CN106733548A - A kind of preparation method of the double-deck oxidation silicone self-cleaning antireflective film of the modified homogeneity in surface - Google Patents

A kind of preparation method of the double-deck oxidation silicone self-cleaning antireflective film of the modified homogeneity in surface Download PDF

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CN106733548A
CN106733548A CN201710013067.2A CN201710013067A CN106733548A CN 106733548 A CN106733548 A CN 106733548A CN 201710013067 A CN201710013067 A CN 201710013067A CN 106733548 A CN106733548 A CN 106733548A
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layer
film
refractive index
homogeneity
antireflective film
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张政军
乐雅
淮晓晨
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Tsinghua University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/10—Glass or silica
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/28—Vacuum evaporation by wave energy or particle radiation
    • C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2506/00—Halogenated polymers
    • B05D2506/10—Fluorinated polymers

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  • Mechanical Engineering (AREA)
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Abstract

A kind of preparation method of the double-deck oxidation silicone self-cleaning antireflective film of the modified homogeneity in surface, the present invention uses electron beam evaporation methods, compact silicon dioxide layer and porous silicon dioxide nano rod layer that two-layer refractive index is progressively successively decreased are sequentially depositing in transparent or semitransparent substrate, refractive index per layer film is controlled by the incident angle of electron beam evaporation plating, and thickness is adjusted according to substrate difference.The mixed solution for finally being constituted with perfluoro capryl trichlorosilane and n-hexane carries out surface chemical modification treatment to the laminated film.Research finds：In addition to there is multi-angle incident light of the laminated film in visible-range good anti-reflection to act on, surface chemical modification treatment also makes its surface by amphipathic property qualitative change into hydrophobic oleophobic property, antireflective film automatically cleaning effect is greatly improved, the application request of the surface such as optics, photonic device, colour filter anti-reflection can be met.

