CN1740823A - A multiwindow wideband anti-reflection PMMA-SiO2 thin film and producing method thereof - Google Patents
A multiwindow wideband anti-reflection PMMA-SiO2 thin film and producing method thereof Download PDFInfo
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- CN1740823A CN1740823A CNA2005100277782A CN200510027778A CN1740823A CN 1740823 A CN1740823 A CN 1740823A CN A2005100277782 A CNA2005100277782 A CN A2005100277782A CN 200510027778 A CN200510027778 A CN 200510027778A CN 1740823 A CN1740823 A CN 1740823A
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- sio
- pmma
- colloidal sol
- reflection
- film
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Abstract
The present invention utilizes sol-gel process, after the SiO2 sol is formed, the polymethyl methacrylate (PMMA) is added, then the above-mentioned materials are undergone the process of heat-treatment rotary film-coating procedure so as to obtain the invented multi-window broadband increased transmission PMMA-SiO2 film with high light transmittance at 351nm, 527nm and 1054nm.
Description
Technical field
The invention belongs to optically thin technology field of membrane materials, 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, to avoid sensitive element to be subjected to the destruction of unnecessary reflection, 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.
Summary of the invention
The object of the present invention is to provide and a kind ofly can realize novel silica membrane of 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 PMMA-SiO
2Film is by SiO
2Mix polymethylmethacrylate (PMMA) in the colloidal sol and form, PMMA content is the 0.27-0.35% of silicon dioxide gel quality.
By PMMA-SiO provided by the invention
2Anti-reflection film can realize that the broadband multiwindow is anti-reflection.At 351nm, 527nm and 1054nm all have high transmittance, and mxm. has all surpassed 98%.When the PMMA proportion is 0.29%, film transmittance the best, at 351nm, 527nm and 1054nm transmittance are respectively 98.2%, 98.8%, 100.0%.
The PMMA-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 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 polymethylmethacrylate and the SiO of ether then
2Colloidal sol mixes, and uses the spin-coating method film forming, and last, rete was at 150-180 ℃ of thermal treatment 6-8 hour.
Among the present invention, said base catalysis uses ammoniacal liquor (NH
4OH) or ammonium bicarbonate (NH
4HCO
3), its consumption is SiO
2The 1-5% of sol system quality, the pH value of regulation system is 8-8.5.
The PMMA-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 obtains to use in the ultra-intense laser system of high energy nuclear fusion simulated experiment.
Embodiment
Further introduce embodiments 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, the PMMA that will dissolve in ether then mixes with colloidal sol;
5, spin-coating film, spin coating rotating speed are 3000-4000rpm/s,
6, with rete thermal treatment, about 150-250 ℃, handle 6-8h, can obtain required anti-reflection film.
Embodiment 1:
The composition of anti-reflection film is expressed as with mass percent: ethyl orthosilicate 7.4%, absolute ethyl alcohol 60.7%, polyglycol (400) 30.4%, polymethylmethacrylate 0.29%, ammoniacal liquor 1.5%, raw material (removing PMMA) is mixed the back stirred 4 hours at 30 ℃, refluxing remains on about 8.5 the solution pH value, and the colloidal sol ageing will be dissolved in ether after 7 days PMMA mixes with colloidal sol, use the spin-coating method film forming, rotating speed 4000rpm/s, spin coating 1min, and can obtain desired PMMA-SiO at 150 ℃ of thermal treatment 6h
2Film.This film is at 351nm, and the transmittance of 527nm and 1054nm is respectively 98.2%, 98.8%, and 100.0%.
Embodiment 2:
The composition of anti-reflection film is expressed as with mass percent: ethyl orthosilicate 7.2%, absolute ethyl alcohol 61.1%, polyglycol (400) 30.5%, polymethylmethacrylate 0.32%, ammoniacal liquor 1.2%; Raw material (removing PMMA) is mixed the back stirred 4 hours at 35 ℃, refluxing remains on about 8 the solution pH value, and the colloidal sol ageing will be dissolved in ether after 8 days PMMA mixes with colloidal sol, use the spin-coating method film forming, rotating speed 4000rpm/s, spin coating 1min, and can obtain desired PMMA-SiO at 200 ℃ of thermal treatment 6h
2Film.This film is at 351nm, and the transmittance of 527nm and 1054nm is respectively 100%, 99.8%, and 95.6%.
