CN100346176C - Multi-window wideband anti-reflection PS-SiO2 thin film and producing method thereof - Google Patents
Multi-window wideband anti-reflection PS-SiO2 thin film and producing method thereof Download PDFInfo
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- CN100346176C CN100346176C CNB2005100277797A CN200510027779A CN100346176C CN 100346176 C CN100346176 C CN 100346176C CN B2005100277797 A CNB2005100277797 A CN B2005100277797A CN 200510027779 A CN200510027779 A CN 200510027779A CN 100346176 C CN100346176 C CN 100346176C
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- colloidal sol
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Abstract
The present invention belongs to the technical field of an optical thin film material, more specifically a novel multiwindow broad band antireflection PS-SiO2 thin film and a preparation method thereof. In the preparation method of the novel multiwindow broad band antireflection PS-SiO2 thin film, after sio 2 collosol is formed by a sol-gel method, polystyrene (PS) is added, the film is formed by heat treatment and spin coating, Compared with the various modified SiO2 antireflection filmsin in days gone by, the antireflection film realizes realize broad band antireflection, and after the PS of difference molecular weights is incorporated, the luminous transmittance is high at 351 nms, 527 nm and 1054 nm, and all the maximum values exceed 98%. The novel multiwindow broad band antireflection PS-SiO2 thin film of the present invention is a good candidate alternate material of a KDP crystal antireflection film and can be applied to a super strength laser system for a high-energy nuclear fusion simulation experiment.
Description
Technical field
The invention belongs to the optical material technical field, be specifically related to a kind of novel collosol and gel SiO
2Anti-reflection film and preparation method thereof.
Technical background
Along with the experiment of inertial confinement fusion (ICF) development, it has been recognized that utilizing the high power short wavelength laser to practice shooting has great superiority, be one of direction of giving priority to of current high power laser system.Optical maser wavelength shortens, and can increase substantially target to the absorptivity of laser, reduce the influence of suprathermal electron in a large number, can also reduce stimulated Raman scattering and stimulated Brillouin scattering, can improve target practice efficiency greatly.Potassium dihydrogen phosphate (KDP) crystal is the requisite harmonic conversion optical element that the short wavelength is provided for inertial confinement fusion, and its significance level is self-evident.
Require it that extremely low surface reflection is arranged for the KDP crystal, be subjected to the destruction of unnecessary reflection to avoid sensitive element.All adopt coating technique for addressing this problem present countries in the world, and the porous silica anti-reflection film of Prepared by Sol Gel Method is because of making it to have good optical character and high laser-damaged threshold value is generally adopted.
China has obtained many technical progresses to the research work of sol-gel silica anti-reflection film, but some index of domestic anti-reflection film is compared with the leading level in the world and is still had bigger gap, realized that as Lao Lunsi, the livermore laboratory (LLNL) of the U.S. broadband multiwindow (can be simultaneously at 1.054 μ m, 0.527 three wave bands of μ m and 0.351 μ m use), and our present bandwidth is narrower, can not realize a film multiwindow, limit its application greatly.
Summary of the invention
The object of the present invention is to provide a kind of novel silica membrane that can realize multi-window wideband anti-reflection and preparation method thereof.
What the present invention proposed can realize broadband multiwindow anti-reflection silicon dioxide film, is a kind of PS-SiO
2Film is by SiO
2Mix polystyrene (PS) in the colloidal sol and form, polystyrene accounts for SiO
2The 0.025-0.075% of colloidal sol quality.
Novel PS-SiO by the present invention's proposition
2Anti-reflection film can realize that the broadband multiwindow is anti-reflection.At 351nm, 527nm and 1054nm high transmittance is arranged all, mxm. has all surpassed 98%.
Among the present invention, the PS that mixes in the silicon dioxide gel, when its molecular weight was 4000-6000, the quality percentage composition of PS was the 0.036-0.072% of silicon dioxide gel.When the PS proportion is 0.068%, film transmittance the best, at 351nm, 527nm and 1054nm transmittance are respectively 98.9%, 98.0%, 98.8%.
Among the present invention, the PS that mixes in the silicon dioxide gel, when its molecular weight was about 9000-11000, the quality percentage composition of PS was the 0.028-0.058% of silicon dioxide gel.When the PS proportion is 0.056%, film transmittance the best, at 351nm, 527nm and 1054nm transmittance are respectively 97.2%, 98.5%, 99.5%.
