CN107098352A - A kind of preparation method of high temperature resistant aeroge and aerogel type porous ceramics - Google Patents
A kind of preparation method of high temperature resistant aeroge and aerogel type porous ceramics Download PDFInfo
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- CN107098352A CN107098352A CN201610092998.1A CN201610092998A CN107098352A CN 107098352 A CN107098352 A CN 107098352A CN 201610092998 A CN201610092998 A CN 201610092998A CN 107098352 A CN107098352 A CN 107098352A
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- Prior art keywords
- oxide
- colloidal sol
- high temperature
- temperature resistant
- aeroge
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- 239000000919 ceramic Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000004964 aerogel Substances 0.000 title claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 24
- 230000032683 aging Effects 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000012986 modification Methods 0.000 claims abstract description 8
- 230000004048 modification Effects 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 4
- 239000000835 fiber Substances 0.000 claims description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 19
- 230000003647 oxidation Effects 0.000 claims description 15
- 238000007254 oxidation reaction Methods 0.000 claims description 15
- -1 phenolic aldehyde Chemical class 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 12
- 238000013019 agitation Methods 0.000 claims description 9
- 229910052749 magnesium Inorganic materials 0.000 claims description 9
- 239000011777 magnesium Substances 0.000 claims description 9
- 239000010955 niobium Substances 0.000 claims description 9
- 230000005855 radiation Effects 0.000 claims description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 8
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 8
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 8
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 239000003292 glue Substances 0.000 claims description 7
- 229910052758 niobium Inorganic materials 0.000 claims description 7
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 7
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 6
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 6
- 229910052721 tungsten Inorganic materials 0.000 claims description 6
- 239000010937 tungsten Substances 0.000 claims description 6
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- 239000004411 aluminium Substances 0.000 claims description 5
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 5
- 229910017052 cobalt Inorganic materials 0.000 claims description 5
- 239000010941 cobalt Substances 0.000 claims description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 5
- 239000002131 composite material Substances 0.000 claims description 5
- 238000006073 displacement reaction Methods 0.000 claims description 5
- 229910052750 molybdenum Inorganic materials 0.000 claims description 5
- 239000011733 molybdenum Substances 0.000 claims description 5
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 5
- 229910021332 silicide Inorganic materials 0.000 claims description 5
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 claims description 5
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 5
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 229910052715 tantalum Inorganic materials 0.000 claims description 5
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 5
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 5
- 229910052726 zirconium Inorganic materials 0.000 claims description 5
- FRWYFWZENXDZMU-UHFFFAOYSA-N 2-iodoquinoline Chemical compound C1=CC=CC2=NC(I)=CC=C21 FRWYFWZENXDZMU-UHFFFAOYSA-N 0.000 claims description 4
- 229910052580 B4C Inorganic materials 0.000 claims description 4
- 229910052582 BN Inorganic materials 0.000 claims description 4
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 4
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 4
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 4
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 4
- LTPBRCUWZOMYOC-UHFFFAOYSA-N beryllium oxide Inorganic materials O=[Be] LTPBRCUWZOMYOC-UHFFFAOYSA-N 0.000 claims description 4
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 4
- 239000011651 chromium Substances 0.000 claims description 4
- IJKVHSBPTUYDLN-UHFFFAOYSA-N dihydroxy(oxo)silane Chemical compound O[Si](O)=O IJKVHSBPTUYDLN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052735 hafnium Inorganic materials 0.000 claims description 4
- 229910000449 hafnium oxide Inorganic materials 0.000 claims description 4
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 claims description 4
- 229910052746 lanthanum Inorganic materials 0.000 claims description 4
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims description 4
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 claims description 4
- 239000003870 refractory metal Substances 0.000 claims description 4
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 claims description 4
- 229910001936 tantalum oxide Inorganic materials 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 229910001935 vanadium oxide Inorganic materials 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000009736 wetting Methods 0.000 claims description 4
- 229910003454 ytterbium oxide Inorganic materials 0.000 claims description 4
- 229940075624 ytterbium oxide Drugs 0.000 claims description 4
- 239000011787 zinc oxide Substances 0.000 claims description 4
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 claims description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 3
- 229910052776 Thorium Inorganic materials 0.000 claims description 3
- 229910052796 boron Inorganic materials 0.000 claims description 3
- 229910000428 cobalt oxide Inorganic materials 0.000 claims description 3
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims description 3
- 230000007062 hydrolysis Effects 0.000 claims description 3
- 238000006460 hydrolysis reaction Methods 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims description 3
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 3
- 229910000484 niobium oxide Inorganic materials 0.000 claims description 3
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 3
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 3
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims description 3
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 150000003377 silicon compounds Chemical class 0.000 claims description 3
