CN101774592A - High heat insulation transparent SiO2 aerogel film material and preparation method thereof - Google Patents
High heat insulation transparent SiO2 aerogel film material and preparation method thereof Download PDFInfo
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- CN101774592A CN101774592A CN200910193595A CN200910193595A CN101774592A CN 101774592 A CN101774592 A CN 101774592A CN 200910193595 A CN200910193595 A CN 200910193595A CN 200910193595 A CN200910193595 A CN 200910193595A CN 101774592 A CN101774592 A CN 101774592A
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Abstract
The invention discloses a high heat insulation transparent SiO2 aerogel film material and a preparation method thereof, wherein the preparation method is realized by adopting a sol-gel technique to control the technological condition via using acid/alkali two-step catalytic method, and using hexamethyldisilazane (HMDS) to carry out organic hydrophobic modification on the surface of colloidal particles. The film material and the preparation method thereof are characterized in that the compound precursor sol has stable property, moderate viscidity and long gel time; the prepared aerogel heat insulation film not only has high porosity, low density and low hear conducting coefficient, but also has high light transmissivity and low refractive index, therefore, it is not only fits for the request of high head insulation, but also fits for the transparency request, and can be used as high heat insulation transparent layer of the landing glass of high-rise building and car glass; the row material for preparing aerogel heat insulation film is low in cost, and benefits for realizing commercial application.
Description
Technical field
The invention belongs to porous heat-insulating transparent oxide film material field, particularly a kind of high heat insulation transparent SiO
2Aerogel film material and preparation method thereof.
Background technology
SiO
2Aerogel (aergoels) is the network structure that is agglomerated into nanoporous by colloidal particle or high-polymer molecular mutually, is full of a kind of high dispersive solid-state material of gaseous state dispersion medium in hole, has continuous random fractal structure.SiO
2The nanoporous form of aerogel has excellent characteristic.Because SiO
2The particle of aerogel nanoscale and void distribution thereof, the tiny three-dimensional net structure that is connected with each other constitutes complicated zigzag hot-fluid transmission path, the nano-porous structure aperture has extremely low thermal conductivity, SiO much smaller than the mean free path of heat conduction carrier (as phonon etc.)
2Aerogel can be anti-1050 ℃, thereby can be applicable to fields such as space flight and aviation, building energy conservation, communications and transportation, has a extensive future.
Adopt sol-gel method to prepare SiO
2Aerogel, owing to have a large amount of organic solvents in the hole of its network structure, solvent sharply volatilizees in the film drying process, causes that capillary tension causes film to shrink, and makes the porosity of film sharply reduce mis-behave.In order to address this problem, research both at home and abroad adopts the supercritical drying drying process to improve the porosity and the performance thereof of film, because this technology cost is higher, High Temperature High Pressure has certain danger simultaneously, is unfavorable for the scale operation and the practical application of aerogel.In recent years, begin one's study both at home and abroad and adopt non-supercritical drying process---the surface modifying method that improves film porosity and performance, realize the bounce-back of film structure in drying process, keep the nano-porous structure of film.SiO
2The heat-proof quality of aerogel not only depends on the nanoporous network structure that it is inner, and depends on its hydrophobic property, at present, adopts trimethylchlorosilane (TMCS) to carry out silanization for the modifying and decorating of film more and handles, at SiO
2Introduce hydrophobic grouping-Si-CH in the network
3, increase the hydrophobic performance of rete thus.Though adopt the TMCS modification can improve SiO
2Aerogel heat-proof quality and hydrophobic performance, but because remaining Cl is arranged in its weave construction
-, thereby reduce SiO
2The light transmission rate of aerogel is unfavorable for that it keeps the good transparency.
Summary of the invention
In order to solve above-mentioned the deficiencies in the prior art part, primary and foremost purpose of the present invention is to provide a kind of high heat insulation transparent SiO
2The preparation method of aerogel film material; This method technology is simple, cost is low, the stable performance of synthetic precursor sol.
Another purpose of the present invention is to provide a kind of high heat insulation transparent SiO of method for preparing
2Aerogel film material; The nanoporous SiO that this material is the porosity height, the transparency is high, thermal conductivity is low
2The aerogel heat-proof thin-film material.
A further object of the present invention is to provide above-mentioned high heat insulation transparent SiO
2The application of aerogel film material.
