CN105540644A - Preparation method for germanium oxide and indium oxide hybrid aerogel composite material - Google Patents
Preparation method for germanium oxide and indium oxide hybrid aerogel composite material Download PDFInfo
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- CN105540644A CN105540644A CN201610067328.4A CN201610067328A CN105540644A CN 105540644 A CN105540644 A CN 105540644A CN 201610067328 A CN201610067328 A CN 201610067328A CN 105540644 A CN105540644 A CN 105540644A
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- germanium oxide
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- 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
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- 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
Abstract
The invention provides a preparation method for germanium oxide and indium 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 indium oxide hybrid aerogel with excellent performance is prepared for the first time. According to the technical scheme provided by the invention, germanium oxide and indium 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 250-300m<2>/g, the density is 0.13-0.20g/m<3>, and the porosity is 80-90%. 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 Indium sesquioxide 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 Indium sesquioxide 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 Indium sesquioxide hybrid aerogel matrix material; Technical scheme manufacture craft provided by the invention is simple, easy to operate, and prepares germanium oxide and the Indium sesquioxide hybrid aerogel of excellent performance first.
Realize the object of the invention technical scheme as follows:
A preparation method for germanium oxide and Indium sesquioxide hybrid aerogel matrix material, described matrix material comprises germanium oxide and Indium sesquioxide 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 mullite fiber, the preparation method of described mullite fiber comprises: take raw material by the stoichiometric ratio of element each in mullite fiber chemical formula, configuration colloid, then mullite amorphous fiber is made through fibroblast, oven dry binder removal, again fiber is loaded in the saggar be made up of electromagnetic wave transparent material, then saggar is put into professional microwave oven, under air or oxygen atmosphere, by adjustment microwave power, control temperature rise rate, be heated to thermal treatment temp, finally be cooled to room temperature, obtain mullite fiber; Described mullite fiber phase purity is high, grain-size 30 ~ 50nm, Fibre diameter 6 ~ 10 μm, and porosity is low;
2) preparation of germanium oxide and Indium sesquioxide hybrid collosol: the proportions mixed solution by germanium chloride, indium chloride, 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 Indium sesquioxide hybrid collosol;
3) infiltrate: by step 2) germanium oxide and the infiltration of Indium sesquioxide hybrid collosol through step 1) inorganic fibers after process;
4) prepare germanium oxide and Indium sesquioxide hybrid aerogel matrix material: at 50 ~ 80 DEG C, make step 3) gained infiltration thing in germanium oxide and Indium sesquioxide hybrid collosol generation gelling, obtain germanium oxide and Indium sesquioxide 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 Indium sesquioxide hybrid aerogel matrix material are carried out high-temperature calcination, obtain germanium oxide and Indium sesquioxide 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 Indium sesquioxide hybrid gel specific surface area 250 ~ 300m
2/ g, porosity 80 ~ 90%.The germanium oxide that described method is prepared and the thermal conductivity of Indium sesquioxide 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 Indium sesquioxide 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 Indium sesquioxide hybrid aerogel, and its excellent properties is specific surface area 250 ~ 300m
2/ more than g, density 0.13 ~ 0.20g/m
3, porosity 80 ~ 90%.