- 238000000352 supercritical drying Methods 0.000 claims description 3
- ZCUFMDLYAMJYST-UHFFFAOYSA-N thorium dioxide Chemical compound O=[Th]=O ZCUFMDLYAMJYST-UHFFFAOYSA-N 0.000 claims description 3
- 229910003452 thorium oxide Inorganic materials 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 3
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims description 3
- WEAMLHXSIBDPGN-UHFFFAOYSA-N (4-hydroxy-3-methylphenyl) thiocyanate Chemical compound CC1=CC(SC#N)=CC=C1O WEAMLHXSIBDPGN-UHFFFAOYSA-N 0.000 claims description 2
- OFEAOSSMQHGXMM-UHFFFAOYSA-N 12007-10-2 Chemical compound [W].[W]=[B] OFEAOSSMQHGXMM-UHFFFAOYSA-N 0.000 claims description 2
- QIJNJJZPYXGIQM-UHFFFAOYSA-N 1lambda4,2lambda4-dimolybdacyclopropa-1,2,3-triene Chemical compound [Mo]=C=[Mo] QIJNJJZPYXGIQM-UHFFFAOYSA-N 0.000 claims description 2
- 229910017083 AlN Inorganic materials 0.000 claims description 2
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 2
- 229910039444 MoC Inorganic materials 0.000 claims description 2
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 2
- 229910026551 ZrC Inorganic materials 0.000 claims description 2
- LRTTZMZPZHBOPO-UHFFFAOYSA-N [B].[B].[Hf] Chemical compound [B].[B].[Hf] LRTTZMZPZHBOPO-UHFFFAOYSA-N 0.000 claims description 2
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 claims description 2
- CFJRGWXELQQLSA-UHFFFAOYSA-N azanylidyneniobium Chemical compound [Nb]#N CFJRGWXELQQLSA-UHFFFAOYSA-N 0.000 claims description 2
- CUOITRGULIVMPC-UHFFFAOYSA-N azanylidynescandium Chemical compound [Sc]#N CUOITRGULIVMPC-UHFFFAOYSA-N 0.000 claims description 2
- SKKMWRVAJNPLFY-UHFFFAOYSA-N azanylidynevanadium Chemical compound [V]#N SKKMWRVAJNPLFY-UHFFFAOYSA-N 0.000 claims description 2
- AJXBBNUQVRZRCZ-UHFFFAOYSA-N azanylidyneyttrium Chemical compound [Y]#N AJXBBNUQVRZRCZ-UHFFFAOYSA-N 0.000 claims description 2
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Inorganic materials [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 claims description 2
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims description 2
- 229910002113 barium titanate Inorganic materials 0.000 claims description 2
- CSSYLTMKCUORDA-UHFFFAOYSA-N barium(2+);oxygen(2-) Chemical compound [O-2].[Ba+2] CSSYLTMKCUORDA-UHFFFAOYSA-N 0.000 claims description 2
- 229910052790 beryllium Inorganic materials 0.000 claims description 2
- YXTPWUNVHCYOSP-UHFFFAOYSA-N bis($l^{2}-silanylidene)molybdenum Chemical compound [Si]=[Mo]=[Si] YXTPWUNVHCYOSP-UHFFFAOYSA-N 0.000 claims description 2
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 2
- LGLOITKZTDVGOE-UHFFFAOYSA-N boranylidynemolybdenum Chemical compound [Mo]#B LGLOITKZTDVGOE-UHFFFAOYSA-N 0.000 claims description 2
- PALQHNLJJQMCIQ-UHFFFAOYSA-N boron;manganese Chemical compound [Mn]#B PALQHNLJJQMCIQ-UHFFFAOYSA-N 0.000 claims description 2
- AUVPWTYQZMLSKY-UHFFFAOYSA-N boron;vanadium Chemical compound [V]#B AUVPWTYQZMLSKY-UHFFFAOYSA-N 0.000 claims description 2
- CXKCTMHTOKXKQT-UHFFFAOYSA-N cadmium oxide Inorganic materials [Cd]=O CXKCTMHTOKXKQT-UHFFFAOYSA-N 0.000 claims description 2
- CFEAAQFZALKQPA-UHFFFAOYSA-N cadmium(2+);oxygen(2-) Chemical compound [O-2].[Cd+2] CFEAAQFZALKQPA-UHFFFAOYSA-N 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 239000011575 calcium Substances 0.000 claims description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000292 calcium oxide Substances 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 2
- 239000001506 calcium phosphate Substances 0.000 claims description 2
- 229910000389 calcium phosphate Inorganic materials 0.000 claims description 2
- 235000011010 calcium phosphates Nutrition 0.000 claims description 2
- 235000012241 calcium silicate Nutrition 0.000 claims description 2
- AOWKSNWVBZGMTJ-UHFFFAOYSA-N calcium titanate Chemical compound [Ca+2].[O-][Ti]([O-])=O AOWKSNWVBZGMTJ-UHFFFAOYSA-N 0.000 claims description 2
- BCFSVSISUGYRMF-UHFFFAOYSA-N calcium;dioxido(dioxo)chromium;dihydrate Chemical compound O.O.[Ca+2].[O-][Cr]([O-])(=O)=O BCFSVSISUGYRMF-UHFFFAOYSA-N 0.000 claims description 2
- 239000004917 carbon fiber Substances 0.000 claims description 2
- 238000003763 carbonization Methods 0.000 claims description 2
- 229910001567 cementite Inorganic materials 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- 229910000423 chromium oxide Inorganic materials 0.000 claims description 2
- 229910021357 chromium silicide Inorganic materials 0.000 claims description 2
- 229960004643 cupric oxide Drugs 0.000 claims description 2
- CRHLEZORXKQUEI-UHFFFAOYSA-N dialuminum;cobalt(2+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Al+3].[Co+2].[Co+2] CRHLEZORXKQUEI-UHFFFAOYSA-N 0.000 claims description 2
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 2
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 claims description 2
- FSBVERYRVPGNGG-UHFFFAOYSA-N dimagnesium dioxido-bis[[oxido(oxo)silyl]oxy]silane hydrate Chemical compound O.[Mg+2].[Mg+2].[O-][Si](=O)O[Si]([O-])([O-])O[Si]([O-])=O FSBVERYRVPGNGG-UHFFFAOYSA-N 0.000 claims description 2
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 2
- 229910001195 gallium oxide Inorganic materials 0.000 claims description 2
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 2
- WHJFNYXPKGDKBB-UHFFFAOYSA-N hafnium;methane Chemical compound C.[Hf] WHJFNYXPKGDKBB-UHFFFAOYSA-N 0.000 claims description 2
- 229910003437 indium oxide Inorganic materials 0.000 claims description 2
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- KSOKAHYVTMZFBJ-UHFFFAOYSA-N iron;methane Chemical compound C.[Fe].[Fe].[Fe] KSOKAHYVTMZFBJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000000391 magnesium silicate Substances 0.000 claims description 2
- 235000019792 magnesium silicate Nutrition 0.000 claims description 2
- 229910052919 magnesium silicate Inorganic materials 0.000 claims description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- UNASZPQZIFZUSI-UHFFFAOYSA-N methylidyneniobium Chemical compound [Nb]#C UNASZPQZIFZUSI-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229910021344 molybdenum silicide Inorganic materials 0.000 claims description 2
- 229910052863 mullite Inorganic materials 0.000 claims description 2
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims description 2
- 150000004767 nitrides Chemical class 0.000 claims description 2
- MMKQUGHLEMYQSG-UHFFFAOYSA-N oxygen(2-);praseodymium(3+) Chemical compound [O-2].[O-2].[O-2].[Pr+3].[Pr+3] MMKQUGHLEMYQSG-UHFFFAOYSA-N 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- 229910003447 praseodymium oxide Inorganic materials 0.000 claims description 2
