CN105540645A - Preparation method for germanium oxide and yttrium oxide hybrid aerogel composite material - Google Patents
Preparation method for germanium oxide and yttrium oxide hybrid aerogel composite material Download PDFInfo
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- CN105540645A CN105540645A CN201610067401.8A CN201610067401A CN105540645A CN 105540645 A CN105540645 A CN 105540645A CN 201610067401 A CN201610067401 A CN 201610067401A CN 105540645 A CN105540645 A CN 105540645A
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- yttrium oxide
- oxide
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- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium oxide Inorganic materials O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 title claims abstract description 96
- PVADDRMAFCOOPC-UHFFFAOYSA-N oxogermanium Chemical compound [Ge]=O PVADDRMAFCOOPC-UHFFFAOYSA-N 0.000 title claims abstract description 96
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 239000004964 aerogel Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000002131 composite material Substances 0.000 title abstract description 5
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000012784 inorganic fiber Substances 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 14
- 230000032683 aging Effects 0.000 claims abstract description 9
- 238000000352 supercritical drying Methods 0.000 claims abstract description 9
- 239000000835 fiber Substances 0.000 claims description 47
- 239000011159 matrix material Substances 0.000 claims description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 230000008595 infiltration Effects 0.000 claims description 16
- 238000001764 infiltration Methods 0.000 claims description 16
- 229910052594 sapphire Inorganic materials 0.000 claims description 16
- 239000010980 sapphire Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000013543 active substance Substances 0.000 claims description 10
- 150000001298 alcohols Chemical class 0.000 claims description 10
- 239000007822 coupling agent Substances 0.000 claims description 10
- 238000003837 high-temperature calcination Methods 0.000 claims description 10
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 8
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000012756 surface treatment agent Substances 0.000 claims description 8
- IEXRMSFAVATTJX-UHFFFAOYSA-N tetrachlorogermane Chemical compound Cl[Ge](Cl)(Cl)Cl IEXRMSFAVATTJX-UHFFFAOYSA-N 0.000 claims description 8
- PCMOZDDGXKIOLL-UHFFFAOYSA-K yttrium chloride Chemical compound [Cl-].[Cl-].[Cl-].[Y+3] PCMOZDDGXKIOLL-UHFFFAOYSA-K 0.000 claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052754 neon Inorganic materials 0.000 claims description 4
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical group CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 2
- QMMBZOSZCYBCDC-UHFFFAOYSA-N NCCNCCC[SiH](OC(OCC)(OCC)OCC)OC Chemical compound NCCNCCC[SiH](OC(OCC)(OCC)OCC)OC QMMBZOSZCYBCDC-UHFFFAOYSA-N 0.000 claims description 2
- 235000011054 acetic acid Nutrition 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- JBIROUFYLSSYDX-UHFFFAOYSA-M benzododecinium chloride Chemical group [Cl-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 JBIROUFYLSSYDX-UHFFFAOYSA-M 0.000 claims description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- SYELZBGXAIXKHU-UHFFFAOYSA-N dodecyldimethylamine N-oxide Chemical compound CCCCCCCCCCCC[N+](C)(C)[O-] SYELZBGXAIXKHU-UHFFFAOYSA-N 0.000 claims description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 235000011187 glycerol Nutrition 0.000 claims description 2
- 150000002596 lactones Chemical class 0.000 claims description 2
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 2
- YWFWDNVOPHGWMX-UHFFFAOYSA-N n,n-dimethyldodecan-1-amine Chemical compound CCCCCCCCCCCCN(C)C YWFWDNVOPHGWMX-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 235000011007 phosphoric acid Nutrition 0.000 claims description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims 1
- 230000018109 developmental process Effects 0.000 abstract description 5
- 238000007711 solidification Methods 0.000 abstract 1
- 230000008023 solidification Effects 0.000 abstract 1
- 238000004381 surface treatment Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000004966 Carbon aerogel Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 150000002291 germanium compounds Chemical class 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G17/00—Compounds of germanium
- C01G17/02—Germanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention provides a preparation method for germanium oxide and yttrium oxide hybrid aerogel composite material. The method comprises the following steps of infiltrating prepared hybrid sol into a treated inorganic fiber material, performing sol solidification and full aging, and then performing supercritical drying so as to obtain a hybrid aerogel composite material. According to the technical scheme provided by the invention, the preparation process is simple and easy to operate, and the germanium oxide and yttrium oxide hybrid aerogel with excellent performance is prepared for the first time. According to the technical scheme provided by the invention, germanium oxide and yttrium oxide hybrid aerogel with high specific surface area, low intensity and high porosity is prepared and has the excellent performances that the specific surface area is 300-400m<2>/g, the density is 0.13-0.20g/m<3>, and the porosity is 70-80%. The aerogel composite material provided by the invention has thermal conductivity less than 0.035w/m.k at a temperature of 1000 DEG C and shrinking percentage less than 3.4%. According to the technical scheme provided by the invention, development and application of a germanium oxide material are broadened.