Purpose of the present invention is achieved through the following technical solutions: a kind of high heat insulation transparent SiO
2The preparation method of aerogel film material comprises following operation steps:
(1) SiO
2The preparation of precursor sol:
A, with tetraethoxy, dehydrated alcohol and deionized water with 1.0: (5.0～5.4): the mixed in molar ratio of (3.0～4.0), at room temperature violent stirring is hydrolyzed/polycondensation; Add the hydrochloric acid ethanol solution, continuously stirring obtains the acid catalyzed reaction product; The hydrogenchloride in the described hydrochloric acid ethanol solution and the mol ratio of tetraethoxy are 1.0: (5.0 * 10
-4～5.5 * 10
-4);
B, add dilute ammonia solution in steps A gained acid catalyzed reaction product, the ammoniacal liquor in the described dilute ammonia solution and the mol ratio of tetraethoxy are (3.5 * 10
-2～3.75 * 10
-2): 1.0; At room temperature stir, leave standstill, obtain SiO
2Precursor sol;
(2) SiO
2The preparation of wet gel thin-film carrier:
Be full of under the atmosphere of dehydrated alcohol, clean transparent solid shape carrier is being immersed SiO
2In the precursor sol, keep 25～35s, with the speed of 5～30cm/min from SiO
2Lift out in the precursor sol, obtain SiO
2The wet gel thin-film carrier;
(3) SiO
2The preparation of aerogel heat-proof film:
With step (2) gained SiO
2The wet gel thin-film carrier places aging 18～24h of dehydrated alcohol and normal hexane to soak 8～12h successively; Immerse then that to contain the hexamethyldisilazane volumetric concentration be the surface modification of carrying out silanization in 7～9% the hexane solution, the time is 12～18 hours; SiO through surface modification
2After the wet gel thin-film carrier is used normal hexane soaking and washing 9～12h, dry under the condition of normal pressure, obtain SiO
2The aerogel heat-proof film.
The volumetric molar concentration of the described hydrochloric acid ethanol solution of steps A is 0.01mol/L; Described violent stirring is to adopt magnetic stirring apparatus to stir under 800～1000r/min rotating speed; The time of described hydrolysis/condensation reaction is 30～45min; Time 60～the 80min of described continuously stirring.
The volumetric molar concentration of the described dilute ammonia solution of step B is 1mol/L; The time of described stirring is 3～5min; The described time of leaving standstill is 50～70min.
To the described SiO of step B
2Add stablizer in the precursor sol, can make colloidal sol keep suitable viscosity in a long time; Described SiO
2The volume ratio of precursor sol and stablizer is 1: (0.4～0.5) can make dissolved adhesiveness keep more than 6 months.Preferred methyl ethyl diketone (the CH of described stablizer
3COCH
2COCH
3).
The described transparent solid shape carrier of step (2) is slide glass, eyeglass or wafer; The transparent solid shape carrier of described cleaning is with the transparent solid shape carrier ultrasonic cleaning 1h in dehydrated alcohol of elder generation, places deionized water for ultrasonic to clean 30min again, and drying obtains clean transparent solid shape carrier then.
The described SiO of step (3)
2The preparation of aerogel heat-proof film is to carry out under 45～55 ℃ of constant temperatures.
The described exsiccant time of step (3) is 24～30h.
A kind of high heat insulation transparent SiO according to method for preparing
2Aerogel.
Above-mentioned high heat insulation transparent SiO
2Aerogel can be applicable to prepare the fall high heat insulation transparent layer of window glass and vehicle glass of high-rise.
Principle of the present invention is: the present invention in conjunction with the organic-silylation process of hexamethyldisilazane to micelle, prepares the SiO of high porosity, high transparent, low thermal conductivity by adopting the technology of sol-gel technique and acid/alkali two-step catalysis under condition of normal pressure
2Aerogel film material.Simultaneously, at SiO
2In the preparation process of precursor,, realize at room temperature can stablizing the precursor sol of depositing more than 6 months by in colloidal sol, adding chemical stabilizer.
In step (3) with SiO
2Wet gel film slide glass places dehydrated alcohol to wear out, to prevent the volatilization of film surface solvent; With SiO
2Wet gel film slide glass places normal hexane to soak to be in order to replace the dehydrated alcohol of gel film network structure, and removes moisture and the unreacted presoma that remains in the sol-gel process in the hole, strengthens the network structure of gel; Will be through the SiO of modification
2Wet gel film slide glass normal hexane soaking and washing is to remove the by product in the silanization process.
