CN105693231A - Preparation method of germanium oxide and zinc oxide hybrid aerogel composite material - Google Patents
Preparation method of germanium oxide and zinc oxide hybrid aerogel composite material Download PDFInfo
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- CN105693231A CN105693231A CN201610067340.5A CN201610067340A CN105693231A CN 105693231 A CN105693231 A CN 105693231A CN 201610067340 A CN201610067340 A CN 201610067340A CN 105693231 A CN105693231 A CN 105693231A
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- zinc oxide
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- germanium oxide
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- germanium
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 184
- 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 95
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 92
- 239000004964 aerogel Substances 0.000 title claims abstract description 48
- 239000002131 composite material Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 13
- 230000032683 aging Effects 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000009396 hybridization Methods 0.000 claims description 87
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 30
- 239000000835 fiber Substances 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 27
- 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 22
- 229910052863 mullite Inorganic materials 0.000 claims description 22
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 20
- 239000012784 inorganic fiber Substances 0.000 claims description 18
- 239000004094 surface-active agent Substances 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 17
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 16
- MJWPFSQVORELDX-UHFFFAOYSA-K aluminium formate Chemical compound [Al+3].[O-]C=O.[O-]C=O.[O-]C=O MJWPFSQVORELDX-UHFFFAOYSA-K 0.000 claims description 16
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 16
- WCOATMADISNSBV-UHFFFAOYSA-K diacetyloxyalumanyl acetate Chemical compound [Al+3].CC([O-])=O.CC([O-])=O.CC([O-])=O WCOATMADISNSBV-UHFFFAOYSA-K 0.000 claims description 16
- 230000008595 infiltration Effects 0.000 claims description 16
- 238000001764 infiltration Methods 0.000 claims description 16
- 239000002243 precursor Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 16
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 14
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- 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 10
- 150000001298 alcohols Chemical class 0.000 claims description 10
- 239000007822 coupling agent Substances 0.000 claims description 10
- 235000019253 formic acid Nutrition 0.000 claims description 10
- 238000003837 high-temperature calcination Methods 0.000 claims description 10
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 8
- 230000002378 acidificating effect Effects 0.000 claims description 8
- 239000004411 aluminium Substances 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 239000003795 chemical substances by application Substances 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
- 210000002950 fibroblast Anatomy 0.000 claims description 8
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 239000001294 propane Substances 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 8
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- 238000009987 spinning Methods 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
- 239000011592 zinc chloride Substances 0.000 claims description 8
- 235000005074 zinc chloride Nutrition 0.000 claims description 8
- 239000001569 carbon dioxide Substances 0.000 claims description 7
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 7
- 239000012530 fluid Substances 0.000 claims description 7
- 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
- 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
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-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
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 4
- 239000003054 catalyst 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
- 239000004310 lactic acid Substances 0.000 claims description 4
- 235000014655 lactic acid Nutrition 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
- 229910052756 noble gas Inorganic materials 0.000 claims description 4
- 239000011975 tartaric acid Substances 0.000 claims description 4
- 235000002906 tartaric acid Nutrition 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
- KBIWNQVZKHSHTI-UHFFFAOYSA-N 4-n,4-n-dimethylbenzene-1,4-diamine;oxalic acid Chemical compound OC(=O)C(O)=O.CN(C)C1=CC=C(N)C=C1 KBIWNQVZKHSHTI-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
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Natural products OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 2