Description

A kind of preparation method of the double-deck oxidation silicone self-cleaning antireflective film of the modified homogeneity in surface
Technical field
Processing method the present invention relates to carry out surface chemical modification to inorganic non-metallic sull, more particularly to one The surface modifying method of the double-deck oxidation silicone self-cleaning antireflective film of homogeneity is planted, belongs to optical anti-reflection thin film technique field.
Background technology
Anti-reflection film is also referred to as antireflective film, because the light that can effectively reduce material surface reflects, increases the transmission capacity of light, A kind of extremely wide thin-film material of range of application, be widely used in daily life, machinery, electronics, laser, medical science, industry, The fields such as astronomy, military affairs.For example：All kinds of optical lens, photoelectric device, digital information display, dielectric film, electric thin, The required antireflection antireflecting coating such as optoelectronic film, colour filter, optical recorder.Antireflective film is mainly by transparent or semitransparent Substrate surface deposits the film that one or more layers refractive index changes in gradient, and incident light can reflect at different materials interface, Interfering between reflected light, makes its phase and amplitude cancel out each other, so as to reduce the reflectivity of light, improves the transmission of light Rate.Yet with actual application, most of antireflective film surface is generally hydrophilic nmature, the washing away of steam, oil in environment Fat, organic pollution, dust etc. are contaminated material surface, so as to reduce the antireflection of antireflective film in the absorption of film surface Property and stability, influence antireflective film practical application effect.Traditional improved method is to antireflective film surface using surfactant Cleaned, this not only aggravates environmental pollution, and needs are repeated, and expend substantial amounts of manpower and financial resources.Therefore hair is needed The anti-reflection membrane preparation technology of Zhan Xin, while the effect of film anti-reflection is improved, will also change film surface to steam, grease Deng the wetability of pollutant, to meet the requirement in practical application to self-cleaning performance.
The content of the invention
It is an object of the invention to provide the homogeneity bilayer silica (SiO that a kind of surface is modified2) automatically cleaning antireflective film system Preparation Method, enables the antireflective film prepared by it to be respectively provided with good anti-reflection for the multi-angle incident light in visible-range Power, while also having excellent automatic cleaning action, is expected to meet the device surfaces such as optics, photonic device, colour filter to subtracting The application request of anti-anti-reflection film automatically cleaning effect.
In order to achieve the above object, the technical solution adopted by the present invention is：
A kind of preparation method of the double-deck oxidation silicone self-cleaning antireflective film of the modified homogeneity in surface, it is characterised in that the method bag Include following steps：
1) electron beam evaporation methods are utilized, angle of deposit is first set as 0 °, deposited in transparent or semitransparent substrate A layer thickness is the compact silicon dioxide layer of 50~55nm；
2) angle of deposit is set as 80 °, obtain compact silicon dioxide layer on, deposition a layer thickness be 110~ The porous silicon dioxide nano rod layer of 115nm, porosity is 60%~70%；
3) dose volume percentage concentration is the mixing of 0.005~0.03% perfluoro capryl trichlorosilane and n-hexane composition Solution is molten；
4) by step 2) in the mixed solution prepared of the deposition that the obtains substrate immersion that has homogeneity bilayer silica, leaching Bubble time about 40~80S, makes one layer of fluorine octyltrichlorosilane of adsorption and n-hexane group of porous silicon dioxide nano rod layer Into macromolecule layer.
In above-mentioned technical proposal, the porosity of described porous silicon dioxide nano rod layer is 60%~70%；The cause The refractive index of close silicon oxide layer is 1.21~1.45, and the refractive index of porous oxidation silicon nanorod layer is 1.17~1.21, polytetrafluoro The refractive index of ethene nanometer rods layer is 1~1.17.
During the transparent or semitransparent substrate includes quartz plate, BK7, SF5, LAK14, FTO and sends Simon Rex glass Any one, their refractive index is between 1.45~1.95.
Antireflective film prepared by the present invention has the technique effect of advantages below and high-lighting：1. antireflection：By in base The film that two-layer refractive index changes in gradient is deposited on body, segmentation reduces matrix with environment to the refractive index difference of light, makes outermost The reflection of light is down to or is reduced close to 1 to interfacial refraction rate between layer film and environment.2. self-cleaning property：Using perfluoro capryl The mixed solution of trichlorosilane and n-hexane composition carries out surface chemical modification treatment to the laminated film, can be by chemical surface Absorption, makes porous SiO2Nanorod surfaces adsorb the macromolecule layer of one layer of fluorine octyltrichlorosilane and n-hexane composition.High score Sub- material specific strength is high, water insoluble, and it is coated in antireflective film surface, can improve film surface to pollutants such as steam, greases Contact angle, wetability of these pollutants to film surface is reduced, so that film possesses automatically cleaning effect.Actually used During will not receive environment steam, grease, the pollution of dust granule and reduce the anti-reflective of film.
