/00 , C01B33/158 , C03C1/00 , C01B33/12 , B01J21/00
CPC分类号： B01J13/0091 , C01B33/1585 , C03C1/006 , Y02P20/544
摘要： A two-step method is described for making transparent aerogels which have a density of less than 0.003 g/cm.sup.3 to those with a density of more than 0.8 g/cm.sup.3, by a sol/gel process and supercritical extraction. Condensed metal oxide intermediate made with purified reagents can be diluted to produce stable aerogels with a density of less than 0.02 g/cm.sup.3. High temperature, direct supercritical extraction of the liquid phase of the gel produces hydrophobic aerogels which are stable at atmospheric moisture conditions. Monolithic, homogeneous silica aerogels with a density of less than 0.02 to higher than 0.8 g/cm.sup.3, with high thermal insulation capacity, improved mechanical strength and good optical transparency, are described.
摘要翻译：描述了通过溶胶/凝胶法和超临界萃取法制备密度小于0.003g / cm 3的透明气凝胶至密度大于0.8g / cm 3的透明气凝胶的两步法。用纯化试剂制成的冷凝金属氧化物中间体可以稀释，以产生密度小于0.02g / cm3的稳定气凝胶。高温，直接超临界萃取凝胶的液相产生在大气湿度条件下稳定的疏水性气凝胶。描述了具有小于0.02至高于0.8g / cm 3的密度的均匀二氧化硅气凝胶，具有高绝热能力，改进的机械强度和良好的光学透明性。

4. 发明授权

US08075716B1 Process for preparing energetic materials 有权
标题翻译：制备高能材料的方法
公开(公告)号：US08075716B1
公开(公告)日：2011-12-13
申请号：US09481043
申请日：2000-01-11
申请人： Randall L. Simpson , Ronald S. Lee , Thomas M. Tillotson , Lawrence W. Hrubesh , Rosalind W. Swansiger , Glenn A. Fox
发明人： Randall L. Simpson , Ronald S. Lee , Thomas M. Tillotson , Lawrence W. Hrubesh , Rosalind W. Swansiger , Glenn A. Fox
IPC分类号： C06B45/00
CPC分类号： C06B45/00 , Y02P20/544
摘要： Sol-gel chemistry is used for the preparation of energetic materials (explosives, propellants and pyrotechnics) with improved homogeneity, and/or which can be cast to near-net shape, and/or made into precision molding powders. The sol-gel method is a synthetic chemical process where reactive monomers are mixed into a solution, polymerization occurs leading to a highly cross-linked three dimensional solid network resulting in a gel. The energetic materials can be incorporated during the formation of the solution or during the gel stage of the process. The composition, pore, and primary particle sizes, gel time, surface areas, and density may be tailored and controlled by the solution chemistry. The gel is then dried using supercritical extraction to produce a highly porous low density aerogel or by controlled slow evaporation to produce a xerogel. Applying stress during the extraction phase can result in high density materials. Thus, the sol-gel method can be used for precision detonator explosive manufacturing as well as producing precision explosives, propellants, and pyrotechnics, along with high power composite energetic materials.
摘要翻译：溶胶 - 凝胶化学物质用于制备具有改进的均匀性的高能材料（爆炸物，推进剂和烟火），和/或可以铸造成近净形状和/或制成精密成型粉末。溶胶 - 凝胶法是将反应性单体混合到溶液中的合成化学方法，发生聚合，导致高度交联的三维固体网络，导致凝胶。高能材料可以在溶液形成期间或在该过程的凝胶阶段期间被引入。组合物，孔和一次粒径，凝胶时间，表面积和密度可以通过溶液化学定制和控制。然后使用超临界萃取干燥凝胶以产生高度多孔的低密度气凝胶或通过受控的缓慢蒸发以产生干凝胶。在提取阶段施加应力可导致高密度材料。因此，溶胶 - 凝胶法可用于精密雷管炸药制造，以及生产精密炸药，推进剂和烟火以及大功率复合材料。

