CN103524049A - Preparation method of monolayer SiO2 antireflection film - Google Patents
Preparation method of monolayer SiO2 antireflection film Download PDFInfo
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- CN103524049A CN103524049A CN201310450117.5A CN201310450117A CN103524049A CN 103524049 A CN103524049 A CN 103524049A CN 201310450117 A CN201310450117 A CN 201310450117A CN 103524049 A CN103524049 A CN 103524049A
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- preparation
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- individual layer
- reflection
- reflection film
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- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 8
- 229910052681 coesite Inorganic materials 0.000 title abstract 4
- 229910052906 cristobalite Inorganic materials 0.000 title abstract 4
- 235000012239 silicon dioxide Nutrition 0.000 title abstract 4
- 229910052682 stishovite Inorganic materials 0.000 title abstract 4
- 229910052905 tridymite Inorganic materials 0.000 title abstract 4
- 239000002356 single layer Substances 0.000 title abstract 3
- 239000011521 glass Substances 0.000 claims abstract description 21
- 238000004140 cleaning Methods 0.000 claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract description 12
- 238000000576 coating method Methods 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 17
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 239000005357 flat glass Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 150000001298 alcohols Chemical class 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000002243 precursor Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- 230000002378 acidificating effect Effects 0.000 claims description 4
- 230000032683 aging Effects 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 239000010413 mother solution Substances 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 238000002203 pretreatment Methods 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 238000003980 solgel method Methods 0.000 claims description 4
- 238000007711 solidification Methods 0.000 claims description 4
- 230000008023 solidification Effects 0.000 claims description 4
- 238000003786 synthesis reaction Methods 0.000 claims description 4
- 238000012360 testing method Methods 0.000 claims description 4
- 238000007598 dipping method Methods 0.000 claims description 3
- 239000007888 film coating Substances 0.000 claims description 3
- 238000009501 film coating Methods 0.000 claims description 3
- 230000000873 masking effect Effects 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000004528 spin coating Methods 0.000 claims description 3
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 2
- -1 as presoma Substances 0.000 claims description 2
- 238000012986 modification Methods 0.000 claims description 2
- 230000004048 modification Effects 0.000 claims description 2
- 229910000077 silane Inorganic materials 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 5
- 238000000465 moulding Methods 0.000 abstract description 2
- 238000004806 packaging method and process Methods 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 34
- 230000003667 anti-reflective effect Effects 0.000 description 6
- 239000012528 membrane Substances 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 238000006124 Pilkington process Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000001935 peptisation Methods 0.000 description 1
- 230000002085 persistent effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
Landscapes
- Surface Treatment Of Glass (AREA)
Abstract
The invention discloses a preparation method of a monolayer SiO2 antireflection film. The preparation method comprises steps as follows: (1) pretreatment of a glass substrate; (2) preparation of SiO2 sol; (3) sol coating and molding; (4) film curing; and (5) cooling, checking and packaging. The monolayer SiO2 antireflection film has excellent anti-reflection performance, very excellent thixotropy, good self-cleaning performance and excellent chemical stability, and the preparation method is simple.
Description
Technical field
The present invention relates to a kind of individual layer SiO
2the preparation method of anti-reflection film, belongs to anti-reflection film preparing technical field.
Background technology
The anti-reflection film of silicon solar cell device is mainly used in packaged glass surface, for improving sunlight transmissivity and the protection packaging glass of packaged glass.Float glass process ultra-clear glasses is for more than encapsulating annual 3500000 square meters of annual production of solar cell, and increase year by year.Compare with organic membrane, mineral membrane has excellent heat, chemically stable shape, resistance to microorganism property and the higher advantages such as physical strength, in catalysis, gas delivery, be that the fields such as processing, membrane reactor have huge application potential.
Along with the continually developing and studying of anti-reflection film, the coating technique of optical anti-reflective film is also in continuous development.The thickness of optical anti-reflective film will be controlled on the order of magnitude of visible wavelength 1/4, and the requirement of the uniformity coefficient of anti-reflection film is unusual harshness also.However, in people's persistent exploration, many effective, advanced coating techniques have still been grasped.At present, conventional film coating method has vacuum evaporation, chemistry to play mutually the methods such as deposition, sol-gel coating.Three compares, sol-gel coating equipment is simple, can operate at normal temperatures and pressures, membrane uniformity is high, microtexture is controlled, be suitable for different shapes, size substrate, can fill a prescription by control, preparation technology obtains optical thin film, become various optical thin films and the most competitive preparation method of top coat.
