CN102757055A - Sol-gel preparation method for hydrophobic mesoporous silicon dioxide film - Google Patents
Sol-gel preparation method for hydrophobic mesoporous silicon dioxide film Download PDFInfo
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- CN102757055A CN102757055A CN2011101101059A CN201110110105A CN102757055A CN 102757055 A CN102757055 A CN 102757055A CN 2011101101059 A CN2011101101059 A CN 2011101101059A CN 201110110105 A CN201110110105 A CN 201110110105A CN 102757055 A CN102757055 A CN 102757055A
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- mesoporous silicon
- hydrophobicity
- silicon dioxde
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- sol
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Abstract
The invention aims to overcome the defects of poor hydrophobic modification effect, easiness in causing mesoporous structure damages during high-temperature treatment, and the like existing in the conventional method, and provides a sol-gel production process for preparing a hydrophobic mesoporous silicon dioxide film. The process has the advantages of simple experimental equipment, convenience for operating, ready availability of raw materials, low energy consumption, low cost, and industrial popularization and practical application values. The mesoporous silicon dioxide film disclosed by the invention has a good mesoporous structure and high hydrophobicity. The average pore diameter of the obtained hydrophobic mesoporous silicon dioxide film is 8 nanometers, the pore volume is 0.8g/cm<-3>, and the contact angle is up to 115 degrees. The improvement on the hydrophobicity of the mesoporous silicon dioxide film is an effective means for improving the performance, popularizing and applying.
Description
[technical field]
The present invention relates to a kind of technical field of semiconductors, specifically is a kind of process for preparing sol-gel of hydrophobicity mesoporous silicon dioxde film.
[background technology]
There is a large amount of surface hydroxyls in the mesoporous silicon dioxde film surface; These hydroxyls are active physics adsorption centers; They very easily form the water molecules film through the adsorption by hydrogen bond water molecules at hole surface; Between mesoporous film and the water avalanche that polycondensation finally causes pore structure will take place further, thereby influence its application in industry.Therefore, the hydrophobicity of raising mesoporous silicon dioxde film is the effective way that improves its performance and apply.The hydrophobicity that improves at present mesoporous silicon dioxde film mainly contains two kinds of methods: the one, eliminate the hydroxyl groups of hole surface as far as possible; Sample is handled under the high temperature more than 800 ℃; Make mutual polycondensation of silicon hydroxyl and final the disappearance, but the high-temperature calcination meeting causes very big destruction to network structure, may cause the densification of mould material to reduce the rate of permeation of gas; And in the process of cooling, hydroxylation possibly take place in fenestra surface again.The 2nd, through chemically modified; Hydrophobic treatment is carried out in the duct; Silane precursor and silicon hydroxyl with containing hydrophobic grouping react, and replace the hydroxyl that is connected on the Si atom with hydrophobic grouping, and the silicon hydroxyl that the lip-deep activity in duct is higher replaces with the inert hydrophobic grouping.About hydrophobically modified a lot of reports are arranged in the current document to mesopore molecular sieve, but fewer to the hydrophobically modified of mesoporous film report.
[summary of the invention]
The objective of the invention is to overcome existing method hydrophobically modified weak effect, be prone to cause shortcomings such as meso-hole structure destruction during pyroprocessing, a kind of sol-gel method production technique for preparing the hydrophobicity mesoporous silicon dioxde film is provided.Experimental installation of the present invention is simple, easy to operate, and raw material is easy to get, and the little cost of energy consumption is low, has industry and promotes and actual application value.
Mesoporous silicon dioxde film of the present invention has good meso-hole structure and strong hydrophobicity.
