CN101935168A - Preparation method of self-cleaning antireflection film with photocatalytic function on surface - Google Patents
Preparation method of self-cleaning antireflection film with photocatalytic function on surface Download PDFInfo
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- CN101935168A CN101935168A CN 201010262335 CN201010262335A CN101935168A CN 101935168 A CN101935168 A CN 101935168A CN 201010262335 CN201010262335 CN 201010262335 CN 201010262335 A CN201010262335 A CN 201010262335A CN 101935168 A CN101935168 A CN 101935168A
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Abstract
The invention discloses a preparation method of a self-cleaning antireflection film with the photocatalytic function on the surface, relating to the field of solar photocatalysis. The method comprises the following steps of: proportionally mixing silica sol obtained through the acid catalysis and the base catalysis of acetate orthosilicate; firstly, coating an antireflection film on a clean glass surface by using a czochralski method; then, coating a layer of titania sol prepared through the hydrolysis of N-butyl titanate; and solidifying at 120 DEG C for 2 h and thermally treating at 500 DEG C for 2 h to obtain the self-cleaning antireflection film with the transmittance over 96 percent and the photocatalytic function on the surface. The antireflection film on the glass surface has higher transmittance while ensuring the firm combination with the glass; and the surface of the antireflection film has the photocatalytic function and the self-cleaning function.
Description
Technical field
The present invention relates to the self-cleaning antireflective film preparation method that a kind of surface has photo-catalysis function, relate to the solar energy photocatalytic field.
Background technology
No matter be the photo-thermal conversion using of the photovoltaic generation or the sun power of sun power, all need the sunlight Watch glass (pipe) that sees through as much as possible is converted to electricity or heat by opto-electronic conversion battery or photo-thermal baffle again.With present glass manufacture craft, the best glass of transmittance also can only reach 90% transmittance.Still there is the sunlight about 10% can not reach photoelectricity or photo-thermal converting member.In order to improve the utilization ratio of sunlight, need increase at glass surface and be coated with one or more layers antireflective film, to reduce the reflection of light.Simultaneously, because solar opto-electronic board or the device in the solar energy thermal conversion in the photovoltaic generation often are in abominable field work environment, glass surface dust, greasy dirt, rainwater etc. pollute unavoidable, and the transmitance that this also can reduce sunlight greatly influences light-electricity and light-thermal conversion efficiency.Therefore, require glass surface increase be coated with antireflective film in, glass surface also should possess certain self-cleaning ability.
Nineteen thirty-seven, Bruch has been coated with the individual layer antireflective film at glass surface first, after this this technology has obtained using widely in various fields, for example, precision optics camera lenses such as the prism of the object lens of photographic camera, the camera lens of Kamera, telescopical lens and microscope, stadimeter and swab handle and lens, liquid-crystal display, glass curtain wall, glass surfaces such as laser window all add and have plated anti-reflection film.With the transmittance that increases glass, the purpose that reaches the reflection of minimizing light.The glass coating technology that adopts mainly contains at present: physical vapor deposition, chemical Vapor deposition process, plasma reinforced chemical vapour deposition, ion beam assisted depositing, molecular beam epitaxy, vacuum-evaporation, magnetic control system sputtering method and sol-gel method.Used anti-reflection material comprises nano metal and nonmetal oxide, for example SiO
2, ZrO
2, TiO
2, CeO
2, MgF
2, Ta
2O
5Deng.Wherein sol-gel method has does not need cost and complex equipment, technology is simple, with low cost, controllable structure, be fit to large-area coating film, and can be from characteristics such as molecular level design and cuttings, become film coating method with fastest developing speed in nearly 30 years, and on light, electricity, magnetic functional materials, realized industrial applications.In the selection of antireflective film material, because silica membrane low price, specific refractory power is moderate, the surface strength height, it is the first-selection of glass surface antireflective film material, utilize the sol-gel hydrolysis to prepare silicon sol two kinds of methods are arranged, or the silicon sol that utilizes acid catalysiss such as hydrochloric acid to obtain, it is little to be characterized in forming the sol particle degree, combine firmly with glass surface, but specific refractory power is higher, shortcoming is that the antireflective film transmittance that forms is on the low