Description
Technical field
The present invention relates to a kind of preparation method of aerogel, specifically, relate to the preparation method of a kind of germanium oxide and yttrium oxide aerogel composite.
Background technology
Aerogel refers to assembles the nanoporous network of formation for skeleton mutually with nano particle, and in network skeleton hole, be full of the lightweight nano solid material of gaseous state dispersion medium.Aerogel is as a kind of nano material, except the characteristic with nano material, also there are other excellent properties, as: high porosity, high-specific surface area, extremely low density, low thermal conductivity and low sound transmission speed etc., have huge application prospect in catalysis, space flight, medicine, the energy, building and metallurgy etc.
Meanwhile, aerogel kind have also been obtained extreme enrichment, and as metal aerogel, organic aerogel and carbon aerogels, so far increasing Novel air gel is progressively developed.
Germanium oxide can be widely used in and make high pure metal germanium, germanium compound, chemical catalyst, medicine industry, PET resin, electron device etc.; Such as, the glass containing germanium oxide has higher specific refractory power and dispersion, can be used as pantoscope and microscope camera lens.In order to expand the development of aerogel further, the present invention has the germanium oxide of unique texture and performance and the preparation method of yttrium oxide hybrid aerogel matrix material by setting forth first, development and the application of such material can better be promoted, widen the kind of aerogel simultaneously, promote the development of aerogel science and technology.
Summary of the invention
The object of this invention is to provide the preparation method of the little germanium oxide of a kind of high-specific surface area, low density, high porosity, low heat conduction and shrinking percentage and yttrium oxide hybrid aerogel matrix material; Technical scheme manufacture craft provided by the invention is simple, easy to operate, and prepares germanium oxide and the yttrium oxide hybrid aerogel of excellent performance first.
Realize the object of the invention technical scheme as follows:
A preparation method for germanium oxide and yttrium oxide hybrid aerogel matrix material, described matrix material comprises germanium oxide and yttrium oxide hybrid aerogel, inorganic fibers, and described preparation method comprises the steps:
1) process of inorganic fibers: at 150 ~ 200 DEG C, dry inorganic fibre 4 ~ 6 hours; Inorganic fibre is immersed after being the surface treatment agent solution of the proportions of 1:2 ~ 4:0.004 ~ 0.008:0.012 ~ 0.02 by inorganic fibre, distilled water, tensio-active agent and coupling agent weight ratio, dry 1 ~ 3 hour at 160 ~ 220 DEG C, cool to obtain the inorganic fibre after surface treatment;
Wherein, described inorganic fibre is sapphire whisker, and described sapphire whisker comprises following component by mass percentage: Al
2o
3, 70 ~ 98%; SiO
2, 2 ~ 30%; Fiber diameter is 0.8 μm ~ 3.0 μm;
2) preparation of germanium oxide and yttrium oxide hybrid collosol: the proportions mixed solution by germanium chloride, Yttrium trichloride, alcohols material, deionized water, propylene oxide and catalyzer according to mol ratio being 0.5 ~ 1:0.5 ~ 2:10 ~ 50:10 ~ 40:0.05 ~ 0.5:10-4 ~ 10-2, after stirring 10 ~ 20min leaves standstill, obtain germanium oxide and yttrium oxide hybrid collosol;
3) infiltrate: by step 2) germanium oxide and the infiltration of yttrium oxide hybrid collosol through step 1) inorganic fibers after process;
4) prepare germanium oxide and yttrium oxide hybrid aerogel matrix material: at 50 ~ 80 DEG C, make step 3) gained infiltration thing in germanium oxide and yttrium oxide hybrid collosol generation gelling, obtain germanium oxide and yttrium oxide hybrid gel; After 20 ~ 50 DEG C of aging 20 ~ 50h, after ethanol or CO 2 supercritical drying; Under protection of inert gas, germanium oxide and yttrium oxide hybrid aerogel matrix material are carried out high-temperature calcination, obtain germanium oxide and yttrium oxide hybrid aerogel matrix material.
