CN105753337A - Preparation method of green and environment-friendly low-cost antireflection film - Google Patents
Preparation method of green and environment-friendly low-cost antireflection film Download PDFInfo
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- CN105753337A CN105753337A CN201610115574.2A CN201610115574A CN105753337A CN 105753337 A CN105753337 A CN 105753337A CN 201610115574 A CN201610115574 A CN 201610115574A CN 105753337 A CN105753337 A CN 105753337A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/23—Oxides
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/213—SiO2
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
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- Organic Chemistry (AREA)
- Surface Treatment Of Optical Elements (AREA)
- Surface Treatment Of Glass (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
The invention discloses a preparation method of a green and environment-friendly low-cost antireflection film. The preparation method comprises the following steps: (1) with the monomers such as styrene and acrylate as raw materials, introducing a silicon-containing precursor and preparing core-shell organic-inorganic nano particles by an emulsion polymerization method; (2) performing pretreatment of substrate glass; (3) coating the substrate glass provided in the step (2) with the emulsion obtained in the step (1) by a dipping-pulling method; and (4) performing high-temperature treatment of the film to form a SiO2 antireflection film with a nano hollow structure. Compared with traditional antireflection film preparation method, no organic solvent is used in the preparation process of the antireflection film in the invention, and the preparation method is green and environment-friendly; and moreover, the preparation process is simple and efficient, and the cost is relatively low. The prepared antireflection film has excellent optical property, the maximum light transmittance can reach 98.8%, and average light transmittance in the visible light waveband is 98.1%.
Description
Technical field
The present invention relates to the preparation method of a kind of environmental protection low cost anti-reflection film, belong to Deposition Techniques for Optical Thin Films field.
Background technology
Anti-reflection film (is also antireflective coating), occupies highly important status in contemporary optics film production, and its production exceedes other optical thin films all.In optical system, two kinds of reasons are had to need to reduce the reflection of piece surface.The first reason be undressed optical element owing to there being reflection loss, its transmissivity is always less than 100%.Such as, the transmissivity of conventional crown glass part only has 92%, and flint glass is the lowest to 85%.Most of instruments all comprise many parts, if piece surface does not plate anti-reflection film, then the total transmittance of instrument will be lower.The second reason be the reflection light of piece surface through multiple reflections, some becomes veiling glare, finally also arrives at image plane, makes the contrast of picture reduce.This seems even more important in some applications, the camera lens of such as motion picture projection, comprises more than ten part, if not being coated with anti-reflection film, cannot use the most completely.
In daily life, anti-reflection film application is extremely wide, camera lens from instruments such as most basic telescope, television set, camera, video camera, microscopes, exhibition booth to show window, museum or the exhibition center in shop, the glass hood plate of solar panel collector, utilize the Energy-saving Building Glass of solar energy, many occasions such as the protective glass plate of instrument and meter, all use the glass being coated with anti-reflection film.
For camera gun plated film, the camera lens of the daily camera used typically is made up of polylith lens, and the light losing that reflection causes is more serious.Such as one by the camera gun of the autozoom of 35 mm of 18 pieces of set of lenses, assume that all there is the reflection of 4 % light at the interface of each glass and air, the camera light transmitance not plating anti-reflection film is 27 %, and the camera light transmitance being coated with one layer of anti-reflection film (residual reflectance is 1.3 %) is 66 %, the camera light transmitance being coated with multi-layered antireflection coating (residual reflectance is 0.5) is 85%.The most a large amount of reflection light can form shade on emulsion layer, affects photographic quality, especially when taking pictures in some backlight position, can form echo and the phenomenon such as hot spot, fold-over.After being coated with anti-reflection film, image quality is obviously improved.