5. 发明申请

US20090017339A1 Aerogel and Xerogel Composites for use as Carbon Anodes 有权
标题翻译：气凝胶和Xerogel复合材料用作碳阳极
公开(公告)号：US20090017339A1
公开(公告)日：2009-01-15
申请号：US12118571
申请日：2008-05-09
申请人： John F. Cooper , Thomas M. Tillotson , Lawrence W. Hrubesh
发明人： John F. Cooper , Thomas M. Tillotson , Lawrence W. Hrubesh
IPC分类号： H01M8/00 , H01M4/88
CPC分类号： C10L5/44 , C04B35/524 , C04B35/624 , C04B35/62605 , C04B35/6264 , C04B35/62655 , C04B35/83 , C04B2235/48 , C04B2235/77 , C04B2235/96 , C10L5/46 , C10L5/48 , H01M4/587 , H01M4/96 , H01M8/143 , H01M2008/147 , Y02E50/10 , Y02E50/30 , Y02E60/526
摘要： A method for forming a reinforced rigid anode monolith and fuel and product of such method. The method includes providing a solution of organic aerogel or xerogel precursors including at least one of a phenolic resin, phenol (hydroxybenzene), resorcinol(1,3-dihydroxybenzene), or catechol(1,2-dihydroxybenzene); at least one aldehyde compound selected from the group consisting of formaldehyde, acetaldehyde, and furfuraldehyde; and an alkali carbonate or phosphoric acid catalyst; adding internal reinforcement materials comprising carbon to said precursor solution to form a precursor mixture; gelling said precursor mixture to form a composite gel; drying said composite gel; and pyrolyzing said composite gel to form a wettable aerogel/carbon composite or a wettable xerogel/carbon composite, wherein said composites comprise chars and said internal reinforcement materials, and wherein said composite is suitable for use as an anode with the chars being fuel capable of being combusted in a molten salt electrochemical fuel cell in the range from 500 C to 800 C to produce electrical energy. Additional methods and systems/compositions are also provided.
摘要翻译：一种用于形成强化刚性阳极整料和燃料的方法及其制造方法。该方法包括提供有机气凝胶或干凝胶前体的溶液，其包括酚醛树脂，苯酚（羟基苯），间苯二酚（1,3-二羟基苯）或邻苯二酚（1,2-二羟基苯）中的至少一种; 至少一种选自甲醛，乙醛和糠醛的醛化合物; 和碱金属碳酸盐或磷酸催化剂; 向所述前体溶液中加入包含碳的内部增强材料以形成前体混合物; 胶凝所述前体混合物形成复合凝胶; 干燥所述复合凝胶; 并且热解所述复合凝胶以形成可湿性气凝胶/碳复合材料或可湿性干凝胶/碳复合材料，其中所述复合材料包含炭和所述内部增强材料，并且其中所述复合材料适合用作阳极，在熔融盐电化学燃料电池中在500℃至800℃范围内燃烧以产生电能。还提供了附加的方法和系统/组合物。