- 235000011054 acetic acid Nutrition 0.000 claims description 2
- 239000002253 acid Substances 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
- 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
- 235000011187 glycerol Nutrition 0.000 claims description 2
- 235000011167 hydrochloric acid Nutrition 0.000 claims description 2
- 150000002596 lactones Chemical class 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
- 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
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- JHJUUEHSAZXEEO-UHFFFAOYSA-M sodium;4-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=C(S([O-])(=O)=O)C=C1 JHJUUEHSAZXEEO-UHFFFAOYSA-M 0.000 claims description 2
- 239000001117 sulphuric acid Substances 0.000 claims description 2
- 235000011149 sulphuric acid Nutrition 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims 1
- 230000018109 developmental process Effects 0.000 abstract description 5
- 239000000443 aerosol Substances 0.000 abstract 1
- 239000002657 fibrous material Substances 0.000 abstract 1
- 238000004381 surface treatment Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 4
- 229910001873 dinitrogen Inorganic materials 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
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 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
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- -1 medical industry Substances 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
- 238000000352 supercritical drying Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—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
- C04B35/453—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 zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
- C04B35/62231—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on oxide ceramics
- C04B35/6224—Fibres based on silica
- C04B35/62245—Fibres based on silica rich in aluminium oxide
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62844—Coating fibres
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62886—Coating the powders or the macroscopic reinforcing agents by wet chemical techniques
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
Abstract
The invention provides a preparation method of a germanium oxide and zinc oxide hybrid aerogel composite material. The method comprises the following steps: impregnating prepared hybrid sol into a treated inorganic fibrous material, gelling and sufficiently aging, and then super-critically drying to obtain the hybrid aerosol composite material. According to the technical scheme provided by the invention, the preparation process is simple and easy in operation; and moreover, the germanium oxide and zinc oxide hybrid aerogel with excellent performance is prepared for the first time. By adopting the technical scheme provided by the invention, the prepared germanium oxide and zinc oxide hybrid aerogel is high in specific surface area, low in density, high in porosity and excellent in performance, wherein the specific surface area is 250 to 300 m<2>/g, the density is 0.13 to 0.20 g/m<3>, and the porosity is 80 to 90 percent. At the temperature of 1000 DEG C, the heat conductivity of the aerogel composite material is less than 0.035 w/m.k, and the shrinkage rate is less than 3.4 percent. By adopting the technical scheme provided by the invention, the development and application ranges of the germanium oxide material are widened.
Description
Technical field
The preparation method that the present invention relates to a kind of aeroge, specifically, relates to a kind of germanium oxide and the preparation method of zinc oxide aerogel composite。
Background technology
Aeroge refers to that the nanoporous network mutually assembling composition with nano-particle is skeleton, and is full of the lightweight nano solid material of gaseous state disperse medium in network skeleton hole。Aeroge 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., in catalysis, space flight, medicine, the energy, building and metallurgy etc., there is huge application prospect。
Meanwhile, aeroge kind have also been obtained extreme enrichment, and such as metal aerogel, organic aerogel and carbon aerogels, so far increasing Novel air gel is progressively developed。
Germanium oxide can be widely used for making high pure metal germanium, germanium compound, chemical catalyst, medical industry, PET resin, electronic device etc.；Such as, the glass containing germanium oxide has higher refractive index and dispersion, can as pantoscope and microscope camera lens。In order to expand the development of aeroge further, the present invention will set forth have the germanium oxide of unique texture and performance and the preparation method of zinc oxide hybridization aerogel composite first, can better promote development and the application of such material, widen the kind of aeroge simultaneously, promote the development of aeroge science and technology。