- 239000010453 quartz Substances 0.000 claims description 2
- 229910001954 samarium oxide Inorganic materials 0.000 claims description 2
- 229940075630 samarium oxide Drugs 0.000 claims description 2
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims description 2
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium oxide Chemical compound O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 claims description 2
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 claims description 2
- 229910003451 terbium oxide Inorganic materials 0.000 claims description 2
- SCRZPWWVSXWCMC-UHFFFAOYSA-N terbium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Tb+3].[Tb+3] SCRZPWWVSXWCMC-UHFFFAOYSA-N 0.000 claims description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 2
- 229910001887 tin oxide Inorganic materials 0.000 claims description 2
- 229910021341 titanium silicide Inorganic materials 0.000 claims description 2
- 229910003470 tongbaite Inorganic materials 0.000 claims description 2
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 2
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims description 2
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims description 2
- RCFBAMFJCITZIC-UHFFFAOYSA-N zinc;dioxido(oxo)silane;zirconium(4+) Chemical compound [Zn+2].[Zr+4].[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O RCFBAMFJCITZIC-UHFFFAOYSA-N 0.000 claims description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 2
- 229910021355 zirconium silicide Inorganic materials 0.000 claims description 2
- 229910000859 α-Fe Inorganic materials 0.000 claims description 2
- LLYXJBROWQDVMI-UHFFFAOYSA-N 2-chloro-4-nitrotoluene Chemical compound CC1=CC=C([N+]([O-])=O)C=C1Cl LLYXJBROWQDVMI-UHFFFAOYSA-N 0.000 claims 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- 229910045601 alloy Inorganic materials 0.000 claims 1
- 239000000956 alloy Substances 0.000 claims 1
- XTDAIYZKROTZLD-UHFFFAOYSA-N boranylidynetantalum Chemical compound [Ta]#B XTDAIYZKROTZLD-UHFFFAOYSA-N 0.000 claims 1
- UFGZSIPAQKLCGR-UHFFFAOYSA-N chromium carbide Chemical compound [Cr]#C[Cr]C#[Cr] UFGZSIPAQKLCGR-UHFFFAOYSA-N 0.000 claims 1
- 229910001940 europium oxide Inorganic materials 0.000 claims 1
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 claims 1
- 239000002184 metal Substances 0.000 claims 1
- 239000011591 potassium Substances 0.000 claims 1
- 229910052700 potassium Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- WQJQOUPTWCFRMM-UHFFFAOYSA-N tungsten disilicide Chemical compound [Si]#[W]#[Si] WQJQOUPTWCFRMM-UHFFFAOYSA-N 0.000 claims 1
- 229910021342 tungsten silicide Inorganic materials 0.000 claims 1
- 239000011148 porous material Substances 0.000 abstract description 13
- 238000011065 in-situ storage Methods 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 150000001875 compounds Chemical class 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 238000013016 damping Methods 0.000 abstract description 2
- 239000012774 insulation material Substances 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
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- 239000000463 material Substances 0.000 description 11
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- 238000005516 engineering process Methods 0.000 description 5
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- 230000008602 contraction Effects 0.000 description 4
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- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
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- 238000001764 infiltration Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
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- 150000003839 salts Chemical class 0.000 description 2
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- 238000010792 warming Methods 0.000 description 2
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 description 1
- PFJFNQUFMTYCHB-UHFFFAOYSA-N C[SiH2]N[SiH3] Chemical group C[SiH2]N[SiH3] PFJFNQUFMTYCHB-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 241000282320 Panthera leo Species 0.000 description 1
- 239000004111 Potassium silicate Substances 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 235000019994 cava Nutrition 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- GVEHJMMRQRRJPM-UHFFFAOYSA-N chromium(2+);methanidylidynechromium Chemical compound [Cr+2].[Cr]#[C-].[Cr]#[C-] GVEHJMMRQRRJPM-UHFFFAOYSA-N 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 108010025899 gelatin film Proteins 0.000 description 1
- 238000000338 in vitro Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical class Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 229910052913 potassium silicate Inorganic materials 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 210000005239 tubule Anatomy 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- ZVWKZXLXHLZXLS-UHFFFAOYSA-N zirconium nitride Chemical compound [Zr]#N ZVWKZXLXHLZXLS-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/16—Preparation of silica xerogels
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- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/49—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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Abstract
The invention discloses a kind of preparation method of high temperature resistant aeroge, by adding high temperature resistant powder or whisker in colloidal sol, realize that colloidal sol and high temperature resistant powder or whisker in-situ are compound, after aging, modification, drying, acquire high temperature resistant aeroge.The present invention also disclosed a kind of preparation method of aerogel type porous ceramics, and above-mentioned high temperature resistant aeroge, which is sintered, can obtain the porous ceramics for remaining with aeroge pore space structure.High temperature resistant aeroge and aerogel type porous ceramics prepared by the present invention can bear 1000 DEG C to more than 1800 DEG C of high temperature, and keep nano aperture structure not cave in, with higher porosity and intensity, and aperture is adjustable from micropore to macropore, except purification separation, absorption, chemical industry catalytic carrier, sound absorption damping, sensing element, the field such as electrochemistry as super insulation material, can also be widely used in.Present invention process is simple and easy to apply, is adapted to large-scale production, improves aeroge resistance to elevated temperatures and application field.