6. 发明授权

US06986818B2 Method for producing nanostructured metal-oxides 失效
标题翻译：生产纳米结构金属氧化物的方法
公开(公告)号：US06986818B2
公开(公告)日：2006-01-17
申请号：US09981076
申请日：2001-10-16
申请人： Thomas M. Tillotson , Randall L. Simpson , Lawrence W. Hrubesh , Alexander Gash
发明人： Thomas M. Tillotson , Randall L. Simpson , Lawrence W. Hrubesh , Alexander Gash
IPC分类号： C06B45/10
CPC分类号： C01F7/34 , C01B13/32 , C01F17/0043 , C01G1/02 , C01G15/00 , C01G19/02 , C01G25/02 , C01G27/02 , C01G33/00 , C01G37/033 , C01G41/00 , C01G43/01 , C01G49/02 , C01P2002/82 , C01P2006/12 , C01P2006/14 , C01P2006/16 , C06B21/0058 , C06B33/00 , C06B47/00 , Y02P20/544
摘要： A synthetic route for producing nanostructure metal-oxide-based materials using sol-gel processing. This procedure employs the use of stable and inexpensive hydrated-metal inorganic salts and environmentally friendly solvents such as water and ethanol. The synthesis involves the dissolution of the metal salt in a solvent followed by the addition of a proton scavenger, which induces gel formation in a timely manner. Both critical point (supercritical extraction) and atmospheric (low temperature evaporation) drying may be employed to produce monolithic aerogels and xerogels, respectively. Using this method synthesis of metal-oxide nanostructured materials have been carried out using inorganic salts, such as of Fe3+, Cr3+, Al3+, Ga3+, In3+, Hf4+, Sn4+, Zr4+, Nb5+, W6+, Pr3+, Er3+, Nd3+, Ce3+, U3+ and Y3+. The process is general and nanostructured metal-oxides from the following elements of the periodic table can be made: Groups 2 through 13, part of Group 14 (germanium, tin, lead), part of Group 15 (antimony, bismuth), part of Group 16 (polonium), and the lanthanides and actinides. The sol-gel processing allows for the addition of insoluble materials (e.g., metals or polymers) to the viscous sol, just before gelation, to produce a uniformly distributed nanocomposites upon gelation. As an example, energetic nanocomposites of FexOy gel with distributed Al metal are readily made. The compositions are stable, safe, and can be readily ignited to thermitic reaction.
摘要翻译：使用溶胶 - 凝胶法生产纳米结构金属氧化物基材料的合成路线。该方法使用稳定且廉价的水合金属无机盐和环境友好的溶剂如水和乙醇。该合成涉及将金属盐溶解在溶剂中，然后加入质子清除剂，其迅速诱导凝胶形成。可以采用临界点（超临界萃取）和大气（低温蒸发）干燥来分别制备单片气凝胶和干凝胶。使用这种方法合成金属氧化物纳米结构材料已经使用无机盐如Fe 3+，3+，3+，3+， 3+，3+，3+，5+，4 +，4 +，3+， SUP> 4 +，Nb 5+，W 6+，Pr 3+，Er 3+， Nd SUP Nd Nd Nd Nd Nd Nd Nd Nd Nd，，，，，U U U U U U U U U U U U U U U U U U U U U U。。。。。。。。。该方法是通用的，并且可以制备来自周期表的以下元素的纳米结构金属氧化物：组2至13，第14族（锗，锡，铅）的一部分，第15族的一部分（锑，铋），部分第16组（onium），镧系元素和锕系元素。溶胶 - 凝胶加工允许在凝胶化之前向粘性溶胶中添加不溶性材料（例如金属或聚合物），以在凝胶化时产生均匀分布的纳米复合材料。作为示例，容易制备具有分布的Al金属的高分子纳米复合材料的Fe x O y O y y y凝胶。组合物是稳定的，安全的，并且可以容易地点燃到耐火反应。

7. 发明授权

US06893518B1 Sol-gel manufactured energetic materials 失效
标题翻译：溶胶凝胶制成高能材料
公开(公告)号：US06893518B1
公开(公告)日：2005-05-17
申请号：US10697477
申请日：2003-10-29
申请人： Randall L. Simpson , Ronald S. Lee , Thomas M. Tillotson , Lawrence W. Hrubesh , Rosalind W. Swansiger , Glenn A. Fox
发明人： Randall L. Simpson , Ronald S. Lee , Thomas M. Tillotson , Lawrence W. Hrubesh , Rosalind W. Swansiger , Glenn A. Fox
IPC分类号： B01J13/00 , C06B21/00 , C06B45/00 , D03D23/00
CPC分类号： C06B21/0066 , B01J13/0091 , C06B21/0091 , C06B45/00 , Y02P20/544 , Y10S977/70 , Y10S977/775 , Y10S977/835 , Y10S977/895 , Y10S977/896
摘要： Sol-gel chemistry is used for the preparation of energetic materials (explosives, propellants and pyrotechnics) with improved homogeneity, and/or which can be cast to near-net shape, and/or made into precision molding powders. The sol-gel method is a synthetic chemical process where reactive monomers are mixed into a solution, polymerization occurs leading to a highly cross-linked three dimensional solid network resulting in a gel. The energetic materials can be incorporated during the formation of the solution or during the gel stage of the process. The composition, pore, and primary particle sizes, gel time, surface areas, and density may be tailored and controlled by the solution chemistry. The gel is then dried using supercritical extraction to produce a highly porous low density aerogel or by controlled slow evaporation to produce a xerogel. Applying stress during the extraction phase can result in high density materials. Thus, the sol-gel method can be used for precision detonator explosive manufacturing as well as producing precision explosives, propellants, and pyrotechnics, along with high power composite energetic materials.
摘要翻译：溶胶 - 凝胶化学物质用于制备具有改进的均匀性的高能材料（爆炸物，推进剂和烟火），和/或可以铸造成近净形状和/或制成精密成型粉末。溶胶 - 凝胶法是将反应性单体混合到溶液中的合成化学方法，发生聚合，导致高度交联的三维固体网络，导致凝胶。高能材料可以在溶液形成期间或在该过程的凝胶阶段期间被引入。组合物，孔和一次粒径，凝胶时间，表面积和密度可以通过溶液化学定制和控制。然后使用超临界萃取干燥凝胶以产生高度多孔的低密度气凝胶或通过受控的缓慢蒸发以产生干凝胶。在提取阶段施加应力可导致高密度材料。因此，溶胶 - 凝胶法可用于精密雷管炸药制造，以及生产精密炸药，推进剂和烟火以及大功率复合材料。