At present, anti-reflection film adopts wet chemical method collosol and gel SiO
2coating, antireflective effect is more general, average 2% left and right, chemical stability and self-cleaning ability, easily adsorb dust and cause transmitance to decline below 20%.Well imagine to possess good antireflective effect, the anti-reflection film of simultaneously taking into account good self-cleaning ability and chemical stability is that the excellent of sun power packaged glass must be joined " clothes ".In addition, solar energy collector anti-reflection film technology dull and stereotyped and vacuum tube glass is also completely not universal at home, and the heating efficiency that promotes solar energy collector is the technological trend of domestic heat collector development.
Summary of the invention
The object of the invention is to for deficiency of the prior art, the individual layer SiO that a kind of antireflective effect is outstanding, possess self-cleaning function is provided
2the preparation method of anti-reflection film.
The present invention is achieved through the following technical solutions: a kind of individual layer SiO
2the preparation method of anti-reflection film, is characterized in that: comprise the following steps:
(1) base plate glass pre-treatment: base plate glass is distinguished ultrasonic 30 minutes in acetone soln and ethanolic soln;
(2) SiO
2the preparation of colloidal sol: this colloidal sol adopts two step synthesis: A) adopt traditional sol-gel method to prepare dilute acidic SiO
2colloidal sol is as mother solution, and preparation method is as follows: by the organic precursor of silicon, alcohols and water, as presoma, mix according to the ratio of mol ratio 1:30:4, add salt acid for adjusting pH to 2～5, stir, and room temperature ageing 1～10 day; B) nano silica powder is dispersed in ethanolic soln, the weight ratio that is then 1:2～10 according to B solution than A solution adds B solution in A solution, after stirring, can become follow-up plated film colloidal sol;
(3) sol coating masking: at glass baseplate surface plated film, form certain thickness film;
(4) film hardening: film is through 200～400 ℃ of heat treatment for solidification in baking oven, and the solvent in volatilization colloidal sol, makes film tight adhesion at glass surface;
(5) cooling rear test package.
Further, the film coating method of described step (3) comprises dipping method of pulling up, method of roll coating, spin coating method, and thickness is 120～130nm.
Further, in described step (2), organic precursor of silicon comprises TEOS, silane and TMOS, preferably TEOS.
Further, the alcohols in described step (2) comprises ethanol, propyl alcohol, Virahol and methyl alcohol.
Preferably alcohols is ethanol.
A kind of individual layer SiO of the present invention
2anti-reflection film can be used for following field:
(1) the anti-reflection and self-cleaning performance for sun power packaged glass promotes;
(2) the anti-reflection and self-cleaning performance for solar energy collector glass promotes;
(3) for the anti-reflection of building glass and automatically cleaning modification.
Beneficial effect of the present invention:
(1) product of the present invention possesses good self-cleaning function and outstanding chemical stability, and water droplet contact angle is less than 15 degree, has overcome traditional Si O
2the bad stability of anti-reflection film, the shortcoming that bonding strength is weak and self-cleaning ability is weak;
(2) colloidal sol that prepared by the present invention possesses unsurpassed thixotropy, i.e. the controlled peptization characteristic of ultra-long time, not gelling automatically when solvent exists;
(3) product of the present invention also possesses characteristic acidproof, scratch resistance;
(4) after product plated film, the outward appearance of product own and former no significant difference, overall appearance, and wear-resisting, acidproof, weather, cohesive force are strong;
(5) preparation were established of product of the present invention rationally, simply.
Accompanying drawing explanation
Fig. 1 is technological line schematic diagram of the present invention.
Fig. 2 is the product antireflective effect figure of the embodiment of the present invention 1.
Embodiment
Below in conjunction with the drawings and specific embodiments, technical scheme of the present invention is elaborated.