Summary of the invention
The preparation method that it is an object of the invention to provide the little germanium oxide of a kind of high-specific surface area, low-density, high porosity, low heat conduction and shrinkage factor and zinc oxide hybridization aerogel composite；Technical scheme processing technology provided by the invention simply, easily operate, and prepares germanium oxide and the zinc oxide hybridization aeroge of excellent performance first。
Realize the object of the invention technical scheme as follows:
The preparation method of a kind of germanium oxide and zinc oxide hybridization aerogel composite, described composite includes germanium oxide and zinc oxide hybridization aeroge, inorganic fibers, and described preparation method comprises the steps:
1) process of inorganic fibers: at 150～200 DEG C, dry inorfil 4～6 hours；After inorfil is immersed the surface treatment agent solution by inorfil, distilled water, surfactant and proportions that coupling agent weight ratio is 1:2～4:0.004～0.008:0.012～0.02, dry 1～3 hour at 160～220 DEG C, cool down to obtain inorfil after surface treatment；
Wherein, described inorfil is polycrystalline mullite fibre, and the preparation method of described polycrystalline mullite fibre comprises the following steps: is dissolved in by aluminium powder in the mixture of formic acid and acetic acid, is heated to reflux, and prepares aluminium triformate and aluminium acetate mixed sols solution；Aluminium triformate and aluminium acetate mixed sols add the acidic silicasol of removing sodium；Solution after mix homogeneously adds spinning-aid agent；Mixed liquor adds surfactant；Spinning solution adds tartaric acid, one or several of citric acid or lactic acid；Above-mentioned mixed liquor is in winding-up or gets rid of fibroblast under strand part；By polycrystalline alumina fiber precursor preliminarily dried；Finally it is heated polycrystal alumina precursor at 500～1400 DEG C processing；
2) preparation of germanium oxide and zinc oxide hybridization colloidal sol: by germanium chloride, zinc chloride, alcohols material, deionized water, expoxy propane and catalyst according to the proportions mixed liquor that mol ratio is 0.5～1:0.5～2:10～50:10～40:0.05～0.5:10-4～10-2, stirring 10～20min obtains germanium oxide and zinc oxide hybridization colloidal sol after standing；
3) infiltration: by step 2) germanium oxide and zinc oxide hybridization colloidal sol infiltrate through step 1) process after inorganic fibers；
4) prepare germanium oxide and zinc oxide hybridization aerogel composite: at 50～80 DEG C, make step 3) gained infiltration thing in germanium oxide and zinc oxide hybridization colloidal sol generation gelling, obtain germanium oxide and zinc oxide hybridization gel；After 20～50 DEG C of aging 20～50h, after ethanol or carbon dioxide supercritical fluid drying；Under inert gas shielding, germanium oxide and zinc oxide hybridization aerogel composite are carried out high-temperature calcination, obtain germanium oxide and zinc oxide hybridization aerogel composite。
Further, described step 4) in noble gas be nitrogen, helium or neon。Described step 4) in high-temperature calcination temperature be 600～1200 DEG C。
Further, described alcohols material is methanol, ethanol, propanol or butanol。Described catalyst is hydrochloric acid, sulphuric acid, phosphoric acid, formic acid, acetic acid, ethanedioic acid or Fluohydric acid.。Described coupling agent is gamma-aminopropyl-triethoxy-silane, N-β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane, MTMS or vinyltrimethoxy silane。Described surfactant is dodecyl dimethyl benzyl ammonium chloride, dodecylbenzene sodium sulfonate, dimethyl dodecyl amine oxide, dodecyl-dimethyl amine second lactone or glycerin polyoxyethylene ether。
Further, the germanium oxide that prepared by described method and zinc oxide hybridization gel specific surface area 250～300m2/ g, porosity 80～90%。Germanium oxide that described method is prepared and zinc oxide hybridization aerogel composite thermal conductivity at 1000 DEG C are less than 0.035w/m k, and shrinkage factor 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 simply, easily operate, and is suitable for large-scale production, and prepares germanium oxide and the zinc oxide hybridization aeroge 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 zinc oxide hybridization aeroge, and its excellent properties is specific surface area 250～300m2/ more than g, density 0.13～0.20g/m3, porosity 80～90%。