At present, the main preparation methods of anti-reflection film has physical vaporous deposition, chemical vapour deposition technique and sol-gal process, especially the most extensive with collosol and gel research.Although the film that physical vaporous deposition obtains has the features such as purity is high, quality is good, thickness is easy to control, but its equipment needed thereby is complicated, need high-pressure installation, topmost shortcoming is that its film forming speed is low and energy consumption is bigger；Film prepared by chemical vapour deposition technique has that purity is high, compactness is good, well-crystallized, residual stress are little and for advantages such as complex-shaped device energy uniform coateds, but its reaction is temperature required the highest, typically will be at about 1000 DEG C, and it is higher to the requirement of material purity during deposition, which has limited the kind of coating material, substantially reduce its range.It is easily controllable that sol-gal process has course of reaction; the material component of preparation is homogeneous; the advantages such as product purity is high and technique is simple; but the variable that its course of reaction relates to is too much; collosol stability is difficult to control to and manufacturing cycle is long; and often use organic solvent when preparing coated solution, do not meet the purpose of environmental protection.
Summary of the invention
The problem such as the cost height that present invention aim at solving preparing anti-reflection film at present, method complexity, cycle length, non-environmental protection, it is provided that the preparation method of a kind of environmental protection low cost anti-reflection film.
For solving the problems referred to above, the technical solution used in the present invention is: the preparation method of a kind of environmental protection low cost anti-reflection film, it specifically comprises the following steps that
(1) add styrene, acrylic ester monomer, initiator and emulsifying agent to mix, deoxygenation, heating, after reaction, add containing silicon precursor, use the polymerization of semi-continuous process emulsion to prepare hud typed organic-inorganic nano particle；
(2) with water, nano particle prepared by step (1) is diluted to the coated solution that concentration is 5-30 %；
(3) pre-treatment of substrate glasses: by substrate glasses cleaning, after drying, process a period of time with plasma cleaner；
(4) lifting coating process: using dip-coating method, under the conditions of certain lifting temperature, pull rate, the coated solution obtained by step (2) lifts plated film in the substrate glasses that step (3) obtains；
(5) post processing of film: the film obtained in step (4) carries out high-temperature post-treatment, removes the organic matter in film, i.e. obtains the inorganic silicon dioxide anti-reflection film having nano hollow structure.
In the present invention, acrylic ester monomer described in step (1) is one or more of styrene, methyl methacrylate, vinylacetate, n-butyl acrylate, n-BMA, octadecyl methacrylate, hydroxyethyl methacrylate, dimethylaminoethyl methacrylate, hydroxy propyl methacrylate, butyl acrylate, acrylamide, ethyl acrylate or α-methacrylic acid.
In the present invention, step (1) described initiator is any one in potassium peroxydisulfate, ammonium persulfate, dibenzoyl peroxide (BPO) or DMA (DMA) etc..
In the present invention, described in step (1), emulsifying agent is for can include dodecyl sodium sulfate, alkylbenzenesulfonate, sulfosuccinic acid diisobutyl ester sodium salt, alkyl alcohol ethoxylates sodium sulphate, alkyl alcohol ethoxylates ammonium sulfate, double tridecanol sulfosuccinate sodium, iso-octyl sulfate ammonium, n-octyl sodium sulphate, methacrylic acid hydroxide sodium dimercaptosulphanatein, 2-acrylamido-2 methyl propane sulfonic acid sodium salt, ALS, Zhong Xin phenol polyethenoxy ether, castor oil polyoxyethylene ether, iso-octyl ammonium sulfate, sapn Span, tween Tween, castor oil/rilanit special and ethylene oxide condensate.
nullIn the present invention，Described in step (1), silane coupler is methyl silicate、Tetraethyl orthosilicate、Positive silicic acid propyl ester、MTMS、Trimethoxysilyl propyl methacrylate TMOS、Propyl trimethoxy silicane、Propyl-triethoxysilicane、Octyl group trimethoxy silane、Octyltri-ethoxysilane、Isooctyltrimethoxysi,ane、Isooctyltriethoxysilane、Hexadecyl trimethoxy silane、Hexadecyl、Phenyltrimethoxysila,e、Phenyl triethoxysilane、Dimethoxydiphenylsilane、Diphenyl diethoxy silane、Aminomethyl phenyl dimethoxysilane、Aminomethyl phenyl diethoxy silane、Vinyltrimethoxy silane、Epoxy radicals trimethoxy silane、Epoxy radicals triethoxysilane、Aminopropyl trimethoxysilane、Epoxy radicals triethoxysilane、Dimethyldimethoxysil,ne、One or more in the silane couplers such as methyl allyl acyloxypropyl trimethoxysilane.