Brief description of the drawings
Fig. 1 is the schematic cross-section of the double-deck oxidation silicone self-cleaning antireflective film of the modified homogeneity in surface of the present invention.
Wherein：1- substrates；2- densifications SiO2Layer；The porous SiO of 3-2Nanometer rods layer.Incident light is in air-porous SiO2Nanometer Rod bed boundary, bilayer SiO2There is reflection at interface and antireflective film-substrate interface and transmit.
Fig. 2 is that the cross-sectional scans Electronic Speculum in kind of the double-deck oxidation silicone self-cleaning antireflective film of the modified homogeneity in surface of the present invention is shone Piece.
Fig. 3 is the experiment of the Normal incidence reflectance rate of the double-deck oxidation silicone self-cleaning antireflective film of the modified homogeneity in surface of the present invention Value and calculated value.
Wherein：Ds is represented and is utilized optical software, calculates the Normal incidence reflectance rate in the BK7 deposition on glass antireflective film； De is represented according to optical software result of calculation, and the Normal incidence reflectance of the antireflective film is deposited using electron beam evaporation equipment experiment Rate.
Fig. 4 is different incidence angles of the double-deck oxidation silicone self-cleaning antireflective film of the modified homogeneity in surface of the present invention in visible ray Three-dimensional reflection rate under degree, different wave length.
Fig. 5 is the vertical reflectivity of room temperature and process of the double-deck oxidation silicone self-cleaning antireflective film of the modified homogeneity in surface of the present invention Vertical reflectivity after 100 DEG C of annealings.
Fig. 6 is the vertical reflectivity of room temperature and process of the double-deck oxidation silicone self-cleaning antireflective film of the modified homogeneity in surface of the present invention Vertical reflectivity after 200 DEG C of annealings.
Fig. 7 is the vertical reflectivity of room temperature and process of the double-deck oxidation silicone self-cleaning antireflective film of the modified homogeneity in surface of the present invention Vertical reflectivity after 300 DEG C of annealings.
Specific embodiment
The preparation method of the homogeneity bilayer SiO2 automatically cleaning antireflective films that a kind of surface that the present invention is provided is modified, first with The thickness and refractive index of the compound antireflective films of TFCalc optical software simulated dual-layers SiO2, find and optimize anti-reflection parameter；Then, root Calculated according to simulation, be sequentially depositing the fine and close SiO2 that double-deck refractive index is progressively successively decreased in transparent or semitransparent substrate surface successively With porous SiO2 nanometer rods laminated films；Then using the mixed solution of perfluoro capryl trichlorosilane and n-hexane composition to this Laminated film carries out surface chemical modification treatment.The refractive index of the dense oxide silicon layer is 1.21~1.45, porous silica The refractive index of nanometer rods layer is 1.17~1.21, and the refractive index of polytetrafluorethylenano nano rod layer is 1~1.17.
Refractive index per layer film is controlled by the incident angle of electron beam evaporation plating, and thickness is adjusted according to substrate difference；It Thickness be respectively 50~55nm, 110~115nm；Wherein porous SiO2The porosity of layer is 65%~67%.It is described transparent Translucent substrate using quartz plate, BK7, SF5, LAK14, FTO or send in Simon Rex glass any one, their refraction Rate is between 1.45~1.95.
It specifically includes following steps：
1) at room temperature, transparent or semitransparent substrate is fixed on the sample stage of electron beam evaporation deposition machine；Using SiO2It is deposition material, electron beam equipment vacuum is evacuated to 3 × 10-4Pa；The transparent or semitransparent substrate include quartz plate, BK7, SF5, LAK14, FTO and any one in Simon Rex glass is sent, their refractive index is between 1.45~1.95.
2) angle of deposit is set as 0 °, it is the fine and close SiO of 50~55nm that a layer thickness is deposited in BK7 substrates2Layer；
3) angle of deposit is set as 80 °, in the fine and close SiO by 2) obtaining2On layer, deposition a layer thickness be 110~ 115nm porous SiO2Nanometer rods, porosity is 65%~67%；
4) dose volume percentage concentration be 0.005~0.03% perfluoro capryl trichlorosilane and n-hexane mixing it is molten Liquid, wherein n-hexane are solvent, then by the upper homogeneity bilayer SiO of deposition2Substrate immersion prepare mixed solution in, during immersion Between about 40~80S, make porous silicon dioxide nano rod layer one layer of fluorine octyltrichlorosilane of adsorption and n-hexane composition Macromolecule layer.
The present invention is illustrated with reference to the accompanying drawings and examples.Following embodiments are illustrative, are not limits Qualitatively, it is impossible to limit protection scope of the present invention with following embodiments.
Embodiment 1
1) using bilayer SiO in TFCalc optical softwares simulation BK7 substrate of glass2The thickness and refractive index of antireflective film, seek Optimization anti-reflection parameter is looked for, its light normal-incidence reflection rate at reference wavelength 550nm is down to 0；Wherein BK7 glass is anti- The rate of penetrating is 4.267%, is 1.52 in the refractive index of 550nm reference wavelengths；