The PS-SiO that the present invention proposes
2The preparation method of anti-reflection film is as follows: at first be equipped with SiO with the sol-gel legal system
2Colloidal sol, raw material are ethyl orthosilicate (TEOS), absolute ethyl alcohol (C
2H
5OH), polyglycol (PEG), catalysis under alkali condition, the quality percentage composition of each component is ethyl orthosilicate: 7-8%, absolute ethyl alcohol: 60-65%, all the other are polyglycol; With gained SiO
2The colloidal sol ageing will be dissolved in the polystyrene and the SiO of ether then
2Colloidal sol mixes, and uses the spin-coating method film forming; At last, rete was at 150-250 ℃ of following thermal treatment 6-8 hour.
In the said method, base catalysis uses ammoniacal liquor (NH
4OH) or ammonium bicarbonate (NH
4HCO
3) etc., its consumption is SiO
2The 1-5% of sol system quality makes the pH value of system be 8-8.5.
The PS-SiO of the present invention's preparation
2Film has very high transmittance, and has realized the high printing opacity in broadband, and at 351nm, the high transmission rate of 527nm and 1054nm has all surpassed 98%.This optical thin film can become the alternate material of KDP crystal anti-reflection film, and can obtain to use in the ultra-intense laser system of high energy nuclear fusion simulated experiment.
Embodiment
Further introduce the specific embodiment of the present invention below, and illustrated by way of example.
1, measure ethyl orthosilicate by above-mentioned mass percent, absolute ethyl alcohol, ammoniacal liquor (or ammonium bicarbonate), PEG400 (or PEG200), and with it mixing;
2, at 30-35 ℃ mixed solution was stirred 3-4 hour;
3, reflux, reflux temperature is 50-60 ℃, backflow 6-8 hour, gets SiO
2Colloidal sol;
4, with SiO
2Colloidal sol ageing 7-10 days will be dissolved in the PS and the SiO of ether then
2Colloidal sol mixes;
5, spin-coating film, spin coating rotating speed are 2000-4000rpm/s;
6, with rete thermal treatment, handle 6-8h at 150-250 ℃, can obtain required anti-reflection film.
Embodiment 1:
The composition of anti-reflection film is expressed as with mass percent: ethyl orthosilicate 7.3%, ammoniacal liquor 1.5%, absolute ethyl alcohol 60.8%, polyglycol (400) 30.4%, molecular weight is about 5000 polystyrene and accounts for 0.068% of silicon dioxide gel quality, raw material (except that PS) is mixed the back to be stirred 4 hours at 30 ℃, backflow remains on about 8.5 the solution pH value, the colloidal sol ageing will be dissolved in ether after 7 days PS mixes with colloidal sol, use the spin-coating method film forming, rotating speed is 2000rpm/s, spin coating 1min, and can obtain desired PS-SiO at 150 ℃ of thermal treatment 6h
2Film.This film is at 351nm, and the transmittance of 527nm and 1054nm is respectively 98.9%, 98.0%, and 98.8%.
Embodiment 2:
The composition of anti-reflection film is expressed as with mass percent: ethyl orthosilicate 7.5%, ammoniacal liquor 1.2%, absolute ethyl alcohol 60.6%, polyglycol (200) 30.7%, molecular weight is about 5000 polystyrene 0.070%, raw material (except that PS) is mixed the back to be stirred 4 hours at 34 ℃, backflow remains on about 8 the solution pH value, the colloidal sol ageing will be dissolved in ether after 9 days PS mixes with colloidal sol, use the spin-coating method film forming, rotating speed is 4000rpm/s, spin coating 1min, and can obtain desired PS-SiO at 220 ℃ of thermal treatment 6h
2Film.This film is at 351nm, and the transmittance of 527nm and 1054nm is respectively 93.7%, 95.9%, and 100%.
Embodiment 3:
The composition of anti-reflection film is expressed as with mass percent: ethyl orthosilicate 7%, ammoniacal liquor 1%, absolute ethyl alcohol 61.2%, polyglycol (400) 30.1%, molecular weight is about 10,000 polystyrene 0.056%, raw material (except that PS) is mixed the back to be stirred 3 hours at 32 ℃, backflow remains on about 8.5 the solution pH value, the colloidal sol ageing will be dissolved in ether after 10 days PS mixes with colloidal sol, uses the spin-coating method film forming, and rotating speed is 4000rpm/s, spin coating 1min, and can obtain desired PS-SiO at 180 ℃ of thermal treatment 8h
2Film.This film is at 351nm, and the transmittance of 527nm and 1054nm is respectively 97.2%, 98.5%, and 99.5%.