The present invention compared with prior art has following advantage and beneficial effect: the stable performance of (1) configuration synthetic precursor sol, and modest viscosity, gel time is long, can deposit more than half a year; (2) prepared SiO
2The aerogel heat-proof film not only has high porosity, low density and low thermal conductivity, and have light high permeability and a low-refraction, meet the requirement of heat-insulation transparent, both can be used as the fall thermofin of window glass of high-rise, can be used as the thermal insulation layer of vehicle glass again; Improve energy-saving effect; (3) preparation SiO
2The material cost that the aerogel heat-proof film is adopted is low, helps realizing the commercialization application.
Description of drawings
Fig. 1 is the high heat insulation transparent SiO of the present invention's preparation
2The shape appearance figure of aerogel heat-proof thin-film material sample, a figure are the surface topography map of sample, and b figure is the cross section shape appearance figure of sample.
Embodiment
The present invention is described in further detail below in conjunction with embodiment and accompanying drawing, but embodiments of the present invention are not limited thereto.
Embodiment 1
(1) preparation of acid catalyst solutions and alkaline catalysts solution
Measure concentrated hydrochloric acid (HCl) and the 7.44mL strong aqua (NH of 0.0418mL
4OH), be dissolved in the dehydrated alcohol (CH of 99.9164ml respectively
3CH
2OH) and 92.56ml deionized water (H
2O) in, being mixed with concentration is the hydrochloric acid ethanol solution of 0.01mol/L and the dilute ammonia solution of 1mol/L.
(2) SiO
2The preparation of precursor sol
A, 40ml tetraethoxy, 14.66ml dehydrated alcohol and 2.72ml deionized water added successively in the beaker of a dried and clean and mix, adopt magnetic stirring apparatus violent stirring at room temperature, be hydrolyzed/polycondensation 35min; Add 2.5ml hydrochloric acid ethanol solution, continuously stirring 60min obtains the acid catalyzed reaction product;
B, in steps A gained acid catalyzed reaction product, add the 1.76ml dilute ammonia solution, at room temperature stir 3min, leave standstill 55min, obtain SiO
2Precursor sol;
(3) SiO
2The preparation of wet gel film slide glass:
Be full of under the atmosphere of dehydrated alcohol, clean slide glass (76cm * 26cm size) is being immersed SiO
2In the precursor sol, keep 30s, with the speed of 20cm/min from SiO
2Lift out in the precursor sol, obtain SiO
2Wet gel film slide glass;
(3) SiO
2The preparation of aerogel heat-proof film:
With step (2) gained SiO
2Wet gel film slide glass places aging 18h of dehydrated alcohol and normal hexane to soak 12h successively; Immerse then that to contain the hexamethyldisilazane volumetric concentration be the surface modification of carrying out silanization in 7% the hexane solution, the time is 12 hours; SiO through surface modification
2After wet gel film slide glass was used normal hexane soaking and washing 12h, drying was 24 hours under the condition of normal pressure, obtains SiO
2The aerogel heat-proof film; Said process all is to carry out in 50 ℃ thermostat container.
Gained SiO
2The shape appearance figure of aerogel heat-proof film as shown in Figure 1, a is a surface topography map, b is the cross section shape appearance figure.
To gained SiO
2The aerogel heat-proof film carries out the test of performance perameter, and the result is as follows:
Specific refractory power: 1.085～1.096;
Density (g/cm
3): 0.407～0.459
Porosity: 79.03～82.18;
Light transmission rate:＞90%
Thermal conductivity (W/mK) (room temperature): 0.0274～0.0352.
Embodiment 2
(1) preparation of acid catalyst solutions and alkaline catalysts solution
Measure concentrated hydrochloric acid (HCl) and the 7.44mL strong aqua (NH of 0.0418mL
4OH), be dissolved in the dehydrated alcohol (CH of 99.9164ml respectively
3CH
2OH) and 92.56ml deionized water (H
2O) in, being mixed with concentration is the hydrochloric acid ethanol solution of 0.01mol/L and the dilute ammonia solution of 1mol/L.