3, technical scheme provided by the invention is prepared germanium oxide and zinc oxide hybridization aerogel composite thermal conductivity at 1000 DEG C are less than 0.035w/m k, and shrinkage factor is less than 3.4%。
4, technical scheme provided by the invention, has widened development and the application of germanium oxide material。
Detailed description of the invention
Further technical scheme is clearly and completely described below in conjunction with the embodiment of the present invention, it is clear that described embodiment is only a part of embodiment of the present invention, rather than whole embodiments。Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain, broadly fall into the scope of protection of the invention。
Embodiment 1
1) process of inorganic fibers: at 200 DEG C, dry inorfil 6 hours；After inorfil is immersed the surface treatment agent solution by inorfil, distilled water, surfactant and proportions that coupling agent weight ratio is 1:4:0.008:0.02, dry 1 hour at 220 DEG C, cool down to obtain inorfil after surface treatment；
Wherein, inorfil is polycrystalline mullite fibre, and the step of the preparation method of polycrystalline mullite fibre is: is dissolved in by aluminium powder in the mixture of formic acid and acetic acid, is heated to reflux, and prepares aluminium triformate and aluminium acetate mixed sols solution；Aluminium triformate and aluminium acetate mixed sols add the acidic silicasol of removing sodium；Solution after mix homogeneously adds spinning-aid agent；Mixed liquor adds surfactant；Spinning solution adds tartaric acid；Above-mentioned mixed liquor is fibroblast when winding-up；Polycrystalline alumina fiber precursor is dried；Finally it is heated polycrystal alumina precursor processing at 1400 DEG C, obtains polycrystalline mullite fibre；
2) preparation of germanium oxide and zinc oxide hybridization colloidal sol: be 1:0.5:10:10:0.05:10 according to mol ratio by germanium chloride, zinc chloride, alcohols material, deionized water, expoxy propane and catalyst-4Proportions mixed liquor, stirring 20min stand after, obtain germanium oxide and zinc oxide hybridization colloidal sol；
3) infiltration: by step 2) germanium oxide and zinc oxide hybridization colloidal sol infiltrate through step 1) process after inorganic fibers；
4) prepare germanium oxide and zinc oxide hybridization aerogel composite: at 80 DEG C, make step 3) gained infiltration thing in germanium oxide and zinc oxide hybridization colloidal sol generation gelling, obtain germanium oxide and zinc oxide hybridization gel；After 50 DEG C of aging 20h, after supercritical drying；Under inert nitrogen gas is protected, germanium oxide and zinc oxide hybridization aerogel composite are carried out 600 DEG C of high-temperature calcinations, obtains germanium oxide and zinc oxide hybridization aerogel composite。
Embodiment 2
1) process of inorganic fibers: at 150 DEG C, dry inorfil 6 hours；After inorfil is immersed the surface treatment agent solution by inorfil, distilled water, surfactant and proportions that coupling agent weight ratio is 1:2:0.004:0.012, dry 3 hours at 160 DEG C, cool down to obtain inorfil after surface treatment；
Wherein, inorfil is polycrystalline mullite fibre, and the step of the preparation method of polycrystalline mullite fibre is: is dissolved in by aluminium powder in the mixture of formic acid and acetic acid, is heated to reflux, and prepares aluminium triformate and aluminium acetate mixed sols solution；Aluminium triformate and aluminium acetate mixed sols add the acidic silicasol of removing sodium；Solution after mix homogeneously adds spinning-aid agent；Mixed liquor adds surfactant；Spinning solution adds citric acid；Above-mentioned mixed liquor is fibroblast under getting rid of strand part；Polycrystalline alumina fiber precursor is dried；Finally it is heated polycrystal alumina precursor processing at 500 DEG C, obtains polycrystalline mullite fibre；
2) preparation of germanium oxide and zinc oxide hybridization colloidal sol: be 0.5:2:50:40:0.5:10 according to mol ratio by germanium chloride, zinc chloride, alcohols material, deionized water, expoxy propane and catalyst-2Proportions mixed liquor, stirring 15min stand after, obtain germanium oxide and zinc oxide hybridization colloidal sol；
3) infiltration: by step 2) germanium oxide and zinc oxide hybridization colloidal sol infiltrate through step 1) process after inorganic fibers；
4) prepare germanium oxide and zinc oxide hybridization aerogel composite: at 50 DEG C, make step 3) gained infiltration thing in germanium oxide and zinc oxide hybridization colloidal sol generation gelling, obtain germanium oxide and zinc oxide hybridization gel；After 20 DEG C of aging 50h, after ethanol or carbon dioxide supercritical fluid drying；Under noble gas neon is protected, germanium oxide and zinc oxide hybridization aerogel composite are carried out 1200 DEG C of high-temperature calcinations, obtains germanium oxide and zinc oxide hybridization aerogel composite。