The present invention realizes through following technical scheme:
Hydrophobicity mesoporous silicon dioxde film sol-gel method method production technique involved in the present invention includes following steps:
Step 1 takes by weighing an amount of cetyl trimethylammonium bromide and is dissolved in wiring solution-forming in the ethanol of certain volume;
Step 2 adds certain proportion blended tetraethoxy and methyltriethoxy silane in step 1 gained solution, stir for some time under the room temperature;
Step 3 adds certain proportion blended HNO in the solution of step 2 gained
3, the second alcohol and water mixing solutions;
Step 4 is inserted the certain hour that refluxes in the water bath with thermostatic control with the solution of step 3 gained, again ageing for some time under the room temperature, obtains SiO
2Colloidal sol;
Step 5 is a coating liquid with the colloidal sol of step 4 gained, adopts the dip-coating method on the smooth glass sheet of washing through overpickling, alcohol, to apply SiO
2Film;
Step 6, moves in the constant temperature oven to complete drying then at the film for some time of seasoning at room temperature with the step 5 gained;
Step 7 is with the tube furnace (N of the dry gained film immigration of step 6 temperature programmed control
2Atmosphere) in, and calcine certain hour at a certain temperature and promptly get the hydrophobicity mesoporous silicon dioxde film.
Wherein
In the step 1, the concentration of said solution is 0.8g/L.
In the step 2, the molar ratio of tetraethoxy and methyltriethoxy silane is 3: 1, and the reaction times is at 1h-1.5h.
In the step 3, HNO
3, the second alcohol and water volume ratio be 1: 2: 3.
In the step 4, holding temperature is at 60 ℃-80 ℃, and soaking time is at 4h-6h, and digestion time is 10h-12h.
In the step 6, seasoning time 4h-5h, holding temperature is at 55 ℃-75 ℃, and soaking time is at 12h-20h.
In the step 7, calcining temperature is at 400 ℃-700 ℃, and soaking time is at 2h-5h.
The present invention has following beneficial effect: its mesoporous silicon dioxde film has kept good meso-hole structure, and mean pore size is at 5nm-10nm, and pore volume is 0.69-0.9g/cm
-3Hydrophobic methyl group successfully part has replaced the surperficial hydrophilic hydroxyl groups group of fenestra, and contact angle reaches more than 110 °, explains that it has good hydrophobicity; Simultaneously, the preparation method that the present invention adopted is simple, operation easily, and safer.
[embodiment]
Below in conjunction with embodiment the present invention is described further.Production technology of the present invention is to implement easily to this professional people.Present embodiment provided detailed embodiment and process, but protection scope of the present invention is not limited to following embodiment being to implement under the prerequisite with technical scheme of the present invention.The experimental technique of unreceipted actual conditions in the following example, usually according to normal condition, or the condition of advising according to manufacturer.
Embodiment
Take by weighing the 0.08g cetyl trimethylammonium bromide and be dissolved in wiring solution-forming in the ethanol that 100ml ethanol is dissolved in certain volume;
Add 1: 3 blended tetraethoxy of mol ratio and methyltriethoxy silane 3ml, stir 1h under the room temperature;
Add certain volume than 1: 2: 3 blended HNO
3, the second alcohol and water mixing solutions 30ml;
Solution is inserted the 4h that refluxes in the water bath with thermostatic control, and ageing 10h under the room temperature obtains SiO again
2Colloidal sol;
With the colloidal sol of gained is coating liquid, adopts the dip-coating method on the smooth glass sheet of washing through overpickling, alcohol, to apply SiO
2Film;
With film seasoning 5h at room temperature, move into dry 15h in 60 ℃ of constant temperature ovens then;
The film that drying is crossed moves into the tube furnace (N of temperature programmed control
2Atmosphere) in, and calcining 3h promptly gets the hydrophobicity mesoporous silicon dioxde film under 400 ℃.
The hydrophobicity mesoporous silicon dioxde film mean pore size that present embodiment obtains is at 8nm, and pore volume is 0.8g/cm
-3Contact angle reaches 115 °.
Utilize above-mentioned sol-gel process can prepare mesoporous silicon dioxde film, and reach its distinctive beneficial effect.