(2) SiO
2The preparation of precursor sol
A, 30ml tetraethoxy, 11.43ml dehydrated alcohol and 2.38ml deionized water added successively in the beaker of a dried and clean and mix, adopt magnetic stirring apparatus violent stirring at room temperature, be hydrolyzed/polycondensation 30min; Add 2.06ml hydrochloric acid ethanol solution, continuously stirring 80min obtains the acid catalyzed reaction product;
B, in steps A gained acid catalyzed reaction product, add the 1.41ml dilute ammonia solution, at room temperature stir 5min, leave standstill 50min, obtain SiO
2Precursor sol;
(3) SiO
2The preparation of wet gel film slide glass:
Be full of under the atmosphere of dehydrated alcohol, clean eyeglass (80cm * 30cm size) is being immersed SiO
2In the precursor sol, keep 25s, with the speed of 25cm/min from SiO
2Lift out in the precursor sol, obtain SiO
2Wet gel film eyeglass;
(3) SiO
2The preparation of aerogel heat-proof film:
With step (2) gained SiO
2Wet gel film eyeglass places aging 20h of dehydrated alcohol and normal hexane to soak 8h successively; Immerse then that to contain the hexamethyldisilazane volumetric concentration be the surface modification of carrying out silanization in 8% the hexane solution, the time is 15 hours; SiO through surface modification
2After wet gel film eyeglass was used normal hexane soaking and washing 9h, drying was 26 hours under the condition of normal pressure, obtains SiO
2The aerogel heat-proof film; Said process all is to carry out in 50 ℃ thermostat container.
To gained SiO
2The aerogel heat-proof film carries out the test of performance perameter, and the result is as follows:
Specific refractory power: 1.076～1.097;
Density (g/cm
3): 0.364～0.464
Porosity: 78.80～83.96;
Light transmission rate:＞90%
Thermal conductivity (W/mK) (room temperature): 0.0270～0.0319.
Embodiment 3
(1) preparation of acid catalyst solutions and alkaline catalysts solution
Measure concentrated hydrochloric acid (HCl) and the 7.44mL strong aqua (NH of 0.0418mL
4OH), be dissolved in the dehydrated alcohol (CH of 99.9164ml respectively
3CH
2OH) and 92.56ml deionized water (H
2O) in, being mixed with concentration is the hydrochloric acid ethanol solution of 0.01mol/L and the dilute ammonia solution of 1mol/L.
(2) SiO
2The preparation of precursor sol
A, 50ml tetraethoxy, 19.79ml dehydrated alcohol and 4.52ml deionized water added successively in the beaker of a dried and clean and mix, adopt magnetic stirring apparatus violent stirring at room temperature, be hydrolyzed/polycondensation 45min; Add 3.77ml hydrochloric acid ethanol solution, continuously stirring 66min obtains the acid catalyzed reaction product;
B, in steps A gained acid catalyzed reaction product, add the 2.27ml dilute ammonia solution, at room temperature stir 4min, leave standstill 70min, obtain SiO
2Precursor sol;
(3) SiO
2The preparation of wet gel film slide glass:
Be full of under the atmosphere of dehydrated alcohol, clean wafer (60cm * 18cm size) is being immersed SiO
2In the precursor sol, keep 28s, with the speed of 24cm/min from SiO
2Lift out in the precursor sol, obtain SiO
2The wet gel thin film wafers;
(3) SiO
2The preparation of aerogel heat-proof film:
With step (2) gained SiO
2The wet gel thin film wafers places aging 24h of dehydrated alcohol and normal hexane to soak 8h successively; Immerse then that to contain the hexamethyldisilazane volumetric concentration be the surface modification of carrying out silanization in 9% the hexane solution, the time is 16 hours; SiO through surface modification
2After the wet gel thin film wafers was used normal hexane soaking and washing 10h, drying was 30 hours under the condition of normal pressure, obtains SiO
2The aerogel heat-proof film; Said process all is to carry out in 50 ℃ thermostat container.
To gained SiO
2The aerogel heat-proof film carries out the test of performance perameter, and the result is as follows:
Specific refractory power: 1.079～1.088;
Density (g/cm
3): 0.378～0.421;
Porosity: 81.45～83.35;
Light transmission rate:＞90%
Thermal conductivity (W/mK) (room temperature): 0.0260～0.0304.