Description
Technical field
The present invention relates to the preparation method of a kind of aeroge and porous ceramics, more particularly to a kind of high temperature resistant aeroge and gas
The preparation method of gel-type porous ceramics.
Background technology
Porous ceramics is otherwise known as micropore ceramics, foamed ceramics, with 3 D stereo network skeleton structure, in head in 1978
First succeeded in developing in the U.S..It can be divided into by pore size porous ceramics:Micropore ceramics (aperture is less than 2nm), mesoporous ceramic (hole
Footpath is between 2 ~ 50nm) and macropore ceramics (aperture is more than 50nm).Porous ceramics is characterized in primarily its porosity characteristic, the key of preparation
It is to form loose structure with difficult point.It is different with the requirement to material property according to application target, many is gradually developed in recent years not
Same technology of preparing.Wherein application relatively succeeds, and research is more active to be had：Add pore creating material technique, particle packing shaping work
Skill, foam process, Foam dipping method, conventional preparation techniques and gradient pores preparation method, the ion such as sol gel process
The new preparation process such as exchange process.
Sol-gal process is mainly used to prepare micropore ceramics material, particularly micropore ceramics film.This method is typically adopted
Pioneered body with inorganic salts or alkoxide, and precursor hydrolysis obtains colloidal sol, then condenses into the nothing being made up of MOM keys on porous support
Machine polymer gel film.Sol gel process can prepare aperture in nanoscale, the porous ceramic film of even air hole distribution, its
Maximum, which is advantageous in that, can readily obtain a variety of composition ground composite membrane, therefore just turn into inorganic separating film preparation field work
Most actively research field, causes the attention of lot of domestic and foreign researcher in skill.Xi Hongxia etc. uses aluminium isopropoxide for original
Material, prepares that stability is good, pin-free, flawless Al2O3 mesoporous films with sol-gel technique, and minimum-value aperture is up to 8nm.Fan
Bolt lion etc. prepares the microporous silica membrane in 3nm apertures by raw material of tetraethyl orthosilicate with sol-gel technique.
To prepare macropore ceramics, patent CN2009100718459 discloses a kind of ceramic aerogel and by gel injection-moulding
The method that shaping prepares ceramic aerogel, by organic monomers such as NMA, alkyl acrylamide, acrylic acid and poly-
The crosslinking agents such as (ethylene glycol) methacrylate are dissolved in solvent, add ceramic powder and dispersant, adjust pH value, mix
Suspension is obtained after even, is stirred after then adding initiator into suspension, carries out being crosslinked admittedly in casting mold die cavity
Change, ceramic aerogel is made by drying, dumping, sintering afterwards.The gained ceramic aerogel ceramic aerogel porosity is 50%
~80%, aperture is micron order, and most probable pore size is below 3 μm.But contain in the patented method compared with multimachine material, it is excluded
Mechanism is by thermal oxide or decomposes exclusion in vitro, forms hole, will result in heat treatment process, substantial amounts of organic matter is decomposed
Heat and gas are released, skeleton structure is impacted.
And aperture is rarely reported in 20 ~ 50nm porous ceramics.
Aeroge is mutually assembled with nanometer scale ultramicro powder is constituted nanoporous network structure, and average cell size is 20
~ 50nm, density low can reach 0.003g/cm3, and spiracular slit rate is up to 80~99.8%, and specific surface area is up to 1000m2/g, heat-resisting temperature
Degree is up to 1300 ~ 1800 DEG C, and room temperature thermal conductivity factor low can reach 0.013w/ (mk), is most light solid and thermal insulation so far
The best material of performance.But the mechanical property such as aeroge intensity and toughness is typically poor, stomata easily caves under external force
It is broken.The mechanical property of aeroge can preferably be improved by carrying out heat treatment at a certain temperature.But heat treatment temperature is general
No more than 500 DEG C, if heat treatment temperature is too high, nanoscale hole hole will cave in and cause aeroge to be densified completely.
Therefore cause the temperature in use of aeroge not high, even across heat treatment, its temperature in use also is difficult to more than 1000 DEG C.
To overcome the shortcomings of original porous ceramics technology of preparing, and improve the resistance to elevated temperatures of original aerogel material,
Spy proposes the present invention program.