side, patent ZL200920005801.1 utilizes acid catalysis to ethyl silicate hydrolysis rotary plating exactly, and its transmittance only can reach 94%.And the silicon sol that utilizes base catalysiss such as ammoniacal liquor to obtain, it is big to be characterized in forming the sol particle degree, effective in the antireflective film anti-reflection that glass surface forms, if do not consider the industrialization practicality, can even bring up to more than 99% the transmittance of sheet glass, but film and glass bonded firmness extreme difference can't carry out actual use.The colloidal sol of acid catalysis and base catalysis preparation is mixed by a certain percentage, can take into account both advantages, promptly kept higher transmittance, simultaneously, have to have kept antireflective film and glass to be combined with higher firm degree.The colloidal sol that colloidal sol that patent 200910048696.4 and patent 200910127056.2 obtain the ethyl silicate base catalysis exactly and acid catalysis obtain mixes, and utilizes spin coating or dipping to lift at the glass surface plated film, obtains antireflective film after the curing.After glass surface was coated with the silicon oxide antireflective film, the vesicular structure that the surface forms made its easier dust that is subjected to, greasy dirt; the influence of rainwater; can all offset glass anti-reflection effects and lose practical value, increase again on the surface and be coated with layer protecting film and not only increase cost, tend to make translucent effect to reduce greatly.Because the anatase-type titanium oxide film has hydrophilicity, under the irradiation of UV-light, photocatalysis performance is arranged, effectively decomposing organic matter has self-cleaning function in the pollution of film surface, and to be coated with one deck thin film of titanium oxide be to solve one of self-cleaning method of film surface so increase on the antireflective film surface again.But the thin film of titanium oxide refractive index is too high, increases to be coated with the transmittance that thin film of titanium oxide will reduce antireflective film, and therefore accurately the thickness of controlled oxidation silicon film and thin film of titanium oxide just can obtain existing ideal anti-reflection effect, has the film of self-cleaning function simultaneously.
Summary of the invention
The object of the invention provides the self-cleaning antireflective film preparation method that a kind of surface has photo-catalysis function.
For achieving the above object, the technical solution used in the present invention is:
A kind of surface has the self-cleaning antireflective film preparation method of photo-catalysis function, carry out according to following step: be raw material with the tetraethoxysilance, dehydrated alcohol is a solvent, hydrolysis obtains the acid catalysis silicon sol to hydrochloric acid as acid catalyst, wherein the mol ratio of dehydrated alcohol, tetraethoxysilance, water and hydrochloric acid is 10-25: 1.0: 1-5: 0.01, hydrolysis 3-5 days acid catalysis colloidal sol; With the tetraethoxysilance is raw material, dehydrated alcohol is a solvent, ammonia-catalyzed obtains base catalysis colloidal sol, wherein the mol ratio of dehydrated alcohol, tetraethoxysilance, water and ammoniacal liquor is 25-45: 1: 1-5: 0.8, hydrolysis 3-5 base catalysis colloidal sol, with above-mentioned acid catalysis colloidal sol and base catalysis colloidal sol by volume 3: 1-4: 1 mixes, and is that 90% glass surface lifts and is coated with one deck antireflective film at transmittance; Wherein pull rate is 5-8mm/min, with metatitanic acid fourth fat is raw material, dehydrated alcohol is a solvent, hydrochloric acid is catalyzer, hydrolysis obtains titanium colloidal sol, dehydrated alcohol wherein, metatitanic acid fourth fat, the mol ratio of water and hydrochloric acid is 15-30: 1.0: 1-3: 0.75, hydrolysis obtains titanium colloidal sol after 1 day, with dehydrated alcohol dilution 4-5 doubly after, crystal pulling method is coated with the titanium colloidal sol of the above-mentioned condition preparation of one deck again being coated with the antireflective film surface, pull rate is 5-8mm/min, 120 ℃ of dryings 2 hours,, obtain transmittance and reach more than 96% after 2 hours through 500 ℃ of calcinings, the surface has the glass antireflective film of photo-catalysis function.
Because the technique scheme utilization, the present invention compared with prior art has following advantage:
1, the antireflective film of glass surface also has higher transmittance outside guaranteeing to combine firmly with glass.
2, there is photo-catalysis function on the antireflective film surface, has self-cleaning function.
Description of drawings
The surface that accompanying drawing 1 prepares for the embodiment of the invention one has the transmittance collection of illustrative plates of the self-cleaning antireflective film of photo-catalysis function, and ordinate zou is a transmittance among the figure, and X-coordinate is a lambda1-wavelength, the nm of unit.