In the present invention, the plasma cleaner process time of substrate glasses described in step (3) is 1-5 min.
In the present invention, lifting temperature and be 20-80 DEG C described in step (4), pull rate is 150-500 μm/min.
In the present invention, described in step (5), film post-processing temperature is 400-500 DEG C.
Beneficial effects of the present invention:
(1) the anti-reflection film preparation process of the present invention is simple, and cost is relatively low.
(2) the anti-reflection film preparation process of the present invention does not use any organic solvent, be the preparation process of an environmental protection.
(3) anti-reflection film prepared by the present invention possesses fabulous optical property, and maximum transmission is up to 98.8 %, it is seen that light district average transmittance is up to 98.1 %.
Accompanying drawing explanation
Fig. 1 is the TEM photo of hud typed organic-inorganic nano particle in the present invention.
Fig. 2 is the dynamic light scattering grain size distribution of hud typed organic-inorganic nano particle in the present invention.
Fig. 3 is the SEM photograph on specific embodiment 1 anti-reflection film surface in the present invention.
Fig. 4 is the contrast of anti-reflection film and the substrate glasses light transmittance prepared in specific embodiment 1 in the present invention.
Fig. 5 is the SEM photograph on specific embodiment 2 anti-reflection film surface in the present invention.
Fig. 6 is the contrast of anti-reflection film and the substrate glasses light transmittance prepared in specific embodiment 2 in the present invention.
Detailed description of the invention
Embodiment 1
(1) preparation of nuclear shell type nano meter particle: after 40 g styrene, 30g n-butyl acrylate, 2 g α-methacrylic acids, the double tridecanol sulfosuccinate sodium of 1.5g, 4 g 2% ammonium persulfates and the mixing of 60 g water, emulsify 30 min；Then in four-hole boiling flask, add 80g water, 2.6g20% ammonium persulfate, be warming up to 80 DEG C, be passed through nitrogen 30min deoxygenation simultaneously；Subsequently pre-emulsion is at the uniform velocity instilled in four-hole bottle with constant flow pump in 1 h, react 3 h；It is eventually adding 20 g positive silicic acid propyl ester, reacts 1 h, obtain hud typed organic-inorganic nano particle.
(2) the hud typed organic-inorganic nano particle deionized water obtained in step (1) is diluted to the coated solution of 20% concentration.
(3) cleaned substrate glasses plasma cleaner is processed 1 min.
(4) use dip-coating method, to lift temperature 60 DEG C, the condition of pull rate 150 μm/min, use coated solution in step (2), the substrate glasses obtained in step (3) lifts plated film.
(5) film calcination 4 h at 500 DEG C that will obtain in step (4), obtains the antireflecting silicon dioxide film with loose structure.
The maximum transmission rate of the glass being coated with anti-reflection film of gained can reach 98.8 %, improves 6.8 % than uncoated glass, and visible region average transmittance is 98.1 %, has good antireflective effect.
Embodiment 2
(1) preparation of nuclear shell type nano meter particle: after 30 g styrene, 40g n-butyl acrylate, 2 g α-methacrylic acids, the double tridecanol sulfosuccinate sodium of 1.4g, 3.8g 2% potassium peroxydisulfate and the mixing of 60 g water, emulsify 30 min；Then in four-hole boiling flask, add 80g water, 2.6g20% potassium peroxydisulfate, be warming up to 80 DEG C, be passed through nitrogen 30min deoxygenation simultaneously；Subsequently pre-emulsion is at the uniform velocity instilled in four-hole bottle with constant flow pump in 1 h, react 3 h；It is eventually adding 30 g positive silicic acid propyl ester, reacts 1 h, obtain hud typed organic-inorganic nano particle.