Embodiment 3
1) process of inorganic fibers: at 180 DEG C, dry inorfil 5 hours；After inorfil is immersed the surface treatment agent solution by inorfil, distilled water, surfactant and proportions that coupling agent weight ratio is 1:3:0.006:0.016, dry 2 hours at 200 DEG C, cool down to obtain inorfil after surface treatment；
Wherein, inorfil is polycrystalline mullite fibre, and the step of the preparation method of polycrystalline mullite fibre is: is dissolved in by aluminium powder in the mixture of formic acid and acetic acid, is heated to reflux, and prepares aluminium triformate and aluminium acetate mixed sols solution；Aluminium triformate and aluminium acetate mixed sols add the acidic silicasol of removing sodium；Solution after mix homogeneously adds spinning-aid agent；Mixed liquor adds surfactant；Spinning solution adds lactic acid；Above-mentioned mixed liquor is fibroblast when winding-up；Polycrystalline alumina fiber precursor is dried；Finally it is heated polycrystal alumina precursor at 800 DEG C processing；Obtain polycrystalline mullite fibre；
2) preparation of germanium oxide and zinc oxide hybridization colloidal sol: be 1::30:20:0.1:10 according to mol ratio by germanium chloride, zinc chloride, alcohols material, deionized water, expoxy propane and catalyst-3Proportions mixed liquor, stirring 20min stand after, obtain germanium oxide and zinc oxide hybridization colloidal sol；
3) infiltration: by step 2) germanium oxide and zinc oxide hybridization colloidal sol infiltrate through step 1) process after inorganic fibers；
4) prepare germanium oxide and zinc oxide hybridization aerogel composite: at 70 DEG C, make step 3) gained infiltration thing in germanium oxide and zinc oxide hybridization colloidal sol generation gelling, obtain germanium oxide and zinc oxide hybridization gel；After 40 DEG C of aging 35h, after ethanol or carbon dioxide supercritical fluid drying；Under inert gas helium is protected, germanium oxide and zinc oxide hybridization aerogel composite are carried out 800 DEG C of high-temperature calcinations, obtains germanium oxide and zinc oxide hybridization aerogel composite。
Embodiment 4
1) process of inorganic fibers: at 180 DEG C, dry inorfil 4 hours；After inorfil is immersed the surface treatment agent solution by inorfil, distilled water, surfactant and proportions that coupling agent weight ratio is 1:3:0.007:0.014, dry 3 hours at 180 DEG C, cool down to obtain inorfil after surface treatment；
Wherein, inorfil is polycrystalline mullite fibre, and the step of the preparation method of polycrystalline mullite fibre is: is dissolved in by aluminium powder in the mixture of formic acid and acetic acid, is heated to reflux, and prepares aluminium triformate and aluminium acetate mixed sols solution；Aluminium triformate and aluminium acetate mixed sols add the acidic silicasol of removing sodium；Solution after mix homogeneously adds spinning-aid agent；Mixed liquor adds surfactant；Spinning solution adds citric acid；Above-mentioned mixed liquor is fibroblast under getting rid of strand part；Polycrystalline alumina fiber precursor is dried；Finally it is heated polycrystal alumina precursor at 1000 DEG C processing；Obtain polycrystalline mullite fibre；
2) preparation of germanium oxide and zinc oxide hybridization colloidal sol: be 0.5:1:40:30:0.2:10 according to mol ratio by germanium chloride, zinc chloride, alcohols material, deionized water, expoxy propane and catalyst-4Proportions mixed liquor, stirring 15min stand after, obtain germanium oxide and zinc oxide hybridization colloidal sol；
3) infiltration: by step 2) germanium oxide and zinc oxide hybridization colloidal sol infiltrate through step 1) process after inorganic fibers；
4) prepare germanium oxide and zinc oxide hybridization aerogel composite: at 65 DEG C, make step 3) gained infiltration thing in germanium oxide and zinc oxide hybridization colloidal sol generation gelling, obtain germanium oxide and zinc oxide hybridization gel；After 45 DEG C of aging 30h, after ethanol or carbon dioxide supercritical fluid drying；Under inert nitrogen gas is protected, germanium oxide and zinc oxide hybridization aerogel composite are carried out 900 DEG C of high-temperature calcinations, obtains germanium oxide and zinc oxide hybridization aerogel composite。
Embodiment 5
1) process of inorganic fibers: at 175 DEG C, dry inorfil 4 hours；After inorfil is immersed the surface treatment agent solution by inorfil, distilled water, surfactant and proportions that coupling agent weight ratio is 1:4:0.007:0.018, dry 2 hours at 220 DEG C, cool down to obtain inorfil after surface treatment；