8. 发明授权

US07811711B2 Aerogel and xerogel composites for use as carbon anodes 有权
标题翻译：气凝胶和干凝胶复合材料用作碳阳极
公开(公告)号：US07811711B2
公开(公告)日：2010-10-12
申请号：US12118571
申请日：2008-05-09
申请人： John F. Cooper , Thomas M. Tillotson , Lawrence W. Hrubesh
发明人： John F. Cooper , Thomas M. Tillotson , Lawrence W. Hrubesh
IPC分类号： H01M4/88 , H01M8/14
CPC分类号： C10L5/44 , C04B35/524 , C04B35/624 , C04B35/62605 , C04B35/6264 , C04B35/62655 , C04B35/83 , C04B2235/48 , C04B2235/77 , C04B2235/96 , C10L5/46 , C10L5/48 , H01M4/587 , H01M4/96 , H01M8/143 , H01M2008/147 , Y02E50/10 , Y02E50/30 , Y02E60/526
摘要： A method for forming a reinforced rigid anode monolith and fuel and product of such method. The method includes providing a solution of organic aerogel or xerogel precursors including at least one of a phenolic resin, phenol (hydroxybenzene), resorcinol(1,3-dihydroxybenzene), or catechol(1,2-dihydroxybenzene); at least one aldehyde compound selected from the group consisting of formaldehyde, acetaldehyde, and furfuraldehyde; and an alkali carbonate or phosphoric acid catalyst; adding internal reinforcement materials comprising carbon to said precursor solution to form a precursor mixture; gelling said precursor mixture to form a composite gel; drying said composite gel; and pyrolyzing said composite gel to form a wettable aerogel/carbon composite or a wettable xerogel/carbon composite, wherein said composites comprise chars and said internal reinforcement materials, and wherein said composite is suitable for use as an anode with the chars being fuel capable of being combusted in a molten salt electrochemical fuel cell in the range from 500 C to 800 C to produce electrical energy. Additional methods and systems/compositions are also provided.
摘要翻译：一种用于形成强化刚性阳极整料和燃料的方法及其制造方法。该方法包括提供有机气凝胶或干凝胶前体的溶液，其包括酚醛树脂，苯酚（羟基苯），间苯二酚（1,3-二羟基苯）或邻苯二酚（1,2-二羟基苯）中的至少一种; 至少一种选自甲醛，乙醛和糠醛的醛化合物; 和碱金属碳酸盐或磷酸催化剂; 向所述前体溶液中加入包含碳的内部增强材料以形成前体混合物; 胶凝所述前体混合物形成复合凝胶; 干燥所述复合凝胶; 并且热解所述复合凝胶以形成可湿性气凝胶/碳复合材料或可湿性干凝胶/碳复合材料，其中所述复合材料包含炭和所述内部增强材料，并且其中所述复合材料适合用作阳极，在熔融盐电化学燃料电池中在500℃至800℃范围内燃烧以产生电能。还提供了附加的方法和系统/组合物。