The content of the invention
To overcome hole slump under traditional aeroge high temperature, the present invention proposes a kind of preparation side of high temperature resistant aeroge
Method, preparation process comprises the following steps：
（1）High temperature resistant powder or whisker are added into colloidal sol, obtained presoma is well mixed；
（2）The pH value of presoma is adjusted with acid or alkali, is directly formed and gel is formed after gel, or wetting fibre；
（3）Aging is carried out to gel；
（4）Solvent displacement or modification are carried out to gel；
（5）Gel is dried, aeroge is obtained.
On the basis of foregoing invention, present invention further proposes a kind of preparation method of aerogel type porous ceramics,
Preparation process comprises the following steps：
（1）High temperature resistant powder or whisker are added into colloidal sol, obtained presoma is well mixed；
（2）The pH value of presoma is adjusted with acid or alkali, is directly formed and gel is formed after gel, or wetting fibre；
（3）Aging is carried out to gel；
（4）Solvent displacement or modification are carried out to gel；
（5）Gel is dried, aeroge is obtained；
（6）Aeroge is sintered, aerogel type porous ceramics is obtained.
Step（1）Described colloidal sol includes silica sol, alumina sol, zirconia sol, titanium oxide sol, oxidation
Magnesium colloidal sol, cupric oxide colloidal sol, oxidation ferrum collosol, cobalt oxide colloidal sol, oxidation nickel sol, manganese oxide colloidal sol, zinc oxide colloidal sol, oxidation
Tin oxide sol, cadmium oxide colloidal sol, chromium oxide colloidal sol, niobium oxide colloidal sol, tantalum oxide colloidal sol, cerium oxide sol, vanadium oxide colloidal sol, oxidation
Molybdenum colloidal sol, tungsten oxide colloidal sol, hafnium oxide colloidal sol, thorium oxide sol, beryllium oxide colloidal sol, yittrium oxide colloidal sol, scandium oxide colloidal sol, oxidation
Cerium colloidal sol, strontium oxide strontia colloidal sol, indium oxide colloidal sol, gallium oxide colloidal sol, bismuth oxide colloidal sol, lanthana colloidal sol, ytterbium oxide colloidal sol, oxidation
One or more in europium colloidal sol, neodymia colloidal sol, terbium oxide colloidal sol, praseodymium oxide colloidal sol, samarium oxide colloidal sol, phenolic aldehyde colloidal sol.
Step（1）Described high temperature resistant powder or whisker, including refractory oxide, high temperature resistant composite oxides, resistance to height
It is one or more of in warm carbide, high temperature resistant nitride, high temperature resistant boride, high temperature resistant silicon compound, refractory metal.
Described refractory oxide includes silica, aluminum oxide, zirconium oxide, titanium oxide, iron oxide, barium monoxide, oxidation
Cobalt, nickel oxide, manganese oxide, zinc oxide, magnesia, calcium oxide, niobium oxide, tantalum oxide, cerium oxide, vanadium oxide, molybdenum oxide, oxidation
One or more in tungsten, beryllium oxide, yittrium oxide, lanthana, ytterbium oxide, hafnium oxide, thorium oxide.
Described high temperature resistant composite oxides include alumina silicate, zirconium silicate, calcium silicates, magnesium silicate, zinc zirconium silicate, potassium silicate
One in aluminium, aluminium titanates, barium titanate, calcium titanate, magnesium titanate, cobalt aluminate, magnesium aluminate, magnesium ferrite, magnesium zirconate, calcium chromate, calcium phosphate
Plant or several.
Described high temperature resistant carbide includes carborundum, titanium carbide, zirconium carbide, boron carbide, chromium carbide, cementite, carbonization
One or more in manganese, tungsten carbide, molybdenum carbide, ramet, niobium carbide, hafnium carbide.
Described silicon nitride, aluminium nitride, titanium nitride, zirconium nitride, hafnium nitride, boron nitride, beryllium nitride, scandium nitride, nitridation lanthanum,
One or more in yttrium nitride, niobium nitride, vanadium nitride, tantalum nitride.
Described high temperature resistant boride includes boronation cobalt, chromium boride, hafnium boride, manganese boride, molybdenum boride, niobium (Nb) boride, boronation
One or more in tantalum, vanadium boride, titanium boride, zirconium boride, calcium boride, tungsten boride, lanthanum boride.
Described high temperature resistant silicon compound includes titanium silicide, zirconium silicide, niobium silicide, tantalum silicide, chromium silicide, molybdenum silicide, silication
One or more in tungsten.
Described refractory metal includes the one or more in tungsten, molybdenum, tantalum, cobalt, nickel, chromium, titanium, zirconium, niobium, hafnium.
Step（2）Described fiber includes quartz fibre, high silica fiber, alumina fibre, alumina silicate fibre, mullite
Fiber, silicon carbide fibre, boron carbide fibre, silicon nitride fiber, boron nitride fiber, titanium nitride fiber, boron fibre, carbon fiber, carbon
It is one or more of in nanotube, tungsten filament, molybdenum filament, thorium silk.
Step（1）Described colloidal sol is made by the water soluble salt or Hydrolysis of Organic Chemicals As A Function of Ph of corresponding element or directly from market
Purchase, the solid content of colloidal sol is that the ratio of high temperature resistant powder or whisker and colloidal sol in 5 ~ 40%wt, presoma is mass ratio 1:1~
200, the mode of mixing includes mechanical agitation or ultrasonic wave is scattered.
Step（5）One or more in described drying, including supercritical drying, constant pressure and dry or vacuum drying.