Wherein, inorfil is polycrystalline mullite fibre, and the step of the preparation method of polycrystalline mullite fibre is: is dissolved in by aluminium powder in the mixture of formic acid and acetic acid, is heated to reflux, and prepares aluminium triformate and aluminium acetate mixed sols solution；Aluminium triformate and aluminium acetate mixed sols add the acidic silicasol of removing sodium；Solution after mix homogeneously adds spinning-aid agent；Mixed liquor adds surfactant；Spinning solution adds lactic acid；Above-mentioned mixed liquor is fibroblast under getting rid of strand part；Polycrystalline alumina fiber precursor is dried；Finally it is heated polycrystal alumina precursor at 1200 DEG C processing；Obtain polycrystalline mullite fibre；
2) preparation of germanium oxide and zinc oxide hybridization colloidal sol: be 1:2:35:25:0.4:10 according to mol ratio by germanium chloride, zinc chloride, alcohols material, deionized water, expoxy propane and catalyst-2Proportions mixed liquor, stirring 18min stand after, obtain germanium oxide and zinc oxide hybridization colloidal sol；
3) infiltration: by step 2) germanium oxide and zinc oxide hybridization colloidal sol infiltrate through step 1) process after inorganic fibers；
4) prepare germanium oxide and zinc oxide hybridization aerogel composite: at 75 DEG C, make step 3) gained infiltration thing in germanium oxide and zinc oxide hybridization colloidal sol generation gelling, obtain germanium oxide and zinc oxide hybridization gel；After 40 DEG C of aging 45h, after ethanol or carbon dioxide supercritical fluid drying；Under noble gas neon is protected, germanium oxide and zinc oxide hybridization aerogel composite are carried out 1000 DEG C of high-temperature calcinations, obtains germanium oxide and zinc oxide hybridization aerogel composite。
Embodiment 6
1) process of inorganic fibers: at 200 DEG C, dry inorfil 5 hours；After inorfil is immersed the surface treatment agent solution by inorfil, distilled water, surfactant and proportions that coupling agent weight ratio is 1:3:0.006:0.016, dry 3 hours at 200 DEG C, cool down to obtain inorfil after surface treatment；
Wherein, inorfil is polycrystalline mullite fibre, and the step of the preparation method of polycrystalline mullite fibre is: is dissolved in by aluminium powder in the mixture of formic acid and acetic acid, is heated to reflux, and prepares aluminium triformate and aluminium acetate mixed sols solution；Aluminium triformate and aluminium acetate mixed sols add the acidic silicasol of removing sodium；Solution after mix homogeneously adds spinning-aid agent；Mixed liquor adds surfactant；Spinning solution adds tartaric acid；Above-mentioned mixed liquor is fibroblast when winding-up；Polycrystalline alumina fiber precursor is dried；Finally it is heated polycrystal alumina precursor at 1100 DEG C processing；Obtain polycrystalline mullite fibre；
2) preparation of germanium oxide and zinc oxide hybridization colloidal sol: be 1:2:35:40:0.5:10 according to mol ratio by germanium chloride, zinc chloride, alcohols material, deionized water, expoxy propane and catalyst-3Proportions mixed liquor, stirring 14min stand after, obtain germanium oxide and zinc oxide hybridization colloidal sol；
3) infiltration: by step 2) germanium oxide and zinc oxide hybridization colloidal sol infiltrate through step 1) process after inorganic fibers；
4) prepare germanium oxide and zinc oxide hybridization aerogel composite: at 65 DEG C, make step 3) gained infiltration thing in germanium oxide and zinc oxide hybridization colloidal sol generation gelling, obtain germanium oxide and zinc oxide hybridization gel；After 25 DEG C of aging 35h, after ethanol or carbon dioxide supercritical fluid drying；Under inert gas helium is protected, germanium oxide and zinc oxide hybridization aerogel composite are carried out 1100 DEG C of high-temperature calcinations, obtains germanium oxide and zinc oxide hybridization aerogel composite。
The raw materials used kind of embodiment and ratio thereof are listed in the table below 1。
Table 1
In embodiment, gained properties of sample is listed in the table below 2。
Table 2
Above example is only in order to illustrate that technical scheme is not intended to limit; those of ordinary skill in the field are to be understood that; the specific embodiment of the present invention can being modified with reference to above-described embodiment or equivalent replacement, these are all being applied within the claims awaited the reply without departing from any amendment or equivalent replacement of spirit and scope of the invention。