Embodiment
Embodiment one: add the 53mL dehydrated alcohol successively in clean beaker, 3.2mL deionized water and about 0.04mL concentrated hydrochloric acid (massfraction is 37%), under the magnetic agitation condition, drip the 10mL tetraethoxy, ethanol wherein: tetraethoxysilance: water: the mol ratio of hydrochloric acid is 20: 1.0: 4.0: 0.01, sealing was stirred 5 hours, and room temperature ageing 3 days obtains colloidal sol I.In clean beaker, add 95mL dehydrated alcohol and 2.5mL strong aqua (massfraction is 28%) successively, magnetic agitation, drip 10mL TEOS solution, ethyl silicate wherein: water: ethanol: the mol ratio of ammoniacal liquor is 1: 2: 37: 0.8, magnetic agitation 6 hours, room temperature ageing 5 days, 78 ℃ were refluxed 8 hours, and obtained colloidal sol II.Colloidal sol II and colloidal sol I are 4: 1 mixed by volume, stir after 1 hour, obtain soda acid mixed oxidization silicon sol, are designated as colloidal sol III.
Add the 64.5mL dehydrated alcohol successively in clean beaker, 1.05mL deionized water and 2.85mL hydrochloric acid are put magnetic agitation with beaker, and drip 15ml Butyl Phthalate solution, wherein ethanol: Butyl Phthalate: water: the mol ratio of hydrochloric acid is 25: 1.0: 4.0: 0.75; The above-mentioned colloidal sol that makes is placed on and seals stir about 4 hours, ageing 1 day on the magnetic stirring apparatus.With dehydrated alcohol above-mentioned titanium colloidal sol is diluted, the mol ratio of dilution back ethanol and Butyl Phthalate is 100: 1, promptly gets titanium colloidal sol, is designated as colloidal sol IV again.
The glass substrate of 2 * 10cm (transmittance 90%) is put into sequentially in the NaOH solution of 10% hydrochloric acid and 10% and soaked respectively 2 hours, use dehydrated alcohol and distilled water through the ultrasonic wave thorough washing again, dry, glass substrate after handling was immersed among the colloidal sol III 10 minutes, on the self-control pulling machine, lifted 1 minute with 8cm/min speed, after drying, the glass substrate that will be coated with colloidal sol III again is immersed among the colloidal sol IV, on the self-control pulling machine, lifted 1 minute with 8cm/min speed, dry, 120 ℃ of thermofixations are 1 hour in the baking oven, be warmed up to 500 ℃ with 10 ℃/min temperature rise rate putting to retort furnace, be incubated 2 hours, naturally cool to room temperature, obtain the self-cleaning antireflective film glass that the surface has photo-catalysis function.
Antireflective film glass at the transmittance of 400～800nm as shown in Figure 1, its transmittance can reach more than 96% at visible light wave range.The evaluation of antireflective film photocatalysis performance is carried out in homemade photo catalysis reactor, and with 80mL 5mg/L, pH is that 3 methyl orange solution is light-catalysed target degradation product.Light source adopts 20W ultraviolet germicidal (λ
Max=253.7nm), film is changed in the absorbancy under λ=505nm by methyl orange solution before and after the 722 type spectrophotometric determination photocatalytic degradations at last and comes the evaluation concept catalytic effect apart from the about 10cm of fluorescent tube, and the result shows, through reaction in 4 hours, methyl orange degradation about 60%.
Accompanying drawing 1 has the transmittance collection of illustrative plates of the self-cleaning antireflective film of photo-catalysis function for the surface of the embodiment of the invention one preparation
(ordinate zou is a transmittance, and X-coordinate is a lambda1-wavelength, the nm of unit);
Embodiment two: with the colloidal sol II in the example 1 and colloidal sol I is 3: 1 mixed by volume, stirs after 1 hour, obtains soda acid mixed oxidization silicon sol, is designated as colloidal sol V.In clean beaker, add the 64.5mL dehydrated alcohol successively, 1.05mL deionized water and 2.85mL hydrochloric acid, beaker is placed on the magnetic stirring apparatus to stir drips 15ml Butyl Phthalate solution, wherein ethanol while stirring: Butyl Phthalate: water: the mol ratio of hydrochloric acid is 25: 1.0: 4.0: 0.75; The above-mentioned colloidal sol that makes is placed on and seals stir about 4 hours, ageing 1 day on the magnetic stirring apparatus.With dehydrated alcohol above-mentioned titanium colloidal sol is diluted, the mol ratio of dilution back ethanol and Butyl Phthalate is 150: 1, promptly gets titanium colloidal sol, is designated as colloidal sol VI again.