Embodiment 1
(1) base plate glass pre-treatment: base plate glass is distinguished to ultrasonic 30 minutes in acetone soln and ethanolic soln;
(2) SiO
2the preparation of colloidal sol: this colloidal sol adopts two step synthesis:
A) adopt traditional sol-gel method to prepare dilute acidic SiO
2colloidal sol is as mother solution, and preparation method is as follows: by TEOS, second alcohol and water, as presoma, mixes according to the ratio of mol ratio 1:30:4, adds salt acid for adjusting pH to 2, stir, and room temperature ageing 1～10 day;
B) nano silica powder is dispersed in ethanolic soln, the weight ratio that is then 1:2 according to B solution than A solution adds B solution in A solution, after stirring, can become follow-up plated film colloidal sol;
(3) sol coating masking: utilize dipping method of pulling up at glass baseplate surface plated film, form the film of 120～130nm thickness;
(4) film hardening: film is through 200 ℃ of heat treatment for solidification in baking oven, and the solvent in volatilization colloidal sol, makes film tight adhesion at glass surface;
(5) cooling rear test package.
embodiment 2
(1) base plate glass pre-treatment: base plate glass is distinguished to ultrasonic 30 minutes in acetone soln and ethanolic soln;
(2) SiO
2the preparation of colloidal sol: this colloidal sol adopts two step synthesis:
A) adopt traditional sol-gel method to prepare dilute acidic SiO
2colloidal sol is as mother solution, and preparation method is as follows: using TMOS, first alcohol and water as presoma, according to the ratio of mol ratio 1:30:4, mix, add salt acid for adjusting pH to 5, stir, room temperature ageing 10 days;
B) nano silica powder is dispersed in ethanolic soln; Then the weight ratio that is 1:10 according to B solution than A solution adds B solution in A solution, after stirring, can become follow-up plated film colloidal sol;
(3) sol coating molding: adopt spin coating method at glass baseplate surface plated film, form the thick film of 130nm;
(4) film hardening: film is through 400 ℃ of heat treatment for solidification in baking oven, and the solvent in volatilization colloidal sol, makes film tight adhesion at glass surface;
(5) cooling rear test package.
Above-described embodiment is only in order to illustrate technical scheme of the present invention; but not design of the present invention and protection domain are limited; those of ordinary skill in the art modifies or is equal to replacement technical scheme of the present invention; and not departing from aim and the scope of technical scheme, it all should be encompassed in claim scope of the present invention.
Claims (7)
1. an individual layer SiO
2the preparation method of anti-reflection film, is characterized in that: comprise the following steps:
(1) base plate glass pre-treatment: base plate glass is distinguished ultrasonic 30 minutes in acetone soln and ethanolic soln;
(2) SiO
2the preparation of colloidal sol: this colloidal sol adopts two step synthesis: A) adopt traditional sol-gel method to prepare dilute acidic SiO
2colloidal sol is as mother solution, and preparation method is as follows: by the organic precursor of silicon, alcohols and water, as presoma, mix according to the ratio of mol ratio 1:30:4, add salt acid for adjusting pH to 2～5, stir, and room temperature ageing 1～10 day; B) nano silica powder is dispersed in ethanolic soln; Then the weight ratio that is 1:2～10 according to B solution than A solution adds B solution in A solution, after stirring, can become follow-up plated film colloidal sol;
(3) sol coating masking: at glass baseplate surface plated film, form certain thickness film;
(4) film hardening: film is through 200～400 ℃ of heat treatment for solidification in baking oven, and the solvent in volatilization colloidal sol, makes film tight adhesion at glass surface;
(5) cooling rear test package.
2. a kind of individual layer SiO according to claim 1
2the preparation method of anti-reflection film, is characterized in that: in described step (2), organic precursor of silicon comprises TEOS, silane and TMOS.
3. a kind of individual layer SiO according to claim 1
2the preparation method of anti-reflection film, is characterized in that: the film coating method of described step (3) comprises dipping method of pulling up, method of roll coating, spin coating method, and thickness is 120～130nm.
4. a kind of individual layer SiO according to claim 3
2the preparation method of anti-reflection film, is characterized in that: in described step (2), organic precursor of silicon is TEOS.
5. a kind of individual layer SiO according to claim 1
2the preparation method of anti-reflection film, is characterized in that: the alcohols in described step (2) comprises ethanol, propyl alcohol, Virahol and methyl alcohol.
6. a kind of individual layer SiO according to claim 5
2the preparation method of anti-reflection film, is characterized in that: the alcohols in described step (2) is ethanol.
7. an a kind of individual layer SiO who is prepared by method claimed in claim 1
2the application of anti-reflection film, is characterized in that: described individual layer SiO
2anti-reflection film is applied to following field:
(1) the anti-reflection and self-cleaning performance for sun power packaged glass promotes;
(2) the anti-reflection and self-cleaning performance for solar energy collector glass promotes;
(3) for the anti-reflection of building glass and automatically cleaning modification.