Claims (9)
1. the preparation method of a germanium oxide and zinc oxide hybridization aerogel composite, it is characterised in that described composite includes germanium oxide and zinc oxide hybridization aeroge, inorganic fibers, and described preparation method comprises the steps:
1) process of inorganic fibers: at 150～200 DEG C, dry inorfil 4～6 hours；Inorfil is immersed after processing by weight the surface treatment agent solution for the preparation of the inorfil of ratio of 1:2～4:0.004～0.008:0.012～0.02, distilled water, surfactant and coupling agent, dry 1～3 hour at 160～220 DEG C, cooling；
Wherein, described inorfil is polycrystalline mullite fibre, and the preparation method of described polycrystalline mullite fibre comprises the following steps: is dissolved in by aluminium powder in the mixture of formic acid and acetic acid, is heated to reflux, and prepares aluminium triformate and aluminium acetate mixed sols solution；Aluminium triformate and aluminium acetate mixed sols add the acidic silicasol of removing sodium；Solution after mix homogeneously adds spinning-aid agent；Mixed liquor adds surfactant；Spinning solution adds tartaric acid, one or several of citric acid or lactic acid；Above-mentioned mixed liquor is in winding-up or gets rid of fibroblast under strand part；By polycrystalline alumina fiber precursor preliminarily dried；Finally it is heated polycrystal alumina precursor at 500～1400 DEG C processing；
2) preparation of germanium oxide and zinc oxide hybridization colloidal sol: be 0.5～1:0.5～2:10～50:10～40:0.05～0.5:10 according to mol ratio by germanium chloride, zinc chloride, alcohols material, deionized water, expoxy propane and catalyst-4～10-2Proportions mixed liquor, stirring 10～20min stand after, obtain germanium oxide and zinc oxide hybridization colloidal sol；
3) infiltration: by step 2) germanium oxide and zinc oxide hybridization colloidal sol infiltrate through step 1) process after inorganic fibers；
4) prepare germanium oxide and zinc oxide hybridization aerogel composite: at 50～80 DEG C, make step 3) gained infiltration thing in germanium oxide and zinc oxide hybridization colloidal sol generation gelling, obtain germanium oxide and zinc oxide hybridization gel；At 20～50 DEG C after aging 20～50h, after ethanol or carbon dioxide supercritical fluid drying；Under inert gas shielding, germanium oxide and zinc oxide hybridization aerogel composite are carried out high-temperature calcination, obtain germanium oxide and zinc oxide hybridization aerogel composite。
2. the preparation method of a kind of germanium oxide as claimed in claim 1 and zinc oxide hybridization aerogel composite, it is characterised in that described step 4) in noble gas be nitrogen, helium or neon。
3. the preparation method of a kind of germanium oxide as claimed in claim 1 and zinc oxide hybridization aerogel composite, it is characterised 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 zinc oxide hybridization aerogel composite, it is characterised in that described alcohols material is methanol, ethanol, propanol or butanol。
5. the preparation method of a kind of germanium oxide as claimed in claim 1 and zinc oxide hybridization aerogel composite, it is characterised in that described catalyst is hydrochloric acid, sulphuric acid, phosphoric acid, formic acid, acetic acid, ethanedioic acid or Fluohydric acid.。
6. the preparation method of a kind of germanium oxide as claimed in claim 1 and zinc oxide hybridization aerogel composite, it is characterized in that, described coupling agent is gamma-aminopropyl-triethoxy-silane, N-β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane, MTMS or vinyltrimethoxy silane。
7. the preparation method of a kind of germanium oxide as claimed in claim 1 and zinc oxide hybridization aerogel composite, it is characterized in that, described surfactant is dodecyl dimethyl benzyl ammonium chloride, dodecylbenzene sodium sulfonate, dimethyl dodecyl amine oxide, dodecyl-dimethyl amine second lactone or glycerin polyoxyethylene ether。
8. such as the preparation method of the claim 1～7 germanium oxide as described in any one and zinc oxide hybridization aerogel composite, it is characterised in that germanium oxide prepared by described method and zinc oxide hybridization gel specific surface area 250～300m2/ g, porosity 80～90%。
9. such as the preparation method of the claim 1～7 germanium oxide as described in any one and zinc oxide hybridization aerogel composite, it is characterized in that, germanium oxide that described method is prepared and zinc oxide hybridization aerogel composite thermal conductivity at 1000 DEG C are less than 0.035w/m k, and shrinkage factor is less than 3.4%。
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