The glass substrate of 2 * 10cm (transmittance 90%) is put into sequentially in the NaOH solution of 10% hydrochloric acid and 10% and soaked 2 hours, use dehydrated alcohol and distilled water through the ultrasonic wave thorough washing again, dry, glass substrate after handling was immersed among the colloidal sol V 10 minutes, on the self-control pulling machine, lifted 1 minute with 5cm/min speed, after drying, the glass substrate that will be coated with colloidal sol V again is immersed among the colloidal sol VI, on the self-control pulling machine, lifted 1 minute with 5cm/min speed, dry, 120 thermofixations are 1 hour in the baking oven, be warmed up to 500 ℃ with 10 ℃/min temperature rise rate putting to retort furnace, be incubated 2 hours, naturally cool to room temperature, obtain the self-cleaning antireflective film glass that the surface has photo-catalysis function.
Antireflective film glass transmittance can reach more than 96% at visible light wave range.The evaluation of antireflective film photocatalysis performance is carried out in homemade photo catalysis reactor, and with 80mL 5mg/L, pH is that 3 methyl orange solution is light-catalysed target degradation product.Light source adopts 20W ultraviolet germicidal (λ
Max=253.7nm), film is changed in the absorbancy under λ=505nm by methyl orange solution before and after the 722 type spectrophotometric determination photocatalytic degradations at last and comes the evaluation concept catalytic effect apart from the about 10cm of fluorescent tube, and the result shows, through reaction in 4 hours, methyl orange degradation about 55%.
Claims (1)
1. a surface has the self-cleaning antireflective film preparation method of photo-catalysis function, it is characterized in that carrying out: be raw material with the tetraethoxysilance according to following step, dehydrated alcohol is a solvent, hydrolysis obtains the acid catalysis silicon sol to hydrochloric acid as acid catalyst, the mol ratio of wherein said dehydrated alcohol, tetraethoxysilance, water and hydrochloric acid is 10-25: 1.0: 1-5: 0.01, hydrolysis 3-5 days acid catalysis colloidal sol; With the tetraethoxysilance is raw material, dehydrated alcohol is a solvent, ammonia-catalyzed obtains base catalysis colloidal sol, the mol ratio of wherein said dehydrated alcohol, tetraethoxysilance, water and ammoniacal liquor is 25-45: 1: 1-5: 0.8, hydrolysis 3-5 base catalysis colloidal sol, with above-mentioned acid catalysis colloidal sol and base catalysis colloidal sol by volume 3: 1-4: 1 mixes, and is that 90% glass surface lifts and is coated with one deck antireflective film at transmittance; Wherein pull rate is 5-8mm/min, with metatitanic acid fourth fat is raw material, dehydrated alcohol is a solvent, hydrochloric acid is catalyzer, hydrolysis obtains titanium colloidal sol, wherein said dehydrated alcohol, metatitanic acid fourth fat, the mol ratio of water and hydrochloric acid is 15-30: 1.0: 1-3: 0.75, hydrolysis obtains titanium colloidal sol after 1 day, with dehydrated alcohol dilution 4-5 doubly after, crystal pulling method is coated with the titanium colloidal sol of the above-mentioned condition preparation of one deck again being coated with the antireflective film surface, pull rate is 5-8mm/min, 120 ℃ of dryings 2 hours,, obtain transmittance and reach more than 96% after 2 hours through 500 ℃ of calcinings, the surface has the glass antireflective film of photo-catalysis function.
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| CN102206434A (en) * | 2011-04-01 | 2011-10-05 | 河南思可达光伏材料股份有限公司 | Glass coating liquid for high efficient photoelectric conversion, its preparation method and application |
| CN102674705A (en) * | 2012-05-15 | 2012-09-19 | 常州龙腾太阳能热电设备有限公司 | Preparation method of wear-resistant self-cleaning anti-reflection film on surface of high-temperature vacuum collector tube |
| CN102850894A (en) * | 2012-07-03 | 2013-01-02 | 杭州和合玻璃工业有限公司 | Composite sol for anti-reflection coating and anti-reflection coated photovoltaic glass |
| CN102875032A (en) * | 2011-07-15 | 2013-01-16 | 比亚迪股份有限公司 | Sol composition, preparation method thereof, method for forming self-cleaning and anti-reflective film on glass and self-cleaning and anti-reflective glass |
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