3, the germanium oxide prepared of technical scheme provided by the invention and the thermal conductivity of Indium sesquioxide 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 mullite fiber, the preparation method of mullite fiber comprises: take raw material by the stoichiometric ratio of element each in mullite fiber chemical formula, configuration colloid, then mullite amorphous fiber is made through fibroblast, oven dry binder removal, again fiber is loaded in the saggar be made up of electromagnetic wave transparent material, then saggar is put into professional microwave oven, under oxygen atmosphere, by adjustment microwave power, control temperature rise rate, be heated to thermal treatment temp, finally be cooled to room temperature, obtain mullite fiber; Described mullite fiber phase purity is high, grain-size 30nm, Fibre diameter 6 μm, and porosity is low;
2) preparation of germanium oxide and Indium sesquioxide hybrid collosol: be 1:0.5:10:10:0.05:10 according to mol ratio by germanium chloride, indium chloride, alcohols material, deionized water, propylene oxide and catalyzer
-4proportions mixed solution, stir 20min leave standstill after, obtain germanium oxide and Indium sesquioxide hybrid collosol;
3) infiltrate: by step 2) germanium oxide and the infiltration of Indium sesquioxide hybrid collosol through step 1) inorganic fibers after process;
4) prepare germanium oxide and Indium sesquioxide hybrid aerogel matrix material: at 80 DEG C, make step 3) gained infiltration thing in germanium oxide and Indium sesquioxide hybrid collosol generation gelling, obtain germanium oxide and Indium sesquioxide hybrid gel; After 50 DEG C of aging 20h, after supercritical drying; Under inert nitrogen gas protection, germanium oxide and Indium sesquioxide hybrid aerogel matrix material are carried out 600 DEG C of high-temperature calcinations, obtains germanium oxide and Indium sesquioxide 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 mullite fiber, the preparation method of mullite fiber comprises: take raw material by the stoichiometric ratio of element each in mullite fiber chemical formula, configuration colloid, then mullite amorphous fiber is made through fibroblast, oven dry binder removal, again fiber is loaded in the saggar be made up of electromagnetic wave transparent material, then saggar is put into professional microwave oven, under oxygen atmosphere, by adjustment microwave power, control temperature rise rate, be heated to thermal treatment temp, finally be cooled to room temperature, obtain mullite fiber; Described mullite fiber phase purity is high, grain-size 50nm, Fibre diameter 10 μm, and porosity is low;
2) preparation of germanium oxide and Indium sesquioxide hybrid collosol: be 0.5:2:50:40:0.5:10 according to mol ratio by germanium chloride, indium chloride, alcohols material, deionized water, propylene oxide and catalyzer
-2proportions mixed solution, stir 15min leave standstill after, obtain germanium oxide and Indium sesquioxide hybrid collosol;
3) infiltrate: by step 2) germanium oxide and the infiltration of Indium sesquioxide hybrid collosol through step 1) inorganic fibers after process;
4) prepare germanium oxide and Indium sesquioxide hybrid aerogel matrix material: at 50 DEG C, make step 3) gained infiltration thing in germanium oxide and Indium sesquioxide hybrid collosol generation gelling, obtain germanium oxide and Indium sesquioxide 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 Indium sesquioxide hybrid aerogel matrix material are carried out 1200 DEG C of high-temperature calcinations, obtains germanium oxide and Indium sesquioxide 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 mullite fiber, the preparation method of mullite fiber comprises: take raw material by the stoichiometric ratio of element each in mullite fiber chemical formula, configuration colloid, then mullite amorphous fiber is made through fibroblast, oven dry binder removal, again fiber is loaded in the saggar be made up of electromagnetic wave transparent material, then saggar is put into professional microwave oven, in air atmosphere, by adjustment microwave power, control temperature rise rate, be heated to thermal treatment temp, finally be cooled to room temperature, obtain mullite fiber; Described mullite fiber phase purity is high, grain-size 40nm, Fibre diameter 8 μm, and porosity is low;
2) preparation of germanium oxide and Indium sesquioxide hybrid collosol: be 1::30:20:0.1:10 according to mol ratio by germanium chloride, indium chloride, alcohols material, deionized water, propylene oxide and catalyzer
-3proportions mixed solution, stir 20min leave standstill after, obtain germanium oxide and Indium sesquioxide hybrid collosol;
