CN1399147A - Prepn of laser damage-resisting wide-band antireflecting film - Google Patents
Prepn of laser damage-resisting wide-band antireflecting film Download PDFInfo
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- CN1399147A CN1399147A CN02140488A CN02140488A CN1399147A CN 1399147 A CN1399147 A CN 1399147A CN 02140488 A CN02140488 A CN 02140488A CN 02140488 A CN02140488 A CN 02140488A CN 1399147 A CN1399147 A CN 1399147A
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Abstract
A preparation method of laser damage-resisting wide-band antireflecting film with ethyl emtasilicate as presoma includes mixing water, absolute alcohol, polyvinyl pyrrolidone and polyglycol in a certain proportion in the presence of ammonia water catalyst, reaction by sufficient stirring, ageing, and film plating. The present invention has the advantages of mild preparation condition, low cost and simple operation, and the prepared SiO2 film has antireflecting performance of 400-600 nm bandwidth and high laser damage resistance.
Description
Affiliated field:
A kind of preparation method of antireflective film relates in particular to a kind of high anti-laser that has under the present invention
The SiO of damage threshold
2The preparation method of individual layer broad band antireflective film.
Background technology
Optical element film coated common employing physical coating and sol-gel (Sol-gel) forensic chemistry plated film.Wherein the physics method because of the equipment complexity, involve great expense, the micromechanism of wayward rete, and the not high shortcoming that is difficult to overcome of threshold for resisting laser damage, practical application is restricted.In recent years, the research work of carrying out laser system optical element plated film with the Sol-gel method has had very big development.The Sol-gel method is compared with traditional physical coating method has advantages such as threshold for resisting laser damage height, surface uniformity is good, cost is lower, especially this method is particularly suitable for the preparation of big substrate rete, is the most promising method of the required a large amount of optical films of production laser fusion system of future generation and new pattern laser armament systems.
The broad band antireflective film can effectively improve optical transmittance in wide wavelength coverage, reduce energy loss, at laser system xenon lamp, partition glass and civilianly very big application prospect is arranged aspect optical element film coated.Broad band anti-reflection rete can be coated on Optical Maser System xenon lamp partition glass and the flashlamp, can improve Optical Maser System efficient, reduces the energy loss of whole Optical Maser System greatly.Formed by the hydridization silane of zirconia sol-polyethylene filling agent, fluorine-containing rete and the short crosslinking chemical of conduct according to the broad band antireflective film that document (SPIE vol.2253:764) report abroad is coated with at present, be multilayer film, rete cost height, colloidal sol preparation and coating process complexity.
Summary of the invention:
The object of the present invention is to provide the preparation method that a kind of cost is low, prepare the individual layer broad band antireflective film of simple high resisting laser damage.Preparation of the present invention may further comprise the steps: 1, the preparation of plated film colloidal sol: with ethyl orthosilicate (TEOS) is presoma, under the ammonia-catalyzed condition, add entry, absolute ethyl alcohol (ETOH), polyvinylpyrrolidone (PVP), polyglycol (PEG) in proportion, mixed back is fully stirred and is reacted; Mole between each material matches well and is EtOH/TEOS=20～100; H
2O/TEOS=1～10; PVP/TEOS=2 * 10
-6～1 * 10
-8PEG/TEOS=3 * 10
-4～2 * 10
-3NH3H
2O/TEOS=0.02～0.3.2, ageing: the ageing temperature can be between 0～70 ℃.Digestion time is 3～60 days.3, plated film: adopt rotary plating method or czochralski method to carry out one deck coating single side or double-sided coating.
The invention has the advantages that colloidal sol preparation condition gentleness, cost is lower, and is simple to operate.By the sol-gel approach to SiO
2Introduce polymeric additive in the colloid network, regulate and control its sol-gel process, make the SiO for preparing
2Film not only has width to reach 400-600nm broad band anti-reflection performance, has high threshold for resisting laser damage simultaneously.
Embodiment:
Embodiment 11) preparation of plated film colloidal sol is 5ml Si (OC
2H
5)
4With 100ml absolute ethyl alcohol, 0.08ml NH
3H
2O, 0.8ml H
2O, 0.1mlPEG, 0.19PVP stirring and evenly mixing react; 2) ageing: the solution that gained is mixed places closed container, and 0 ℃ was worn out 60 days.3) plated film: employing lifts coating method and carries out one deck coating single side.4) estimate: with the optical transmittance of PC2501 UV/VIS spectrometer measurement rete
T
c(％)。Measure the laser damage threshold LDT of rete at 1064nm.Data see Table 1.
Embodiment 21) preparation of coating liquid is 5ml Si (OC
2H
5)
4With 50ml absolute ethyl alcohol, 032ml NH
3H
2O, 0.5ml H
2O, 0.1mlPEG, 0.2mlPVP stirring and evenly mixing react; 2) ageing: the solution that gained is mixed places closed container, and 40 ℃ were worn out 10 days.Repeat example 1 3) and 4).