Step（6）The temperature of described sintering is 900 DEG C ~ 2500 DEG C, and sintering atmosphere includes vacuum, air, inert gas
Middle one kind, sintering time is 1 ~ 20h.
Step（2）~（5）And step（6）, technical process can be accelerated using radio-frequency radiation, the frequency of radio-frequency radiation is
300KHz ~ 300GHz, power is 250W ~ 1000kW.
In the present invention, colloidal sol plays a part of following several respects：One is peptizaiton, and high temperature resistant powder or whisker add molten
In glue, by controlling the addition of concentration, the pH value of colloidal sol, high temperature resistant powder or whisker, different presomas can be obtained and glued
Degree, after agitated or ultrasonic wave is scattered, high temperature resistant powder or whisker are wrapped up and are dispersed in colloidal sol without sinking by colloidal sol；
Two be the effect of template in situ, and colloidal sol is during gel, and sol particles, which is reunited, constitutes three-dimensional net structure, high temperature resistant powder
Or whisker also take part in the structure of gel skeleton structure jointly, then through aging, modification, drying, as aeroge；Three be fluxing work
With, when gained aeroge is in hot environment or gained aeroge is sintered, the gel skeleton built by sol particles
Nano-particle will be changed into liquid phase again to crystalline transformation from noncrystal, be combined closely on the surface of high temperature resistant powder or whisker
And gel hole structural portion slump is kept, so as to improve aeroge resistance to elevated temperatures, reduce the sintering of aerogel type ceramics
Temperature, saves sintering time and the energy.
High temperature resistant powder or whisker in the present invention, both sides is played in aeroge and is acted on, one is as gas under high temperature
The reinforcing material of gel skeleton, when temperature is higher, the unformed amorphous nano particle in the skeleton of aeroge will be received to crystal
Rice material transformation, is usually associated with the slump of skeleton in transition process, or even hole is wholly absent referred to as dense body, and resistance to height
The presence of warm powder or whisker can be prevented effectively from the slump of aeroge skeleton with reinforcement aeroge skeleton；Two are, under hot environment,
The nano particle of aeroge skeleton from during non-crystalline conversion is crystal, such as component or crystal formation of high-temperature powder or whisker with
The crystal habit that gel is finally forwarded is the same or close, it is possible to play a part of nucleus Induction Transformation, accelerates conversion process, and
Support nanometer hole on framework not slump.
The present invention first prepares the aeroge of high temperature resistant powder or whisker reinforcement, then prepared by aeroge sintering into aerogel type
Porous ceramics, on the one hand makes full use of the adjustable advantage in aeroge aperture, can prepare the different pore size from micropore to macropore
It is required that porous ceramics；On the other hand conventional sol-gel processes are avoided from gel direct sintering ceramics because of surface tension and hair
, inevitably there is hole slump and the problem of gel skeleton is densified in tubule power.Thus the present invention is to improving aeroge
Resistance to elevated temperatures and prepare high performance porous ceramics and have great importance.
Beneficial effect
Compared with prior art, a kind of high temperature resistant aeroge of the invention and the preparation method of aerogel type porous ceramics have following
Significant effect.
（1）Colloidal sol of the present invention and high temperature resistant powder or whisker in-situ are compound, can obtain the gas of resistance to 1000~1800 high temperature
Gel rubber material, can be applied to the high temperature protection of the equipment such as aerospace craft, panzer, engine, refinery and metallurgical body of heater.
（2）Colloidal sol of the present invention and high temperature resistant powder or whisker in-situ are compound, can obtain adjustable aperture, high porosity, height
The aerogel structure characteristic such as specific surface area, also with high intensity, the high-performance aerogel type of dry linting is not ceramic, so as to extensive
Applied to gas liquid filtering, purification separation, absorption, chemical industry catalytic carrier, ion exchange, sound absorption damping, sensing element, barrier film
The fields such as material, quantum device, photoelectric material, microelectrode, electrochemical cell, it is also possible to make super insulation material.
（3）Colloidal sol of the present invention and high temperature resistant powder or whisker in-situ are compound, and aeroge pottery can be completed at a lower temperature
Porcelain is sintered, and reduces energy consumption raising efficiency.
（4）Present invention process is simple and easy to apply, is adapted to large-scale production and Technique Popularizing.
Accompanying drawing
Nothing.
Specific embodiment
Below to the specific of a kind of high temperature resistant aeroge for providing of the present invention and the preparation method of aerogel type porous ceramics
Embodiment is described in further detail.
Embodiment 1.
Ludox is prepared according to patent CN2014102703529 method, the solid content of Ludox is 8%, and pH value is
3.0, Ludox 1000g is taken, particle diameter is below 2um silica powder 30g, and particle diameter is below 5um silicon nitride powder 40g, with
1200r/min mechanical agitations 5 minutes, then scattered 3 minutes of ultrasonic wave presoma, back mechanical agitation presoma side be added dropwise
PH value is transferred to gel behind 4.6, static 10 minutes by 0.5mol/L ammoniacal liquor；By gel in 60 DEG C of water-baths aging 10h, then with six
Radio-frequency radiation is carried out with frequency 2450MHz, power 500w radio frequency during methyl disilazane substitution, substitution,
Complete to be modified after 27min, complete drying after gel is placed in into constant pressure and dry under infrared lamp, 20min, obtain high temperature resistant aeroge.
High temperature resistant aeroge density 160kg/m3, average pore size 42nm, porosity 86%, the 5h at a temperature of 1000 DEG C, volume contraction
Rate 6%.Above-mentioned high temperature resistant aeroge 30g is taken, is placed in Muffle furnace, 2h is sintered at 1100 DEG C and obtains aerogel type porous ceramics.Should
Aerogel type porous ceramics density 170kg/m3, average pore size 34nm, porosity 72%.