Further, described step 4) in rare gas element be nitrogen, helium or neon.Described step 4) in high-temperature calcination temperature be 600 ~ 1200 DEG C.
Further, described alcohols material is methyl alcohol, ethanol, propyl alcohol or butanols.Described catalyzer is hydrochloric acid, sulfuric acid, phosphoric acid, formic acid, acetic acid, oxalic acid or hydrofluoric acid.Described coupling agent is γ-aminopropyl triethoxysilane, N-β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane, methyltrimethoxy silane or vinyltrimethoxy silane.Described tensio-active agent is dodecyl benzyl dimethyl ammonium chloride, Sodium dodecylbenzene sulfonate, dimethyl dodecyl amine oxide, dodecyl-dimethyl amine second lactone or glycerin polyoxyethylene ether.
Further, the germanium oxide prepared of described method and yttrium oxide hybrid gel specific surface area 300 ~ 400m
2/ g, porosity 70 ~ 80%.The germanium oxide that described method is prepared and the thermal conductivity of yttrium oxide hybrid aerogel matrix material at 1000 DEG C are less than 0.035w/mk, and shrinking percentage is less than 3.4%.
With immediate prior art ratio, technical scheme provided by the invention has following excellent effect:
1, technical scheme preparation technology provided by the invention is simple, easy to operate, is applicable to scale operation, and prepares germanium oxide and the yttrium oxide hybrid aerogel of excellent performance first.
2, technical scheme provided by the invention prepares high-specific surface area, low density, the germanium oxide of high porosity and yttrium oxide hybrid aerogel, and its excellent properties is specific surface area 300 ~ 400m
2/ more than g, density 0.13 ~ 0.20g/m
3, porosity 70 ~ 80%.
3, the germanium oxide prepared of technical scheme provided by the invention and the thermal conductivity of yttrium oxide hybrid aerogel matrix material at 1000 DEG C are less than 0.035w/mk, and shrinking percentage is less than 3.4%.
4, technical scheme provided by the invention, has widened development and the application of germanium oxide material.
Embodiment
Further be clearly and completely described technical scheme below in conjunction with the embodiment of the present invention, obviously, described embodiment is only a part of embodiment of the present invention, instead of whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain, all belongs to the scope of protection of the invention.
Embodiment 1
1) process of inorganic fibers: at 200 DEG C, dry inorganic fibre 6 hours; Inorganic fibre is immersed after being the surface treatment agent solution of the proportions of 1:4:0.008:0.02 by inorganic fibre, distilled water, tensio-active agent and coupling agent weight ratio, dry 1 hour at 220 DEG C, cool to obtain the inorganic fibre after surface treatment;
Wherein, inorganic fibre is sapphire whisker, sapphire whisker following component by mass percentage: Al
2o
3, 98%; SiO
2, 2%; Fiber diameter is 3.0 μm;
2) preparation of germanium oxide and yttrium oxide hybrid collosol: be 1:0.5:10:10:0.05:10 according to mol ratio by germanium chloride, Yttrium trichloride, alcohols material, deionized water, propylene oxide and catalyzer
-4proportions mixed solution, stir 20min leave standstill after, obtain germanium oxide and yttrium oxide hybrid collosol;
3) infiltrate: by step 2) germanium oxide and the infiltration of yttrium oxide hybrid collosol through step 1) inorganic fibers after process;
4) prepare germanium oxide and yttrium oxide hybrid aerogel matrix material: at 80 DEG C, make step 3) gained infiltration thing in germanium oxide and yttrium oxide hybrid collosol generation gelling, obtain germanium oxide and yttrium oxide hybrid gel; After 50 DEG C of aging 20h, after supercritical drying; Under inert nitrogen gas protection, germanium oxide and yttrium oxide hybrid aerogel matrix material are carried out 600 DEG C of high-temperature calcinations, obtains germanium oxide and yttrium oxide hybrid aerogel matrix material.