The foregoing description is a preferred implementation of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. high heat insulation transparent SiO
2Aerogel film material and preparation method thereof is characterized in that comprising following operation steps:
(1) SiO
2The preparation of precursor sol:
A, with tetraethoxy, dehydrated alcohol and deionized water with 1.0: (5.0～5.4): the mixed in molar ratio of (3.0～4.0), at room temperature violent stirring is hydrolyzed/polycondensation; Add the hydrochloric acid ethanol solution, continuously stirring obtains the acid catalyzed reaction product; The hydrogenchloride in the described hydrochloric acid ethanol solution and the mol ratio of tetraethoxy are 1.0: (5.0 * 10
-4～5.5 * 10
-4);
B, add dilute ammonia solution in steps A gained acid catalyzed reaction product, the ammoniacal liquor in the described dilute ammonia solution and the mol ratio of tetraethoxy are (3.5 * 10
-2～3.75 * 10
-2): 1.0; At room temperature stir, leave standstill, obtain SiO
2Precursor sol;
(2) SiO
2The preparation of wet gel thin-film carrier:
Be full of under the atmosphere of dehydrated alcohol, clean transparent solid shape carrier is being immersed SiO
2In the precursor sol, keep 25～35s, with the speed of 5～30cm/min from SiO
2Lift out in the precursor sol, obtain SiO
2The wet gel thin-film carrier;
(3) SiO
2The preparation of aerogel heat-proof film:
With step (2) gained SiO
2The wet gel thin-film carrier places aging 18～24h of dehydrated alcohol and normal hexane to soak 8～12h successively; Immerse then that to contain the hexamethyldisilazane volumetric concentration be the surface modification of carrying out silanization in 7～9% the hexane solution, the time is 12～18 hours; SiO through surface modification
2After the wet gel thin-film carrier is used normal hexane soaking and washing 9～12h, dry under the condition of normal pressure, obtain SiO
2The aerogel heat-proof film.
2. a kind of high heat insulation transparent SiO according to claim 1
2Aerogel film material and preparation method thereof is characterized in that: the volumetric molar concentration of the described hydrochloric acid ethanol solution of steps A is 0.01mol/L; Described violent stirring is to adopt magnetic stirring apparatus to stir under 800～1000r/min rotating speed; The time of described hydrolysis/condensation reaction is 30～45min; Time 60～the 80min of described continuously stirring.
3. a kind of high heat insulation transparent SiO according to claim 1
2Aerogel film material and preparation method thereof is characterized in that: the volumetric molar concentration of the described dilute ammonia solution of step B is 1mol/L; The time of described stirring is 3～5min; The described time of leaving standstill is 50～70min.
4. a kind of high heat insulation transparent SiO according to claim 1
2Aerogel film material and preparation method thereof is characterized in that: to the described SiO of step B
2Add stablizer in the precursor sol, described SiO
2The volume ratio of precursor sol and stablizer is 1: (0.4～0.5).
5. a kind of high heat insulation transparent SiO according to claim 4
2Aerogel film material and preparation method thereof is characterized in that: described stablizer is a methyl ethyl diketone.
6. a kind of high heat insulation transparent SiO according to claim 1
2Aerogel film material and preparation method thereof is characterized in that: the described transparent solid shape carrier of step (2) is slide glass, eyeglass or wafer; The transparent solid shape carrier of described cleaning is with the transparent solid shape carrier ultrasonic cleaning 1h in dehydrated alcohol of elder generation, places deionized water for ultrasonic to clean 30min again, and drying obtains clean transparent solid shape carrier then.
7. a kind of high heat insulation transparent SiO according to claim 1
2Aerogel film material and preparation method thereof is characterized in that: the described SiO of step (3)
2The preparation of aerogel heat-proof film is to carry out under 45～55 ℃ of constant temperatures.
8. a kind of high heat insulation transparent SiO according to claim 1
2Aerogel film material and preparation method thereof is characterized in that: the described exsiccant time of step (3) is 24～30h.
9. high heat insulation transparent SiO according to each described method preparation of claim 1～8
2Aerogel film material.
10. according to the described high heat insulation transparent SiO of claim 9
2Aerogel film material can be applicable to prepare the fall high heat insulation transparent layer of window glass and vehicle glass of high-rise.
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