3) infiltrate: by step 2) germanium oxide and the infiltration of Indium sesquioxide hybrid collosol through step 1) inorganic fibers after process;
4) prepare germanium oxide and Indium sesquioxide hybrid aerogel matrix material: at 70 DEG C, make step 3) gained infiltration thing in germanium oxide and Indium sesquioxide hybrid collosol generation gelling, obtain germanium oxide and Indium sesquioxide hybrid gel; After 40 DEG C of aging 35h, after ethanol or CO 2 supercritical drying; Under inert gas helium protection, germanium oxide and Indium sesquioxide hybrid aerogel matrix material are carried out 800 DEG C of high-temperature calcinations, obtains germanium oxide and Indium sesquioxide 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 mullite fiber, the preparation method of mullite fiber comprises: take raw material by the stoichiometric ratio of element each in mullite fiber chemical formula, configuration colloid, then mullite amorphous fiber is made through fibroblast, oven dry binder removal, again fiber is loaded in the saggar be made up of electromagnetic wave transparent material, then saggar is put into professional microwave oven, in air atmosphere, by adjustment microwave power, control temperature rise rate, be heated to thermal treatment temp, finally be cooled to room temperature, obtain mullite fiber; Described mullite fiber phase purity is high, grain-size 35nm, Fibre diameter 8 μm, and porosity is low;
2) preparation of germanium oxide and Indium sesquioxide hybrid collosol: be 0.5:1:40:30:0.2:10 according to mol ratio by germanium chloride, indium chloride, alcohols material, deionized water, propylene oxide and catalyzer
-4proportions mixed solution, stir 15min leave standstill after, obtain germanium oxide and Indium sesquioxide hybrid collosol;
3) infiltrate: by step 2) germanium oxide and the infiltration of Indium sesquioxide hybrid collosol through step 1) inorganic fibers after process;
4) prepare germanium oxide and Indium sesquioxide hybrid aerogel matrix material: at 65 DEG C, make step 3) gained infiltration thing in germanium oxide and Indium sesquioxide hybrid collosol generation gelling, obtain germanium oxide and Indium sesquioxide hybrid gel; After 45 DEG C of aging 30h, after ethanol or CO 2 supercritical drying; Under inert nitrogen gas protection, germanium oxide and Indium sesquioxide hybrid aerogel matrix material are carried out 900 DEG C of high-temperature calcinations, obtains germanium oxide and Indium sesquioxide 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 mullite fiber, the preparation method of mullite fiber comprises: take raw material by the stoichiometric ratio of element each in mullite fiber chemical formula, configuration colloid, then mullite amorphous fiber is made through fibroblast, oven dry binder removal, again fiber is loaded in the saggar be made up of electromagnetic wave transparent material, then saggar is put into professional microwave oven, under oxygen atmosphere, by adjustment microwave power, control temperature rise rate, be heated to thermal treatment temp, finally be cooled to room temperature, obtain mullite fiber; Described mullite fiber phase purity is high, grain-size 45nm, Fibre diameter 9 μm, and porosity is low;
2) preparation of germanium oxide and Indium sesquioxide hybrid collosol: be 1:2:35:25:0.4:10 according to mol ratio by germanium chloride, indium chloride, alcohols material, deionized water, propylene oxide and catalyzer
-2proportions mixed solution, stir 18min leave standstill after, obtain germanium oxide and Indium sesquioxide hybrid collosol;
3) infiltrate: by step 2) germanium oxide and the infiltration of Indium sesquioxide hybrid collosol through step 1) inorganic fibers after process;
4) prepare germanium oxide and Indium sesquioxide hybrid aerogel matrix material: at 75 DEG C, make step 3) gained infiltration thing in germanium oxide and Indium sesquioxide hybrid collosol generation gelling, obtain germanium oxide and Indium sesquioxide 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 Indium sesquioxide hybrid aerogel matrix material are carried out 1000 DEG C of high-temperature calcinations, obtains germanium oxide and Indium sesquioxide 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 mullite fiber, the preparation method of mullite fiber comprises: take raw material by the stoichiometric ratio of element each in mullite fiber chemical formula, configuration colloid, then mullite amorphous fiber is made through fibroblast, oven dry binder removal, again fiber is loaded in the saggar be made up of electromagnetic wave transparent material, then saggar is put into professional microwave oven, under oxygen atmosphere, by adjustment microwave power, control temperature rise rate, be heated to thermal treatment temp, finally be cooled to room temperature, obtain mullite fiber; Described mullite fiber phase purity is high, grain-size 50nm, Fibre diameter 6 μm, and porosity is low;