9. 发明授权

US06986819B2 Metal-oxide-based energetic materials and synthesis thereof 失效
标题翻译：基于金属氧化物的高能材料及其合成
公开(公告)号：US06986819B2
公开(公告)日：2006-01-17
申请号：US10422488
申请日：2003-04-24
申请人： Thomas M. Tillotson , Randall L. Simpson , Lawrence W. Hrubesh
发明人： Thomas M. Tillotson , Randall L. Simpson , Lawrence W. Hrubesh
IPC分类号： D03D23/00
CPC分类号： C06B21/0066 , C06B21/0091 , C06B45/00 , Y02P20/544
摘要： A method of preparing energetic metal-oxide-based energetic materials using sol-gel chemistry has been invented. The wet chemical sol-gel processing provides an improvement in both safety and performance. Essentially, a metal-oxide oxidizer skeletal structure is prepared from hydrolyzable metals (metal salts or metal alkoxides) with fuel added to the sol prior to gelation or synthesized within the porosity metal-oxide gel matrix. With metal salt precursors a proton scavenger is used to destabilize the sol and induce gelation. With metal alkoxide precursors standard well-known sol-gel hydrolysis and condensation reactions are used. Drying is done by standard sol-gel practices, either by a slow evaporation of the liquid residing within the pores to produce a high density solid nanocomposite, or by supercritical extraction to produce a lower density, high porous nanocomposite. Other ingredients may be added to this basic nanostructure to change physical and chemical properties, which include organic constituents for binders or gas generators during reactions, burn rate modifiers, or spectral emitters.
摘要翻译：已经发明了使用溶胶 - 凝胶化学制备高能金属氧化物基能量材料的方法。湿化学溶胶 - 凝胶加工提高了安全性和性能。本质上，金属氧化物氧化剂骨架结构由可水解金属（金属盐或金属醇盐）制备，其中在凝胶化之前加入到溶胶中的燃料或在孔隙金属氧化物凝胶基质内合成。使用金属盐前体，质子清除剂用于使溶胶不稳定并诱导凝胶化。使用金属醇盐前体标准公知的溶胶 - 凝胶水解和缩合反应。通过标准溶胶 - 凝胶法进行干燥，通过缓慢蒸发在孔内的液体，产生高密度固体纳米复合物，或通过超临界萃取以产生较低密度的多孔纳米复合材料。可以将其它成分加入该基本纳米结构以改变物理和化学性质，其包括反应期间粘合剂或气体发生器的有机成分，燃烧速率调节剂或光谱发射体。

10. 发明授权

US06709600B2 Method for removing organic liquids from aqueous solutions and mixtures 失效
标题翻译：从水溶液和混合物中除去有机液体的方法
公开(公告)号：US06709600B2
公开(公告)日：2004-03-23
申请号：US09957854
申请日：2001-09-21
申请人： Lawrence W. Hrubesh , Paul R. Coronado , Jerome P. Dow
发明人： Lawrence W. Hrubesh , Paul R. Coronado , Jerome P. Dow
IPC分类号： B01D17022
CPC分类号： B01J20/103 , B01J20/2803 , B01J20/28033 , B01J20/28078 , B01J20/3204 , B01J20/3242 , C02F1/281 , C02F1/288 , C02F2101/30
摘要： A method for removing organic liquids from aqueous solutions and mixtures. The method employs any porous material preferably in granular form and having small pores and a large specific surface area, that is hydrophobic so that liquid water does not readily wet its surface. In this method, organics, especially organic solvents that mix with and are more volatile than water, are separated from aqueous solution by preferentially evaporating across the liquid/solid boundary formed at the surfaces of the hydrophobic porous materials. Also, organic solvents that are immiscible with water, preferentially wet the surfaces of the hydrophobic material and are drawn within the porous materials by capillary action.
摘要翻译：从水溶液和混合物中除去有机液体的方法。该方法采用任何多孔材料，优选为颗粒形式，并且具有小孔和大的比表面积，即疏水性使得液态水不容易使其表面湿润。在这种方法中，有机物，特别是与水混合并且比水更易挥发的有机溶剂通过优先蒸发穿过在疏水性多孔材料的表面形成的液体/固体边界而从水溶液中分离出来。此外，与水不混溶的有机溶剂优先地润湿疏水性材料的表面，并通过毛细作用在多孔材料内拉伸。

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