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Preparing method for nanometer porous silica thin-membrane

A silicon dioxide, optical thin film technology, applied in optics, optical components, instruments, etc., to achieve the effect of easy control of film thickness, small equipment investment, and uniform film composition

Inactive Publication Date: 2004-12-08
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no report on the preparation method of optical films with adjustable refractive index in China.

Method used

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  • Preparing method for nanometer porous silica thin-membrane
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  • Preparing method for nanometer porous silica thin-membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1: With tetraethyl orthosilicate (TEOS analytically pure), ethanol (adopting anhydrous, analytically pure), water as raw material, ammoniacal liquor as catalyst. First, mix ethyl orthosilicate, ammonia water, ethanol and deionized water at room temperature in a certain molar ratio (1:2.0:35:0.3), stir, and hydrolysis reaction occurs between ethyl orthosilicate and water under the catalysis of ammonia water At the same time, polycondensation reaction occurs between the hydroxyl groups formed in the hydrolysis reaction, and the sol with white opalescence is formed after standing and aging at room temperature for 3 days, and then the sol is refluxed at 80°C for 8 hours to remove the ammonia gas, and the obtained Alkaline SiO 2 Sol. Mix TEOS, hydrochloric acid (pH=1), ethanol and deionized water at a molar ratio of 1:2.3:38:0.245, stir, and leave to age at room temperature for 1.5 days to make acidic SiO 2 Sol. Acidic SiO 2 The sol was added to the basic SiO ...

Embodiment 2

[0017] Embodiment 2: Using ethyl orthosilicate (TEOS analytical grade), dehydrated alcohol (analytical grade), water as raw material, ammonia water as catalyst. Firstly, tetraethyl orthosilicate, ammonia water, ethanol and deionized water are mixed in a certain molar ratio (0.5:1.5:25:0.3), stirred, and left to stand at room temperature for 5 days to form a sol with white opalescence , and then the sol was refluxed at 90°C for 7 hours to remove the ammonia gas and make basic SiO 2 Sol. Mix TEOS, hydrochloric acid (pH=1), ethanol and deionized water at a molar ratio of 0.6:2.0:26:0.145, stir, and leave to age at room temperature for 1 day to form acidic SiO 2 Sol. Acidic SiO 2 The sol was added to the basic SiO at a molar ratio of 2.0:1.0 2 In the sol, mix and stir at room temperature and then reflux for 4.5 hours to obtain SiO with relatively stable performance. 2 Sol. Preparation of SiO on K9 film substrates by dip-pulling method in a clean environment with relative hum...

Embodiment 3

[0018] Embodiment 3: using ethyl orthosilicate (TEOS analytical grade), dehydrated alcohol (analytical grade), water as raw material, ammonia water as catalyst. Firstly, tetraethyl orthosilicate, ammonia water, ethanol and deionized water are mixed in a certain molar ratio (1:2.0:45:0.3), stirred, left to stand and aged at room temperature for 7 days, and a sol with white opalescence is formed. , and then the sol was refluxed at 110°C for 8 hours to remove the ammonia gas and make basic SiO 2 Sol. Mix TEOS, hydrochloric acid (pH=1), ethanol and deionized water at a molar ratio of 0.7:2.1:28:0.165, stir, and leave to age at room temperature for 2 days to form acidic SiO 2 Sol. Acidic SiO 2 The sol was added to the basic SiO at a molar ratio of 1.0:1.0 2 In the sol, mix and stir at room temperature and then reflux for 4 hours to obtain SiO with relatively stable performance. 2 Sol. Preparation of SiO on K9 film substrates by dip-pulling method in a clean environment with r...

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Abstract

The preparing method is as the follows, positive silester is used as presoma alcohol as solvent and ammonia water as well as hydrochloric acid as catalysts, they are become basic and acidic soliquid after hydrolyzation and polycondensation are carried out silica soliquid can be obtained by further polycondensation and hydrolyzation after basic silica soliquid is agitated in some acidic soliquid, a complete nanomultihole network structure which is not simply piled up can be formed by closely combining particles to be film when using acidic soliquid as coupling agent to link basic soliquid particles together.

Description

technical field [0001] The invention belongs to the technical field of optical film preparation, and in particular relates to a method for preparing a silicon dioxide optical film with a nanoporous structure. Background technique [0002] Traditional coating methods include physical methods such as magnetron sputtering, electron beam evaporation, and vacuum thermal evaporation. However, solid materials with a refractive index lower than 1.38 cannot be obtained by using existing materials, and the film structure prepared by physical methods is relatively simple. Coupled with the complex process and high cost of physical methods, the wide application of optical thin films is limited. The sol-gel method is a chemical synthesis preparation method for materials. Compared with traditional physical methods, it has the advantages of simple process, low cost, controllable structure, suitable for various substrates, continuously adjustable refractive index and can be adjusted at the m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G02B1/00
Inventor 沈军杨帆孙骐吴广明倪星元周斌
Owner TONGJI UNIV
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