Embodiment 31) preparation of coating liquid: with 10ml Si (OC
2H
5)
4With 100ml absolute ethyl alcohol, 2.5mlNH
3H
2O, 0.2mlPEG, 0.1mlPVP stirring and evenly mixing react; 2) ageing: the solution sealing that gained mixes is preserved, place 60 ℃ to wear out 3 days.Repeat embodiment 1 3) and 4).
Embodiment 41) preparation of coating liquid: with 10ml Si (OC
2H
5)
4With 50ml absolute ethyl alcohol, 0.62mlNH
3H
2O, 0.3ml H
2O, 0.2ml PEG, 0.5ml PVP stirring and evenly mixing react; 2) ageing: the solution that gained is mixed places closed container, and 20 ℃ were worn out 30 days.Repeat embodiment 13 and 4).Table 1 (English should be written as Chinese)
| ????T c(％) | Bands of a spectrum scope (nm) | ??LDT(J/cm 2)(1064 ????1ns) | |
| Example 1 | ????95.5％ | ????400-800 | ????35.00 |
| Example 2 | ????95.4％ | ????600-1100 | ????32.00 |
| Example 3 | ????95.6％ | ????500-900 | ????40.00 |
| Example 4 | 99.3% (two-sided) | ????700-1100 | ????45.00 |
Claims (1)
1. the preparation method of a resisting laser damage broad band antireflective film is characterized in that preparation may further comprise the steps:
(1) preparation of plated film colloidal sol: with the ethyl orthosilicate is presoma, under the ammonia-catalyzed condition, adds entry, absolute ethyl alcohol, polyvinylpyrrolidone and polyglycol in proportion, and mixed back is fully stirred and reacted; Mole between each material matches well and is EtOH/TEOS=20～100; H
2O/TEOS=1～10; PVP/TEOS=2 * 10
-6～1 * 10
-8PEG/TEOS=3 * 10
-4～2 * 10
-3Ammoniacal liquor/TEOS=0.02～0.3.
(2) ageing: the ageing temperature can be between 0～70 ℃, and digestion time is 3～60 days;
(3) plated film: adopt rotary plating method or czochralski method to carry out one deck coating single side or double-sided coating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021404887A CN1167959C (en) | 2002-07-19 | 2002-07-19 | Prepn of laser damage-resisting wide-band antireflecting film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021404887A CN1167959C (en) | 2002-07-19 | 2002-07-19 | Prepn of laser damage-resisting wide-band antireflecting film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1399147A true CN1399147A (en) | 2003-02-26 |
| CN1167959C CN1167959C (en) | 2004-09-22 |
Family
ID=4750319
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021404887A Expired - Fee Related CN1167959C (en) | 2002-07-19 | 2002-07-19 | Prepn of laser damage-resisting wide-band antireflecting film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1167959C (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101280155B (en) * | 2007-04-02 | 2010-08-18 | 中国科学院化学研究所 | Self-cleaning film and preparation thereof |
| CN101979352A (en) * | 2010-10-28 | 2011-02-23 | 常熟耀皮特种玻璃有限公司 | Organic coating material capable of reducing light reflectivity of glass surface and glass |
| CN102485807A (en) * | 2010-12-01 | 2012-06-06 | 常熟卓辉光电科技有限公司 | Coating material capable of reducing light reflection of glass surface |
| CN101517437B (en) * | 2006-09-29 | 2012-07-04 | 西门子公司 | Transparent porous SiO2 coating for a transparent substrate material |
| CN101995589B (en) * | 2009-08-14 | 2013-03-13 | 比亚迪股份有限公司 | Method for preparing silica antireflective film |
| CN104150786A (en) * | 2014-08-11 | 2014-11-19 | 南开大学 | Method for preparing wide-spectrum high-transmittance antireflection film by film coating method |
-
2002
- 2002-07-19 CN CNB021404887A patent/CN1167959C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101517437B (en) * | 2006-09-29 | 2012-07-04 | 西门子公司 | Transparent porous SiO2 coating for a transparent substrate material |
| CN101280155B (en) * | 2007-04-02 | 2010-08-18 | 中国科学院化学研究所 | Self-cleaning film and preparation thereof |
| CN101995589B (en) * | 2009-08-14 | 2013-03-13 | 比亚迪股份有限公司 | Method for preparing silica antireflective film |
| CN101979352A (en) * | 2010-10-28 | 2011-02-23 | 常熟耀皮特种玻璃有限公司 | Organic coating material capable of reducing light reflectivity of glass surface and glass |
| CN102485807A (en) * | 2010-12-01 | 2012-06-06 | 常熟卓辉光电科技有限公司 | Coating material capable of reducing light reflection of glass surface |
| CN104150786A (en) * | 2014-08-11 | 2014-11-19 | 南开大学 | Method for preparing wide-spectrum high-transmittance antireflection film by film coating method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1167959C (en) | 2004-09-22 |
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Granted publication date: 20040922 Termination date: 20120719 |