Embodiment 2
1) process of inorganic fibers: at 150 DEG C, dry inorganic fibre 6 hours; Inorganic fibre is immersed after being the surface treatment agent solution of the proportions of 1:2:0.004:0.012 by inorganic fibre, distilled water, tensio-active agent and coupling agent weight ratio, dry 3 hours at 160 DEG C, cool to obtain the inorganic fibre after surface treatment;
Wherein, inorganic fibre is sapphire whisker, sapphire whisker following component by mass percentage: Al
2o
3, 70%; SiO
2, 30%; Fiber diameter is 0.8 μm;
2) preparation of germanium oxide and yttrium oxide hybrid collosol: be 0.5:2:50:40:0.5:10 according to mol ratio by germanium chloride, Yttrium trichloride, alcohols material, deionized water, propylene oxide and catalyzer
-2proportions mixed solution, stir 15min leave standstill after, obtain germanium oxide and yttrium oxide hybrid collosol;
3) infiltrate: by step 2) germanium oxide and the infiltration of yttrium oxide hybrid collosol through step 1) inorganic fibers after process;
4) prepare germanium oxide and yttrium oxide hybrid aerogel matrix material: at 50 DEG C, make step 3) gained infiltration thing in germanium oxide and yttrium oxide hybrid collosol generation gelling, obtain germanium oxide and yttrium oxide hybrid gel; After 20 DEG C of aging 50h, after ethanol or CO 2 supercritical drying; Under the protection of rare gas element neon, germanium oxide and yttrium oxide hybrid aerogel matrix material are carried out 1200 DEG C of high-temperature calcinations, obtains germanium oxide and yttrium oxide hybrid aerogel matrix material.
Embodiment 3
1) process of inorganic fibers: at 180 DEG C, dry inorganic fibre 5 hours; Inorganic fibre is immersed after being the surface treatment agent solution of the proportions of 1:3:0.006:0.016 by inorganic fibre, distilled water, tensio-active agent and coupling agent weight ratio, dry 2 hours at 200 DEG C, cool to obtain the inorganic fibre after surface treatment;
Wherein, inorganic fibre is sapphire whisker, sapphire whisker following component by mass percentage: Al
2o
3, 80%; SiO
2, 20%; Fiber diameter is 1.0 μm;
2) preparation of germanium oxide and yttrium oxide hybrid collosol: be 1::30:20:0.1:10 according to mol ratio by germanium chloride, Yttrium trichloride, alcohols material, deionized water, propylene oxide and catalyzer
-3proportions mixed solution, stir 20min leave standstill after, obtain germanium oxide and yttrium oxide hybrid collosol;
3) infiltrate: by step 2) germanium oxide and the infiltration of yttrium oxide hybrid collosol through step 1) inorganic fibers after process;
4) prepare germanium oxide and yttrium oxide hybrid aerogel matrix material: at 70 DEG C, make step 3) gained infiltration thing in germanium oxide and yttrium oxide hybrid collosol generation gelling, obtain germanium oxide and yttrium oxide hybrid gel; After 40 DEG C of aging 35h, after ethanol or CO 2 supercritical drying; Under inert gas helium protection, germanium oxide and yttrium oxide hybrid aerogel matrix material are carried out 800 DEG C of high-temperature calcinations, obtains germanium oxide and yttrium oxide hybrid aerogel matrix material.
Embodiment 4
1) process of inorganic fibers: at 180 DEG C, dry inorganic fibre 4 hours; Inorganic fibre is immersed after being the surface treatment agent solution of the proportions of 1:3:0.007:0.014 by inorganic fibre, distilled water, tensio-active agent and coupling agent weight ratio, dry 3 hours at 180 DEG C, cool to obtain the inorganic fibre after surface treatment;
Wherein, inorganic fibre is sapphire whisker, sapphire whisker following component by mass percentage: Al
2o
3, 90%; SiO
2, 10%; Fiber diameter is 2.0 μm;
2) preparation of germanium oxide and yttrium oxide hybrid collosol: be 0.5:1:40:30:0.2:10 according to mol ratio by germanium chloride, Yttrium trichloride, alcohols material, deionized water, propylene oxide and catalyzer
-4proportions mixed solution, stir 15min leave standstill after, obtain germanium oxide and yttrium oxide hybrid collosol;
3) infiltrate: by step 2) germanium oxide and the infiltration of yttrium oxide hybrid collosol through step 1) inorganic fibers after process;
4) prepare germanium oxide and yttrium oxide hybrid aerogel matrix material: at 65 DEG C, make step 3) gained infiltration thing in germanium oxide and yttrium oxide hybrid collosol generation gelling, obtain germanium oxide and yttrium oxide hybrid gel; After 45 DEG C of aging 30h, after ethanol or CO 2 supercritical drying; Under inert nitrogen gas protection, germanium oxide and yttrium oxide hybrid aerogel matrix material are carried out 900 DEG C of high-temperature calcinations, obtains germanium oxide and yttrium oxide hybrid aerogel matrix material.