Embodiment 3:
The composition of anti-reflection film is expressed as with mass percent: ethyl orthosilicate 7.2%, ammonium bicarbonate 1%, absolute ethyl alcohol 62%, polyglycol (200) 30.4%, polymethylmethacrylate 0.35%, raw material (removing PMMA) is mixed the back stirred 4 hours at 30 ℃, refluxing remains on about 8.5 the solution pH value, and the colloidal sol ageing will be dissolved in ether after 10 days PMMA mixes with colloidal sol, use the spin-coating method film forming, rotating speed 3000rpm/s, spin coating 1min, and can obtain desired PMMA-SiO at 220 ℃ of thermal treatment 6h
2Film.This film is at 351nm, and the transmittance of 527nm and 1054nm is respectively 94.0%, 94.7%, and 99.0%.
Claims (3)
1, a kind of multi-window wideband anti-reflection PMMA-SiO
2Film is characterized in that by SiO
2Mix polymethylmethacrylate in the colloidal sol and form, polymethylmethacrylate accounts for SiO
2The 0.27-0.35% of colloidal sol quality.
2, a kind of multi-window wideband anti-reflection PMMA-SiO as claimed in claim 1
2Film 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, 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 polymethylmethacrylate and the SiO of ether then
2Colloidal sol mixes, and uses the spin-coating method film forming, and last, rete was at 150-250 ℃ of thermal treatment 6-8 hour.
3, preparation method according to claim 2 is characterized in that said base catalysis uses ammoniacal liquor or ammonium bicarbonate, and the pH value of regulation system is 8-8.5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100277782A CN100340872C (en) | 2005-07-15 | 2005-07-15 | A multiwindow wideband anti-reflection PMMA-SiO2 thin film and producing method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100277782A CN100340872C (en) | 2005-07-15 | 2005-07-15 | A multiwindow wideband anti-reflection PMMA-SiO2 thin film and producing method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1740823A true CN1740823A (en) | 2006-03-01 |
| CN100340872C CN100340872C (en) | 2007-10-03 |
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ID=36093266
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|---|---|---|---|
| CNB2005100277782A Expired - Fee Related CN100340872C (en) | 2005-07-15 | 2005-07-15 | A multiwindow wideband anti-reflection PMMA-SiO2 thin film and producing method thereof |
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| CN (1) | CN100340872C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101844877A (en) * | 2010-05-29 | 2010-09-29 | 无锡海达安全玻璃有限公司 | Processing method for high anti-reflective glass for packaging solar battery pack |
| CN102659322A (en) * | 2012-04-06 | 2012-09-12 | 南昌航空大学 | Preparation method of glass/polymethyl methacrylate (PMMA) micro-nano interface structure laminated material |
| CN106519527A (en) * | 2016-09-28 | 2017-03-22 | 天津科技大学 | Antireflective organic glass and preparation method thereof |
| CN110308501A (en) * | 2019-07-24 | 2019-10-08 | 中国工程物理研究院激光聚变研究中心 | A kind of light laser film and preparation method thereof, application |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103691374B (en) * | 2013-12-12 | 2016-01-27 | 齐鲁工业大学 | There is the preparation method of the PMMA nanometer ghost of different thickness of the shell |
Family Cites Families (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 |
| CN1248017C (en) * | 2003-09-28 | 2006-03-29 | 华中科技大学 | High-luminousness optical lens and making method thereof |
-
2005
- 2005-07-15 CN CNB2005100277782A patent/CN100340872C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101844877A (en) * | 2010-05-29 | 2010-09-29 | 无锡海达安全玻璃有限公司 | Processing method for high anti-reflective glass for packaging solar battery pack |
| 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 |
| CN102659322A (en) * | 2012-04-06 | 2012-09-12 | 南昌航空大学 | Preparation method of glass/polymethyl methacrylate (PMMA) micro-nano interface structure laminated material |
| CN102659322B (en) * | 2012-04-06 | 2014-04-02 | 南昌航空大学 | Preparation method of glass/polymethyl methacrylate (PMMA) micro-nano interface structure laminated material |
| CN106519527A (en) * | 2016-09-28 | 2017-03-22 | 天津科技大学 | Antireflective organic glass and preparation method thereof |
| CN106519527B (en) * | 2016-09-28 | 2018-06-26 | 天津科技大学 | A kind of anti-reflection organic glass and preparation method thereof |
| CN110308501A (en) * | 2019-07-24 | 2019-10-08 | 中国工程物理研究院激光聚变研究中心 | A kind of light laser film and preparation method thereof, application |
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| Publication number | Publication date |
|---|---|
| CN100340872C (en) | 2007-10-03 |
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Granted publication date: 20071003 Termination date: 20100715 |