2) preparation of germanium oxide and Indium sesquioxide hybrid collosol: be 1:2:35:40:0.5:10 according to mol ratio by germanium chloride, indium chloride, alcohols material, deionized water, propylene oxide and catalyzer
-3proportions mixed solution, stir 14min leave standstill after, obtain germanium oxide and Indium sesquioxide hybrid collosol;
3) infiltrate: by step 2) germanium oxide and the infiltration of Indium sesquioxide hybrid collosol through step 1) inorganic fibers after process;
4) prepare germanium oxide and Indium sesquioxide hybrid aerogel matrix material: at 65 DEG C, make step 3) gained infiltration thing in germanium oxide and Indium sesquioxide hybrid collosol generation gelling, obtain germanium oxide and Indium sesquioxide hybrid gel; After 25 DEG C of aging 35h, after ethanol or CO 2 supercritical drying; Under inert gas helium protection, germanium oxide and Indium sesquioxide hybrid aerogel matrix material are carried out 1100 DEG C of high-temperature calcinations, obtains germanium oxide and Indium sesquioxide hybrid aerogel matrix material.
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 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 Indium sesquioxide hybrid aerogel matrix material, is characterized in that, described matrix material comprises germanium oxide and Indium sesquioxide 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 mullite fiber, the preparation method of described mullite fiber comprises: take raw material by the stoichiometric ratio of element each in mullite fiber chemical formula, configuration colloid, then mullite amorphous fiber is made through fibroblast, oven dry binder removal, again fiber is loaded in the saggar be made up of electromagnetic wave transparent material, then saggar is put into professional microwave oven, under air or oxygen atmosphere, by adjustment microwave power, control temperature rise rate, be heated to thermal treatment temp, finally be cooled to room temperature, obtain mullite fiber; Described mullite fiber phase purity is high, grain-size 30 ~ 50nm, Fibre diameter 6 ~ 10 μm, and porosity is low;
2) preparation of germanium oxide and Indium sesquioxide 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, indium chloride, alcohols material, deionized water, propylene oxide and catalyzer
-4~ 10
-2proportions mixed solution, stir 10 ~ 20min leave standstill after, obtain germanium oxide and Indium sesquioxide hybrid collosol;
3) infiltrate: by step 2) germanium oxide and the infiltration of Indium sesquioxide hybrid collosol through step 1) inorganic fibers after process;
4) prepare germanium oxide and Indium sesquioxide hybrid aerogel matrix material: at 50 ~ 80 DEG C, make step 3) gained infiltration thing in germanium oxide and Indium sesquioxide hybrid collosol generation gelling, obtain germanium oxide and Indium sesquioxide 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 Indium sesquioxide hybrid aerogel matrix material are carried out high-temperature calcination, obtain germanium oxide and Indium sesquioxide hybrid aerogel matrix material.
2. the preparation method of a kind of germanium oxide as claimed in claim 1 and Indium sesquioxide 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 Indium sesquioxide 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 Indium sesquioxide 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 Indium sesquioxide 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 Indium sesquioxide 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 Indium sesquioxide 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 Indium sesquioxide hybrid aerogel matrix material, it is characterized in that, germanium oxide prepared by described method and Indium sesquioxide hybrid gel specific surface area 250 ~ 300m
2/ g, porosity 80 ~ 90%.
9. as the germanium oxide of claim 1 ~ 7 as described in any one and the preparation method of Indium sesquioxide hybrid aerogel matrix material, it is characterized in that, the germanium oxide that described method is prepared and the thermal conductivity of Indium sesquioxide 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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| CN111661872A (en) * | 2020-06-16 | 2020-09-15 | 华东师范大学 | Preparation method of nano germanium oxide |
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Application publication date: 20160504 |