2) SiO that refractive index is progressively successively decreased is deposited in substrate successively2/SiO2Nanometer rods laminated film.Specific steps are such as Under：
1. clean BK7 substrate of glass is fixed on the sample stage of electron beam evaporation deposition machine；
2. at room temperature, using SiO2Be deposition material, by the chamber of electron beam evaporation deposition machine be evacuated to vacuum be by Electron beam equipment vacuum is evacuated to 3 × 10-4Pa；
3. angle of deposit is set as 0 °, it is the fine and close SiO of 55nm that a layer thickness is deposited in BK7 substrates2Layer；
4. angle of deposit is set as 80 °, in the fine and close SiO for obtaining2On layer, deposition a layer thickness is that 115nm is porous SiO2Nanometer rods；
5. by the upper homogeneity bilayer SiO of deposition2Substrate immersion perfluoro capryl trichlorosilane and n-hexane composition volume hundred During point concentration is 0.01% mixed solution, time about 40~60S carries out surface chemical modification treatment；
3) Fig. 1, Fig. 2 are combined, the refractive index of laminated film is from fine and close SiO2Layer arrives porous SiO2Nanometer rods layer is gradually reduced. Porous SiO2The refractive index of nanometer rods layer depends on its porosity, and the refractive index with macroporosity film is small.Its refractive index It is 1.19 in 550nm reference waves strong point, corresponding porosity is respectively 66%.
Substrate light normal-incidence reflection rate at reference wavelength 550nm is down to from 4.267% and is connect as seen from Figure 3 0 is bordering on, and experimental result is consistent with analog result.As shown in table 1：Wherein ds is represented using optical software calculating in BK7 glass The Normal incidence reflectance rate of the two-layer compound antireflective film deposited on glass；De is represented according to optical software result of calculation, using electricity The Normal incidence reflectance rate of the compound antireflective film of beamlet evaporation equipment experiment deposition.
The modified homogeneity bilayer SiO in the surface of table 12The reflectivity % of automatically cleaning antireflective film
Meanwhile, we are also analyzed when the light of different wave length enters the reflection of the compound antireflective film from incidence angles degree Rate.Such as Fig. 4, in whole visible-range and in the case of incident angle difference, the mass reflex rate of the antireflective film is less than 1.7%, or even the reflectivity also only 1.2~1.7% when higher than 750nm wavelength, it was demonstrated that the compound antireflective film it is excellent Anti-reflection effect.
4) there is excellent self-cleaning property and temperature stability in order to illustrate the laminated film, by its with come to the surface Learn the double-deck SiO of modification2Film has carried out Experimental comparison：
Specific experiment is：The laminated film is made annealing treatment in 100 DEG C, 200 DEG C, 300 DEG C respectively, film pair is measured The reflectivity and film of visible ray are to deionized water, the contact angle of castor oil.
A. after annealed treatment, the laminated film is almost unchanged to the reflectivity of visible ray, and maximum deviation is ± 0.3%.
B. before and after making annealing treatment, the double-deck SiO of surface chemical modification treatment is not carried out2Film is to deionized water, castor oil Contact angle it is constant, be respectively 9 °, 7 °；The modified homogeneity bilayer SiO in surface of the invention2Automatically cleaning antireflective film to go from Sub- water, the contact angle of castor oil increase with the rising of temperature, and are all higher than 90 ° (referring to following table).Illustrate to use perfluor The mixed solution of octyltrichlorosilane and n-hexane composition carries out surface chemical modification treatment to the laminated film, can make film table Face greatly improves antireflective film automatically cleaning effect by amphipathic property qualitative change into hydrophobic oleophobic property, can meet optics, The application request of the surface such as photonic device, colour filter anti-reflection.
Contact angle of the 3 two kinds of antireflective films of table to deionized water
Contact angle of the 4 two kinds of antireflective films of table to castor oil
Embodiment 1 fully meets technique effect of the invention, i.e.,：
1) antireflection：By the film changed in gradient in substrate deposit two-layer refractive index, segmentation reduces matrix and ring Border makes the interfacial refraction rate between outermost layer film and environment be down to or be reduced close to 1 the anti-of light the refractive index difference of light Penetrate.
2) self-cleaning property：The mixed solution constituted using perfluoro capryl trichlorosilane and n-hexane is carried out to the laminated film Surface chemical modification is processed, and can be adsorbed by chemical surface, makes porous SiO2Nanorod surfaces adsorb one layer of fluorine octyl group trichlorine The macromolecule layer of silane and n-hexane composition.Macromolecular material specific strength is high, water insoluble, and it is coated in antireflective film surface, meeting Film surface is improved to the contact angle of the pollutants such as steam, grease, wetability of these pollutants to film surface is reduced, so that Film is set to possess automatically cleaning effect.In actual use will not by environment steam, grease, the pollution of dust granule and reduce The anti-reflective of film.