Embodiment 2.
Silica-zirconia colloidal sol is prepared according to patent CN2015102953891 method, the solid content of colloidal sol is
10%, pH value is 3.5, takes colloidal sol 1000g, and particle diameter is below 1um titanium oxide powder 35g, and particle diameter is below 3um zirconium silicate powder
40g, with 1500r/min mechanical agitations 10 minutes, obtains presoma；Back mechanical agitation presoma side be added dropwise 0.5mol/L ammonia
PH value is transferred to 4.7, infiltration alumina fibre gel after 9 minutes by water.Gel is used into frequency 2450MHz, power at 60 DEG C
500w radio frequency carries out completing aging after radio-frequency radiation, 30min, then with trim,ethylchlorosilane at 65 DEG C substitution 2h, it
Gel is placed in vacuum drying chamber afterwards it is warming up to 80 DEG C and be dried, drying is completed after 40min, high temperature resistant aeroge is obtained.Should
High temperature resistant aeroge density 270kg/m3, average pore size 30nm, porosity 78%, the 5h at a temperature of 1000 DEG C, cubical contraction
3%.Above-mentioned high temperature resistant aeroge 30g is taken, is placed in Muffle furnace, 4h is sintered at 1500 DEG C and obtains aerogel type porous ceramics.The gas
Gel-type porous ceramics density 280kg/m3, average pore size 23nm, porosity 65%.
Embodiment 3.
It is 80% ethanol and the mixture of water that 129.59g nickel chlorides are dissolved in into 500g concentration of alcohol, is added while stirring
0.2g polyacrylic acid, 0.3g expoxy propane, particle diameter are below 1um nickel oxide powder 40g, and particle diameter is below 2um boronation molybdenum powder
10g, with 1600r/min mechanical agitations 10 minutes, obtains presoma；The ammoniacal liquor that 0.5mol/L is added dropwise is added to presoma while stirring
PH value is transferred to 5.0, gel after radio-frequency radiation, 5min is carried out with frequency 2450MHz, power 300w radio frequency；By gel 55
DEG C water-bath in aging 24h, then carry out solvent displacement with absolute ethyl alcohol, C02 supercritical dryings carried out afterwards, drying temperature is 50
DEG C, pressure be after 15MPa, 4h high temperature resistant aeroge.High temperature resistant aeroge density 310kg/m3, average pore size 15nm, hole
Gap rate 56%, the 5h at a temperature of 1000 DEG C, cubical contraction 3%.Above-mentioned high temperature resistant aeroge 30g is taken, is placed in Muffle furnace,
3h is sintered at 1600 DEG C and obtains aerogel type porous ceramics.Aerogel type porous ceramics density 316kg/m3, average pore size 10nm,
Porosity 48%.
Embodiment 4.
Silica-lanthana-yittrium oxide colloidal sol is prepared according to patent CN2015102953891 method, consolidating for colloidal sol contains
Measure as 6%, pH value is 3.2, take colloidal sol 1000g, particle diameter is below 0.5um oxidation yttrium powder 35g, and particle diameter is below 4um tungsten
Powder 35g, with 1800r/min mechanical agitations 10 minutes, obtains presoma；Back mechanical agitation presoma side 0.5mol/L is added dropwise
PH value is transferred to 4.8, infiltration silicon carbide fibre gel after 8 minutes by ammoniacal liquor；Gel is used into frequency 2450MHz, power at 60 DEG C
500w radio frequency carries out completing aging after radio-frequency radiation, 30min, then with n-hexane at 45 DEG C solvent substitution 4h, afterwards
Gel is placed in vacuum drying chamber it is warming up to 80 DEG C and be dried, while is carried out with frequency 2450MHz, power 1200w radio frequency
Radio-frequency radiation, 16min, which is dried, to be completed, and obtains high temperature resistant aeroge.High temperature resistant aeroge density 150kg/m3, average pore size
55nm, porosity 92%, the 5h at a temperature of 1000 DEG C, cubical contraction 8%.Above-mentioned high temperature resistant aeroge 30g is taken, Muffle is placed in
In stove, sintering 3h obtains aerogel type porous ceramics at 1600 DEG C.Aerogel type porous ceramics density 160kg/m3, average hole
Footpath 40nm, porosity 80%.
Above-described embodiment is only used for illustrating the inventive concept of the present invention, rather than the restriction to rights protection of the present invention,
Any simple modification, equivalent variations and modification that every technology and method according to the present invention is substantially made to above example,
Still fall within the present invention technology and method scheme in the range of.
Claims (10)
1. a kind of preparation method of high temperature resistant aeroge, it is characterized in that, preparation process comprises the following steps：
（1）High temperature resistant powder or whisker are added into colloidal sol, obtained presoma is well mixed；
（2）The pH value of presoma is adjusted with acid or alkali, is directly formed and gel is formed after gel, or wetting fibre；
（3）Aging is carried out to gel；
（4）Solvent displacement or modification are carried out to gel；
（5）Gel is dried, aeroge is obtained.
2. a kind of preparation method of aerogel type porous ceramics, it is characterized in that, preparation process comprises the following steps：
（1）High temperature resistant powder or whisker are added into colloidal sol, obtained presoma is well mixed；
（2）The pH value of presoma is adjusted with acid or alkali, is directly formed and gel is formed after gel, or wetting fibre；
（3）Aging is carried out to gel；
（4）Solvent displacement or modification are carried out to gel；
（5）Gel is dried, aeroge is obtained；
（6）Aeroge is sintered, aerogel type porous ceramics is obtained.