Embodiment 5
1) process of inorganic fibers: at 175 DEG C, dry inorganic fibre 4 hours; Inorganic fibre is immersed after being the surface treatment agent solution of the proportions of 1:4:0.007:0.018 by inorganic fibre, distilled water, tensio-active agent and coupling agent weight ratio, dry 2 hours at 220 DEG C, cool to obtain the inorganic fibre after surface treatment;
Wherein, inorganic fibre is sapphire whisker, sapphire whisker following component by mass percentage: Al
2o
3, 85%; SiO
2, 15%; Fiber diameter is 2.0 μm;
2) preparation of germanium oxide and yttrium oxide hybrid collosol: be 1:2:35:25:0.4:10 according to mol ratio by germanium chloride, Yttrium trichloride, alcohols material, deionized water, propylene oxide and catalyzer
-2proportions mixed solution, stir 18min leave standstill after, obtain germanium oxide and yttrium oxide hybrid collosol;
3) infiltrate: by step 2) germanium oxide and the infiltration of yttrium oxide hybrid collosol through step 1) inorganic fibers after process;
4) prepare germanium oxide and yttrium oxide hybrid aerogel matrix material: at 75 DEG C, make step 3) gained infiltration thing in germanium oxide and yttrium oxide hybrid collosol generation gelling, obtain germanium oxide and yttrium oxide hybrid gel; After 40 DEG C of aging 45h, after ethanol or CO 2 supercritical drying; Under the protection of rare gas element neon, germanium oxide and yttrium oxide hybrid aerogel matrix material are carried out 1000 DEG C of high-temperature calcinations, obtains germanium oxide and yttrium oxide hybrid aerogel matrix material.
Embodiment 6
1) process of inorganic fibers: at 200 DEG C, dry inorganic fibre 5 hours; Inorganic fibre is immersed after being the surface treatment agent solution of the proportions of 1:3:0.006:0.016 by inorganic fibre, distilled water, tensio-active agent and coupling agent weight ratio, dry 3 hours at 200 DEG C, cool to obtain the inorganic fibre after surface treatment;
Wherein, inorganic fibre is sapphire whisker, sapphire whisker following component by mass percentage: Al
2o
3, 75%; SiO
2, 25%; Fiber diameter is 0.8 μm;
2) preparation of germanium oxide and yttrium oxide hybrid collosol: be 1:2:35:40:0.5:10 according to mol ratio by germanium chloride, Yttrium trichloride, alcohols material, deionized water, propylene oxide and catalyzer
-3proportions mixed solution, stir 14min leave standstill after, obtain germanium oxide and yttrium oxide hybrid collosol;
3) infiltrate: by step 2) germanium oxide and the infiltration of yttrium oxide hybrid collosol through step 1) inorganic fibers after process;
4) prepare germanium oxide and yttrium oxide hybrid aerogel matrix material: at 65 DEG C, make step 3) gained infiltration thing in germanium oxide and yttrium oxide hybrid collosol generation gelling, obtain germanium oxide and yttrium oxide hybrid gel; After 25 DEG C of aging 35h, after ethanol or CO 2 supercritical drying; Under inert gas helium protection, germanium oxide and yttrium oxide hybrid aerogel matrix material are carried out 1100 DEG C of high-temperature calcinations, obtains germanium oxide and yttrium oxide hybrid aerogel matrix material.
The raw materials used kind of the various embodiments described above and ratio thereof, as shown in table 1.
Table 1
In embodiment, gained properties of sample is listed in the table below 2.
Table 2
Above embodiment is only in order to illustrate that technical scheme of the present invention is not intended to limit; those of ordinary skill in the field are to be understood that; can modify to the specific embodiment of the present invention with reference to above-described embodiment or equivalent to replace, these do not depart from any amendment of spirit and scope of the invention or equivalently to replace within the claims that all awaits the reply in application.