Claims (4)

1. a kind of modified homogeneity bilayer in surface aoxidizes the preparation method of silicone self-cleaning antireflective film, it is characterised in that the method includes Following steps：
1) electron beam evaporation methods are utilized, angle of deposit is first set as 0 °, one layer is deposited in transparent or semitransparent substrate Thickness is the compact silicon dioxide layer of 50~55nm；
2) angle of deposit is set as 80 °, on the compact silicon dioxide layer for obtaining, deposition a layer thickness is 110~115nm's Porous silicon dioxide nano rod layer, porosity is 60%~70%；
3) dose volume percentage concentration is that the mixing that 0.005~0.03% perfluoro capryl trichlorosilane and n-hexane are constituted is molten Liquid；
4) by step 2) in the mixed solution prepared of the deposition that the obtains substrate immersion that has homogeneity bilayer silica, during immersion Between be 40~80S, make porous silicon dioxide nano rod layer one layer of fluorine octyltrichlorosilane of adsorption and n-hexane composition Macromolecule layer.
2. according to a kind of preparation method of the double-deck oxidation silicone self-cleaning antireflective film of modified homogeneity of the surface described in claim 1, It is characterized in that：The porosity of described porous silicon dioxide nano rod layer is 60%~70%.
3. according to a kind of preparation method of the double-deck oxidation silicone self-cleaning antireflective film of modified homogeneity of the surface described in claim 1, It is characterized in that：The refractive index of the dense oxide silicon layer is 1.21~1.45, and the refractive index of porous oxidation silicon nanorod layer is
1.17~1.21, the refractive index of polytetrafluorethylenano nano rod layer is 1~1.17.
4. a kind of homogeneity bilayer silica and the compound automatically cleaning of polytetrafluoroethylene (PTFE) according to claim 1,2 or 3 subtract The preparation method of anti-film, it is characterised in that the transparent or semitransparent substrate includes quartz plate, BK7, SF5, LAK14, FTO With send any one in Simon Rex glass, their refractive index is between 1.45~1.95.
CN201710013067.2A 2017-01-09 2017-01-09 A kind of preparation method of the double-deck oxidation silicone self-cleaning antireflective film of the modified homogeneity in surface Pending CN106733548A (en)

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CN109283602A (en) * 2017-07-19 2019-01-29 日亚化学工业株式会社 Manufacturing method, film forming material, optical thin film and the optical component of film
CN107193063A (en) * 2017-07-24 2017-09-22 福建农林大学 It is a kind of to improve SiO simultaneously2The method of anti-reflection film hydrophobicity and oleophobic property
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CN111164140A (en) * 2017-09-29 2020-05-15 日东电工株式会社 Void layer, laminate, method for producing void layer, optical member, and optical device
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US11396614B2 (en) 2017-09-29 2022-07-26 Nitto Denko Corporation Void-containing layer, laminate, method for producing void-containing layer, optical member, and optical apparatus
CN108754432A (en) * 2018-04-28 2018-11-06 浙江福莱新材料股份有限公司 A kind of cold lamination film antireflection layer and preparation method thereof
CN108598193A (en) * 2018-05-24 2018-09-28 圣晖莱南京能源科技有限公司 A kind of flexible CIGS solar battery component
CN113149458A (en) * 2021-02-26 2021-07-23 中建材蚌埠玻璃工业设计研究院有限公司 Cover plate glass of colored photovoltaic module and preparation method thereof
CN113149458B (en) * 2021-02-26 2023-08-22 中建材玻璃新材料研究院集团有限公司 Color photovoltaic module cover plate glass and preparation method thereof

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