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| CN201310450117.5A CN103524049B (en) | 2013-09-29 | 2013-09-29 | A kind of monolayer SiO2the preparation method of anti-reflection film |
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| CN201310450117.5A CN103524049B (en) | 2013-09-29 | 2013-09-29 | A kind of monolayer SiO2the preparation method of anti-reflection film |
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| CN103524049B CN103524049B (en) | 2016-08-24 |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105541120A (en) * | 2015-12-28 | 2016-05-04 | 常熟市金亿复合材料有限公司 | Coating process for hollow glass plate |
| CN105776884A (en) * | 2014-12-24 | 2016-07-20 | 北京有色金属研究总院 | Porous silica anti-reflective film and preparation method thereof |
| CN106892575A (en) * | 2015-12-18 | 2017-06-27 | 北京有色金属研究总院 | A kind of preparation method of porous silica antireflective coating |
| CN107140844A (en) * | 2016-11-03 | 2017-09-08 | 辽宁中迅科技有限公司 | A kind of preparation method of the non-conductive coated glass of the adjustable automatically cleaning of T/R values |
| CN107140840A (en) * | 2017-01-26 | 2017-09-08 | 辽宁中迅科技有限公司 | A kind of method that use solution chemical method prepares anti-dazzle coated glass |
| CN107140845A (en) * | 2016-12-09 | 2017-09-08 | 辽宁中迅科技有限公司 | The method that adjustable wideband anti-reflection coated glass is prepared with solution chemical method |
| CN108341600A (en) * | 2018-03-14 | 2018-07-31 | 江苏大学 | One kind preparing single layer SiO in glass surface2The method of microballoon film |
| CN108439818A (en) * | 2018-03-19 | 2018-08-24 | 江苏大学 | A kind of preparation method of hydrophobicity antiradar reflectivity glass surface |
| CN108545753A (en) * | 2018-04-19 | 2018-09-18 | 常州大学 | A kind of network-like SiO2Plate film sol and its preparation method and application |
Families Citing this family (1)
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| CN107140847A (en) * | 2017-03-22 | 2017-09-08 | 辽宁中迅科技有限公司 | A kind of solution chemistry preparation method of non-conductive anti-reflection anti-dazzle Coating Materials |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105776884A (en) * | 2014-12-24 | 2016-07-20 | 北京有色金属研究总院 | Porous silica anti-reflective film and preparation method thereof |
| CN106892575A (en) * | 2015-12-18 | 2017-06-27 | 北京有色金属研究总院 | A kind of preparation method of porous silica antireflective coating |
| CN105541120A (en) * | 2015-12-28 | 2016-05-04 | 常熟市金亿复合材料有限公司 | Coating process for hollow glass plate |
| CN107140844A (en) * | 2016-11-03 | 2017-09-08 | 辽宁中迅科技有限公司 | A kind of preparation method of the non-conductive coated glass of the adjustable automatically cleaning of T/R values |
| CN107140845A (en) * | 2016-12-09 | 2017-09-08 | 辽宁中迅科技有限公司 | The method that adjustable wideband anti-reflection coated glass is prepared with solution chemical method |
| CN107140840A (en) * | 2017-01-26 | 2017-09-08 | 辽宁中迅科技有限公司 | A kind of method that use solution chemical method prepares anti-dazzle coated glass |
| CN108341600A (en) * | 2018-03-14 | 2018-07-31 | 江苏大学 | One kind preparing single layer SiO in glass surface2The method of microballoon film |
| CN108439818A (en) * | 2018-03-19 | 2018-08-24 | 江苏大学 | A kind of preparation method of hydrophobicity antiradar reflectivity glass surface |
| CN108439818B (en) * | 2018-03-19 | 2020-07-31 | 江苏大学 | Preparation method of hydrophobic low-reflectivity glass surface |
| CN108545753A (en) * | 2018-04-19 | 2018-09-18 | 常州大学 | A kind of network-like SiO2Plate film sol and its preparation method and application |
| CN108545753B (en) * | 2018-04-19 | 2021-03-23 | 常州大学 | Network SiO2Coating sol and preparation method and application thereof |
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| CN103524049B (en) | 2016-08-24 |
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