Claims (8)
1. the present invention is a kind of process for preparing sol-gel of hydrophobicity mesoporous silicon dioxde film, and mesoporous silicon dioxde film of the present invention has good meso-hole structure and strong hydrophobicity.The hydrophobicity mesoporous silicon dioxde film mean pore size that obtains is at 8nm, and pore volume is 0.8g/cm
-3Contact angle reaches 115 °.
2. the process for preparing sol-gel of a kind of hydrophobicity mesoporous silicon dioxde film according to claim 1 comprises the steps:
Step 1 takes by weighing an amount of cetyl trimethylammonium bromide and is dissolved in wiring solution-forming in the ethanol of certain volume;
Step 2 adds certain proportion blended tetraethoxy and methyltriethoxy silane in step 1 gained solution, stir for some time under the room temperature;
Step 3 adds certain proportion blended HNO in the solution of step 2 gained
3, the second alcohol and water mixing solutions;
Step 4 is inserted the certain hour that refluxes in the water bath with thermostatic control with the solution of step 3 gained, again ageing for some time under the room temperature, obtains SiO
2Colloidal sol;
Step 5 is a coating liquid with the colloidal sol of step 4 gained, adopts the dip-coating method on the smooth glass sheet of washing through overpickling, alcohol, to apply SiO
2Film;
Step 6, moves in the constant temperature oven to complete drying then at the film for some time of seasoning at room temperature with the step 5 gained;
Step 7 is with the tube furnace (N of the dry gained film immigration of step 6 temperature programmed control
2Atmosphere) in, and calcine certain hour at a certain temperature and promptly get the hydrophobicity mesoporous silicon dioxde film.
3. the process for preparing sol-gel of a kind of hydrophobicity mesoporous silicon dioxde film according to claim 2 is characterized in that in the step 1, and the concentration of said solution is 0.8g/L.
4. the process for preparing sol-gel of a kind of hydrophobicity mesoporous silicon dioxde film according to claim 2 is characterized in that in the step 2 that the molar ratio of tetraethoxy and methyltriethoxy silane is 3: 1, and the reaction times is at 1h-1.5h.
5. the process for preparing sol-gel of a kind of hydrophobicity mesoporous silicon dioxde film according to claim 2 is characterized in that in the step 3 HNO
3, the second alcohol and water volume ratio be 1: 2: 3.
6. the process for preparing sol-gel of a kind of hydrophobicity mesoporous silicon dioxde film according to claim 2 is characterized in that in the step 4, and holding temperature is at 60 ℃-80 ℃, and soaking time is at 4h-6h, and digestion time is 10h-12h.
7. the process for preparing sol-gel of a kind of hydrophobicity mesoporous silicon dioxde film according to claim 2 is characterized in that in the step 6, seasoning time 4h-5h, and holding temperature is at 55 ℃-75 ℃, and soaking time is at 12h-20h.
8. the process for preparing sol-gel of a kind of hydrophobicity mesoporous silicon dioxde film according to claim 2 is characterized in that in the step 7, and calcining temperature is at 400 ℃-700 ℃, and soaking time is at 2h-5h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101101059A CN102757055A (en) | 2011-04-28 | 2011-04-28 | Sol-gel preparation method for hydrophobic mesoporous silicon dioxide film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101101059A CN102757055A (en) | 2011-04-28 | 2011-04-28 | Sol-gel preparation method for hydrophobic mesoporous silicon dioxide film |
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|---|---|
| CN102757055A true CN102757055A (en) | 2012-10-31 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011101101059A Pending CN102757055A (en) | 2011-04-28 | 2011-04-28 | Sol-gel preparation method for hydrophobic mesoporous silicon dioxide film |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109592908A (en) * | 2019-01-25 | 2019-04-09 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of modified porous silica moistureproof antireflecting coating |
-
2011
- 2011-04-28 CN CN2011101101059A patent/CN102757055A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109592908A (en) * | 2019-01-25 | 2019-04-09 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of modified porous silica moistureproof antireflecting coating |
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Addressee: Kunshan Zhiji Material Technology Co., Ltd. Document name: Notification of Publication of the Application for Invention |
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Application publication date: 20121031 |