(2) the hud typed organic-inorganic nano particle deionized water obtained in step (1) is diluted to the coated solution of 20% concentration.
(3) cleaned substrate glasses plasma cleaner is processed 1 min.
(4) use dip-coating method, to lift temperature 60 DEG C, the condition of pull rate 350 μm/min, use coated solution in step (2), the substrate glasses obtained in step (3) lifts plated film.
(5) film calcination 4 h at 400 DEG C that will obtain in step (4), obtains the antireflecting silicon dioxide film with loose structure.
The maximum transmission rate of the glass being coated with anti-reflection film of gained can reach 98.7 %, improves 6.7 % than uncoated glass, and visible region average transmittance is 96.5 %, has good antireflective effect.
Claims (9)
1. the preparation method of an environmental protection low cost anti-reflection film, it is characterised in that specifically comprise the following steps that
(1) preparation of hud typed organic-inorganic nano particle: with water as solvent, add styrene, acrylic ester monomer, initiator and emulsifying agent to mix, deoxygenation, heating, after reaction, add containing silicon precursor, use the polymerization of semi-continuous process emulsion to prepare hud typed organic-inorganic nano particle；
(2) with water, nano particle prepared by step (1) is diluted to the coated solution that concentration is 5-30 %；
(3) pre-treatment of substrate glasses: by substrate glasses cleaning, after drying, process with plasma cleaner；
(4) coating process: use dip-coating method or spin-coating method, the coated solution plated film in the substrate glasses that step (3) obtains obtained by step (2), obtain film；
(5) post processing of film: the film that step (4) obtains carries out high-temperature post-treatment, removes the organic matter in film, i.e. obtains the antireflecting silicon dioxide film of inorganic nano hollow-core construction.
The preparation method of a kind of environmental protection low cost anti-reflection film the most according to claim 1, it is characterised in that: the particle diameter of the hud typed organic-inorganic nano particle prepared by step (1) is 40-150nm.
The preparation method of a kind of environmental protection low cost anti-reflection film the most according to claim 1, it is characterised in that: acrylic ester monomer described in step (1) includes in methyl methacrylate, vinylacetate, n-butyl acrylate, n-BMA, octadecyl methacrylate, hydroxyethyl methacrylate, dimethylaminoethyl methacrylate, hydroxy propyl methacrylate, butyl acrylate, acrylamide, ethyl acrylate or α-methacrylic acid more than one.
The preparation method of a kind of environmental protection low cost anti-reflection film the most according to claim 1, it is characterised in that: initiator described in step (1) is any one in potassium peroxydisulfate, ammonium persulfate, dibenzoyl peroxide or DMA.
The preparation method of a kind of environmental protection low cost anti-reflection film the most according to claim 1, it is characterized in that: the emulsifying agent in step (1) is the compounding of anionic emulsifier and nonionic emulsifier, specifically include dodecyl sodium sulfate, alkylbenzenesulfonate, sulfosuccinic acid diisobutyl ester sodium salt, alkyl alcohol ethoxylates sodium sulphate, alkyl alcohol ethoxylates ammonium sulfate, double tridecanol sulfosuccinate sodium, iso-octyl sulfate ammonium, n-octyl sodium sulphate, methacrylic acid hydroxide sodium dimercaptosulphanatein, 2-acrylamido-2 methyl propane sulfonic acid sodium salt, ALS, Zhong Xin phenol polyethenoxy ether, castor oil polyoxyethylene ether, iso-octyl ammonium sulfate, sapn Span, tween Tween, in castor oil/rilanit special and ethylene oxide condensate any one.
