Methods of making and using oxide ceramic solids and products and devices related thereto
US-9093717-B2 · Jul 28, 2015 · US
US9808964B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-9808964-B2 |
| Application number | US-201214131821-A |
| Country | US |
| Kind code | B2 |
| Filing date | Jul 12, 2012 |
| Priority date | Jul 12, 2011 |
| Publication date | Nov 7, 2017 |
| Grant date | Nov 7, 2017 |
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A method of forming a porous sol gel, including a dried porous sol gel, is provided comprising forming a sol gel from a sol gel-forming composition comprising a silane solution and a catalyst solution; and non-supercritically drying the sol gel to provide a dried porous sol gel having no springback. The dried porous sol gel can include dried macroporous or mesoporous sol gels or dried hybrid aerogels. The materials may contain open or filled pores. Such materials are useful as thermal insulators.
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What is claimed is: 1. A method of forming a sol gel from a sol gel-forming composition comprising: forming the sol gel from the sol gel-forming composition, wherein the sol gel-forming composition comprises a silane solution and a catalyst solution, wherein the catalyst solution is added to the silane solution at a rate from about 1% to about 50% catalyst solution per volume per second; and non-supercritically drying the sol gel to provide a dried silicon-based porous sol gel having no springback, wherein the dried silicon-based porous sol gel is cast in place on a structure or preformed using a mold. 2. The method of claim 1 wherein the catalyst solution is added to the silane solution at a rate from about 20% to about 50% catalyst solution volume per second. 3. The method of claim 1 wherein the non-supercritical drying comprises drying under ambient conditions. 4. The method of claim 1 wherein silane in the silane solution has a chemical structure of ASi(OX)(OY)(OZ), wherein A, X, Y, and Z are independently selected from C1-C5 alkyl. 5. The method of claim 3 wherein the silane comprises methyltrimethoxysilane and the silane solution further comprises a silane solution solvent. 6. The method of claim 1 wherein the catalyst solution comprises a base, water, solvent and base. 7. The method of claim 6 wherein the base is selected from ammonium hydroxide, sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate and combinations thereof. 8. The method of claim 1 wherein the sol-gel forming composition further comprises a filler. 9. The method of claim 8 wherein the filler is a fiber or powder. 10. The method of claim 9 wherein the fiber is quartz or zirconia. 11. The method of claim 9 wherein the powder is an opacifier. 12. The method of claim 11 wherein the opacifier comprises titania powder. 13. The method of claim 9 wherein the powder is fumed silica or silica powder. 14. The method of claim 1 wherein the dried silicon-based porous sol gel is a dried macroporous or mesoporous sol gel. 15. The method of claim 1 wherein the dried silicon-based porous sol gel is a dried hybrid aerogel. 16. The method of claim 15 wherein the dried hybrid aerogel is ambiently dried or freeze-dried. 17. The method of claim 1 further comprising insulating a structure with the dried silica-based porous sol gel. 18. The method of claim 1 wherein the silica-based sol gel is a microporous silica-based aerogel. 19. The method of claim 1 wherein the dried silicon-based porous sol gel is preformed in the mold and is removed from the mold while still wet or partially wet. 20. A method of forming a sol gel from a sol gel-forming composition comprising: combining a first silane solution with a first catalyst solution to form a first catalyst/silane solution, wherein the catalyst solution is added to the silane solution at a rate from about 1% to about 50% catalyst solution per volume per second; providing the first catalyst/silane solution to a mold or structure; allowing the first catalyst/silane solution to gel and age to form a silicon-based porous sol gel; combining a second silane solution with a second catalyst solution to form a second catalyst/silane solution, wherein the catalyst solution is added to the silane solution at a rate of from about 1% to about 50% catalyst solution per volume per second; casting the second catalyst/silane solution in place in the structure or mold containing the silicon-based porous sol gel to form a wet hybrid silicon-based aerogel; and non-supercritically drying the wet hybrid silicon-based aerogel to produce a dried hybrid silicon-based aerogel having no springback. 21. The method of claim 20 wherein the silicon-based porous sol gel is a dried silicon-based porous sol gel or a partially dried silicon-based porous sol gel.
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