3. preparation method according to claim 1 or 2, it is characterized in that, step（1）It is molten that described colloidal sol includes silica
Glue, alumina sol, zirconia sol, titanium oxide sol, magnesia colloidal sol, cupric oxide colloidal sol, oxidation ferrum collosol, cobalt oxide are molten
Glue, oxidation nickel sol, manganese oxide colloidal sol, zinc oxide colloidal sol, tin oxide sol, cadmium oxide colloidal sol, chromium oxide colloidal sol, niobium oxide are molten
Glue, tantalum oxide colloidal sol, cerium oxide sol, vanadium oxide colloidal sol, molybdenum oxide colloidal sol, tungsten oxide colloidal sol, hafnium oxide colloidal sol, thorium oxide are molten
Glue, beryllium oxide colloidal sol, yittrium oxide colloidal sol, scandium oxide colloidal sol, cerium oxide sol, strontium oxide strontia colloidal sol, indium oxide colloidal sol, gallium oxide are molten
Glue, bismuth oxide colloidal sol, lanthana colloidal sol, ytterbium oxide colloidal sol, europium oxide colloidal sol, neodymia colloidal sol, terbium oxide colloidal sol, praseodymium oxide are molten
One or more in glue, samarium oxide colloidal sol, phenolic aldehyde colloidal sol.
4. preparation method according to claim 1 or 2, it is characterized in that, step（1）Described high temperature resistant powder or whisker,
Including refractory oxide, high temperature resistant composite oxides, high temperature resistant carbide, high temperature resistant nitride, high temperature resistant boride, resistance to height
It is one or more of in warm silicide, refractory metal.
5. preparation method according to claim 4, it is characterized in that, described refractory oxide includes silica, oxidation
Aluminium, zirconium oxide, titanium oxide, iron oxide, barium monoxide, cobalt oxide, nickel oxide, manganese oxide, zinc oxide, magnesia, calcium oxide, oxidation
Niobium, tantalum oxide, cerium oxide, vanadium oxide, molybdenum oxide, tungsten oxide, beryllium oxide, yittrium oxide, lanthana, ytterbium oxide, hafnium oxide, oxidation
One or more in thorium；High temperature resistant composite oxides include alumina silicate, zirconium silicate, calcium silicates, magnesium silicate, zinc zirconium silicate, silicon
Sour potassium aluminium, aluminium titanates, barium titanate, calcium titanate, magnesium titanate, cobalt aluminate, magnesium aluminate, magnesium ferrite, magnesium zirconate, calcium chromate, calcium phosphate
Middle one or more；High temperature resistant carbide includes carborundum, titanium carbide, zirconium carbide, boron carbide, chromium carbide, cementite, carbonization
One or more in manganese, tungsten carbide, molybdenum carbide, ramet, niobium carbide, hafnium carbide；Silicon nitride, aluminium nitride, titanium nitride, nitridation
Zirconium, hafnium nitride, boron nitride, beryllium nitride, scandium nitride, nitridation lanthanum, yttrium nitride, niobium nitride, vanadium nitride, one kind in tantalum nitride or several
Kind；High temperature resistant boride includes boronation cobalt, chromium boride, hafnium boride, manganese boride, molybdenum boride, niobium (Nb) boride, tantalum boride, vanadium boride, boron
Change the one or more in titanium, zirconium boride, calcium boride, tungsten boride, lanthanum boride；High temperature resistant silicon compound include titanium silicide, zirconium silicide,
One or more in niobium silicide, tantalum silicide, chromium silicide, molybdenum silicide, tungsten silicide；Refractory metal include tungsten, molybdenum, tantalum, cobalt,
One or more in nickel, chromium, titanium, zirconium, niobium, hafnium, and the corresponding alloy of above-mentioned metal.
6. preparation method according to claim 1 or 2, it is characterized in that, step（2）Described fiber include quartz fibre,
High silica fiber, alumina fibre, alumina silicate fibre, mullite fiber, silicon carbide fibre, boron carbide fibre, silicon nitride fiber,
It is one or more of in boron nitride fiber, titanium nitride fiber, boron fibre, carbon fiber, CNT, tungsten filament, molybdenum filament, thorium silk.
7. preparation method according to claim 1 or 2, it is characterized in that, step（1）Described colloidal sol by corresponding element water
Soluble or Hydrolysis of Organic Chemicals As A Function of Ph are made or directly from market purchase, the solid content of colloidal sol is resistance to height in 5 ~ 40%wt, presoma
The ratio of warm powder or whisker and colloidal sol is mass ratio 1:1 ~ 200, the mode of mixing includes mechanical agitation or ultrasonic wave is scattered.
8. preparation method according to claim 1 or 2, it is characterized in that, step（5）Described drying, including supercritical drying
One or more in dry, constant pressure and dry or vacuum drying.
9. preparation method according to claim 2, it is characterized in that, step（6）The temperature of described sintering be 900 DEG C ~
2500 DEG C, sintering atmosphere includes one kind in vacuum, air, inert gas, and sintering time is 1 ~ 20h.
10. preparation method according to claim 1 or 2, it is characterized in that, the step of claim 1 or 2（2）~（5）And right
It is required that 2 steps（6）, technical process can be accelerated using radio-frequency radiation, the frequency of radio-frequency radiation is 300KHz ~ 300GHz, power
For 250W ~ 1000kW.
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