Claims (9)
1. a preparation method for germanium oxide and yttrium oxide hybrid aerogel matrix material, is characterized in that, described matrix material comprises germanium oxide and yttrium oxide hybrid aerogel, inorganic fibers, and described preparation method comprises the steps:
1) process of inorganic fibers: at 150 ~ 200 DEG C, dry inorganic fibre 4 ~ 6 hours; After inorganic fibre is immersed the surface treatment agent solution process of preparing by weight the inorganic fibre of ratio be 1:2 ~ 4:0.004 ~ 0.008:0.012 ~ 0.02, distilled water, tensio-active agent and coupling agent, dry 1 ~ 3 hour at 160 ~ 220 DEG C, cooling;
Wherein, described inorganic fibre is sapphire whisker, and described sapphire whisker comprises following component by mass percentage: Al
2o
3, 70 ~ 98%; SiO
2, 2 ~ 30%; Fiber diameter is 0.8 μm ~ 3.0 μm;
2) preparation of germanium oxide and yttrium oxide hybrid collosol: be 0.5 ~ 1:0.5 ~ 2:10 ~ 50:10 ~ 40:0.05 ~ 0.5:10 according to mol ratio by germanium chloride, Yttrium trichloride, alcohols material, deionized water, propylene oxide and catalyzer
-4~ 10
-2proportions mixed solution, stir 10 ~ 20min leave standstill after, obtain germanium oxide and yttrium oxide hybrid collosol;
3) infiltrate: by step 2) germanium oxide and the infiltration of yttrium oxide hybrid collosol through step 1) inorganic fibers after process;
4) prepare germanium oxide and yttrium oxide hybrid aerogel matrix material: at 50 ~ 80 DEG C, make step 3) gained infiltration thing in germanium oxide and yttrium oxide hybrid collosol generation gelling, obtain germanium oxide and yttrium oxide hybrid gel; At 20 ~ 50 DEG C after aging 20 ~ 50h, after ethanol or CO 2 supercritical drying; Under protection of inert gas, germanium oxide and yttrium oxide hybrid aerogel matrix material are carried out high-temperature calcination, obtain germanium oxide and yttrium oxide hybrid aerogel matrix material.
2. the preparation method of a kind of germanium oxide as claimed in claim 1 and yttrium oxide hybrid aerogel matrix material, is characterized in that, described step 4) in rare gas element be nitrogen, helium or neon.
3. the preparation method of a kind of germanium oxide as claimed in claim 1 and yttrium oxide hybrid aerogel matrix material, is characterized in that, described step 4) in high-temperature calcination temperature be 600 ~ 1200 DEG C.
4. the preparation method of a kind of germanium oxide as claimed in claim 1 and yttrium oxide hybrid aerogel matrix material, is characterized in that, described alcohols material is methyl alcohol, ethanol, propyl alcohol or butanols.
5. the preparation method of a kind of germanium oxide as claimed in claim 1 and yttrium oxide hybrid aerogel matrix material, is characterized in that, described catalyzer is hydrochloric acid, sulfuric acid, phosphoric acid, formic acid, acetic acid, oxalic acid or hydrofluoric acid.
6. the preparation method of a kind of germanium oxide as claimed in claim 1 and yttrium oxide hybrid aerogel matrix material, it is characterized in that, described coupling agent is γ-aminopropyl triethoxysilane, N-β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane, methyltrimethoxy silane or vinyltrimethoxy silane.
7. the preparation method of a kind of germanium oxide as claimed in claim 1 and yttrium oxide hybrid aerogel matrix material, it is characterized in that, described tensio-active agent is dodecyl benzyl dimethyl ammonium chloride, Sodium dodecylbenzene sulfonate, dimethyl dodecyl amine oxide, dodecyl-dimethyl amine second lactone or glycerin polyoxyethylene ether.
8., as the germanium oxide of claim 1 ~ 7 as described in any one and the preparation method of yttrium oxide hybrid aerogel matrix material, it is characterized in that, germanium oxide prepared by described method and yttrium oxide hybrid gel specific surface area 300 ~ 400m
2/ g, porosity 70 ~ 80%.
9. as the germanium oxide of claim 1 ~ 7 as described in any one and the preparation method of yttrium oxide hybrid aerogel matrix material, it is characterized in that, the germanium oxide that described method is prepared and the thermal conductivity of yttrium oxide hybrid aerogel matrix material at 1000 DEG C are less than 0.035w/mk, and shrinking percentage is less than 3.4%.
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