nullThe preparation method of a kind of environmental protection low cost anti-reflection film the most according to claim 1，It is characterized in that: described in step (1), silane coupler is methyl silicate、Tetraethyl orthosilicate、Positive silicic acid propyl ester、MTMS、Trimethoxysilyl propyl methacrylate TMOS、Propyl trimethoxy silicane、Propyl-triethoxysilicane、Octyl group trimethoxy silane、Octyltri-ethoxysilane、Isooctyltrimethoxysi,ane、Isooctyltriethoxysilane、Hexadecyl trimethoxy silane、Hexadecyl、Phenyltrimethoxysila,e、Phenyl triethoxysilane、Dimethoxydiphenylsilane、Diphenyl diethoxy silane、Aminomethyl phenyl dimethoxysilane、Aminomethyl phenyl diethoxy silane、Vinyltrimethoxy silane、Epoxy radicals trimethoxy silane、Epoxy radicals triethoxysilane、Aminopropyl trimethoxysilane、Epoxy radicals triethoxysilane、One or more in dimethyldimethoxysil,ne or methyl allyl acyloxypropyl trimethoxysilane.
The preparation method of a kind of environmental protection low cost anti-reflection film the most according to claim 1, it is characterised in that: in step (3), the plasma cleaner process time of substrate glasses is 1-5 min.
The preparation method of a kind of environmental protection low cost anti-reflection film the most according to claim 1, it is characterised in that: controlling lifting temperature in step (4) and be 20-80 DEG C, pull rate is 150-500 μm/min.
The preparation method of a kind of environmental protection low cost anti-reflection film the most according to claim 1, it is characterised in that: the film post-processing temperature in step (5) is 400-500 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107140843A (en) * | 2017-05-09 | 2017-09-08 | 同济大学 | A kind of preparation method of automatically cleaning Water antireflection film |
| CN107193062A (en) * | 2017-05-08 | 2017-09-22 | 同济大学 | A kind of bowl pockets structure high-performance broadband extensive angle anti-reflection film |
| CN109694594A (en) * | 2018-11-14 | 2019-04-30 | 东莞南玻太阳能玻璃有限公司 | A kind of high anti-reflection stain resistance antireflective coating liquid and preparation method thereof and solar-energy photo-voltaic cell packaged glass |
| CN110828582A (en) * | 2018-07-23 | 2020-02-21 | 北京铂阳顶荣光伏科技有限公司 | Post-processing method of anti-reflection and anti-reflection film for solar cell |
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| CN103756395A (en) * | 2014-01-22 | 2014-04-30 | 上海赛肯森材料科技有限公司 | Nano hybrid particle for anti-reflection coating combination as well as preparation method and purpose of nano hybrid particle |
| CN104945647A (en) * | 2015-04-14 | 2015-09-30 | 常州大学 | Preparation method of antireflection PET (polyethylene terephthalate) film |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP2644675A2 (en) * | 2010-11-24 | 2013-10-02 | LG Hausys, Ltd. | Adhesive composition for touch panel, adhesive film, and touch panel |
| CN102153292A (en) * | 2010-12-27 | 2011-08-17 | 上海师范大学 | High-transmission nano silicon dioxide anti-reflection film and preparation method and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107193062A (en) * | 2017-05-08 | 2017-09-22 | 同济大学 | A kind of bowl pockets structure high-performance broadband extensive angle anti-reflection film |
| CN107140843A (en) * | 2017-05-09 | 2017-09-08 | 同济大学 | A kind of preparation method of automatically cleaning Water antireflection film |
| CN110828582A (en) * | 2018-07-23 | 2020-02-21 | 北京铂阳顶荣光伏科技有限公司 | Post-processing method of anti-reflection and anti-reflection film for solar cell |
| CN109694594A (en) * | 2018-11-14 | 2019-04-30 | 东莞南玻太阳能玻璃有限公司 | A kind of high anti-reflection stain resistance antireflective coating liquid and preparation method thereof and solar-energy photo-voltaic cell packaged glass |
| CN109694594B (en) * | 2018-11-14 | 2021-01-01 | 东莞南玻太阳能玻璃有限公司 | High-anti-reflection smudge-resistant antireflection coating liquid, preparation method thereof and solar photovoltaic cell packaging glass |
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