Claims (5)
1, a kind of multi-window wideband anti-reflection PS-SiO
2Film is characterized in that by SiO
2Mix polystyrene in the colloidal sol and form, polystyrene accounts for SiO
2The 0.056-0.070% of colloidal sol quality; And obtain by following preparation process: at first be equipped with SiO with the sol-gel legal system
2Colloidal sol, raw material are ethyl orthosilicate, absolute ethyl alcohol and polyglycol, catalysis under alkali condition, and the mass percentage content of each component is ethyl orthosilicate: 7-8%, absolute ethyl alcohol: 60-65%, all the other are polyglycol; With gained SiO
2The colloidal sol ageing will be dissolved in the polystyrene and the SiO of ether then
2Colloidal sol mixes, and uses the spin-coating method film forming, and rotating speed is 2000-4000 revolutions per second, and the time is 1 minute; At last, rete was at 150-250 ℃ of following thermal treatment 6-8 hour.
2, PS-SiO according to claim 1
2Film is characterized in that the molecular weight of said polystyrene is 5000, and polystyrene accounts for SiO
2The 0.068-0.070% of colloidal sol quality.
3, PS-SiO according to claim 1
2Film is characterized in that the molecular weight of said polystyrene is 10000, and polystyrene accounts for SiO
20.056% of colloidal sol quality.
4, a kind of multi-window wideband anti-reflection PS-SiO
2The preparation method of film is characterized in that at first being equipped with SiO with the sol-gel legal system
2Colloidal sol, raw material are ethyl orthosilicate, absolute ethyl alcohol and polyglycol, catalysis under alkali condition, and the mass percentage content of each component is ethyl orthosilicate: 7-8%, absolute ethyl alcohol: 60-65%, all the other are polyglycol; With gained SiO
2The colloidal sol ageing.To dissolve in the polystyrene and the SiO of ether then
2Colloidal sol mixes, and polystyrene accounts for SiO
2The 0.056%-0.070% of colloidal sol quality: use the spin-coating method film forming, rotating speed is 2000-4000 revolutions per second, and the time is 1 minute; At last, rete was at 150-250 ℃ of following thermal treatment 6-8 hour.
5, preparation method according to claim 4 is characterized in that said base catalysis uses ammoniacal liquor or ammonium bicarbonate, and the pH value of regulation system is 8-8.5.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100277797A CN100346176C (en) | 2005-07-15 | 2005-07-15 | Multi-window wideband anti-reflection PS-SiO2 thin film and producing method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100277797A CN100346176C (en) | 2005-07-15 | 2005-07-15 | Multi-window wideband anti-reflection PS-SiO2 thin film and producing method thereof |
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| Publication Number | Publication Date |
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| CN1740824A CN1740824A (en) | 2006-03-01 |
| CN100346176C true CN100346176C (en) | 2007-10-31 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101844877B (en) * | 2010-05-29 | 2012-06-06 | 无锡海达安全玻璃有限公司 | Processing method for high anti-reflective glass for packaging solar battery pack |
| CN108307601B (en) * | 2017-12-20 | 2020-11-10 | 深圳怡钛积科技股份有限公司 | Sapphire cover plate, preparation method thereof and terminal device |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4609267A (en) * | 1980-12-22 | 1986-09-02 | Seiko Epson Corporation | Synthetic resin lens and antireflection coating |
| CN1529186A (en) * | 2003-09-28 | 2004-09-15 | 华中科技大学 | High-luminousness optical lens and making method thereof |
-
2005
- 2005-07-15 CN CNB2005100277797A patent/CN100346176C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4609267A (en) * | 1980-12-22 | 1986-09-02 | Seiko Epson Corporation | Synthetic resin lens and antireflection coating |
| CN1529186A (en) * | 2003-09-28 | 2004-09-15 | 华中科技大学 | High-luminousness optical lens and making method thereof |
Non-Patent Citations (2)
| Title |
|---|
| KDP晶体增透膜和保护膜性能研究 张伟清，唐永兴，乐月琴，蒋敏华，刘小林，孙今人，强激光与粒子束，第11卷第2期 1999 * |
| 静电自组装法制备SiO2光学增透膜 何方方，许丕池，卢忠远，腾元成，廖其龙，四川大学学报(工程科学版)，第37卷第3期 2005 * |
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