CN109467317A - A kind of surface layer has the antireflecting silicon dioxide film and preparation method thereof of meso-hole structure with hole sealing structure internal layer - Google Patents
A kind of surface layer has the antireflecting silicon dioxide film and preparation method thereof of meso-hole structure with hole sealing structure internal layer Download PDFInfo
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- CN109467317A CN109467317A CN201910006421.8A CN201910006421A CN109467317A CN 109467317 A CN109467317 A CN 109467317A CN 201910006421 A CN201910006421 A CN 201910006421A CN 109467317 A CN109467317 A CN 109467317A
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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
- C03C17/25—Oxides by deposition from the liquid phase
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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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- 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
- C03C2217/70—Properties of coatings
- C03C2217/73—Anti-reflective coatings with specific characteristics
- C03C2217/732—Anti-reflective coatings with specific characteristics made of a single layer
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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
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/111—Deposition methods from solutions or suspensions by dipping, immersion
-
- 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
- C03C2218/00—Methods for coating glass
- C03C2218/30—Aspects of methods for coating glass not covered above
- C03C2218/32—After-treatment
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
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Abstract
The invention discloses a kind of surface layers to have the antireflecting silicon dioxide film of meso-hole structure with hole sealing structure internal layer, and the anti-reflection film is Dual-layer membrane structure, upper layer SiO2SiO in film2Nano particle densification arrangement, lower layer SiO2SiO in film2Nano particle arranges to form multiple nano aperture structures, and the aperture of described hole structure is 2~50nm.Silicon dioxide film prepared by the present invention, surface is hole sealing structure silicon dioxide film, the mesoporous silica films of bottom are reticular structure, it is tightly combined between silica condensation polymer in surface layer, to the fine and close silicon dioxide film for keeping upper layer porosity very low, since surface layer is hole-closing structure, hydrone be cannot be introduced into film hole, so that anti-reflection film has excellent environmental stability and weatherability.
Description
Technical field
The present invention relates to a kind of surface layers to have the antireflecting silicon dioxide film of meso-hole structure with hole sealing structure internal layer, further relates to
The preparation method of above-mentioned anti-reflection film, belongs to optical film technology field.
Background technique
Anti-reflection film is a kind of most widely used film of contemporary optics, using the interference of film to the reflected light of optical surface
Weakened with stray light or is eliminated to increase the transmitance of film.Preparing anti-reflection film using sol-gal process has operation letter
It is single, at low cost, be suitable for the advantages that irregular surface and large-scale industrial production, the especially refractive index of porous membrane can be with
It is significantly less than the refractive index of corresponding body material, and refractive index is continuously adjustable.And the advantages of czochralski method is that thickness is controllable, film layer is equal
Film even, that large area can be prepared.
It is coated with anti-reflection film on the glass cover-plate in solar battery main part, reduces the reflection loss to incident light, improves
Practical transfer efficiency.The wave-length coverage of solar radiation is very wide, but most energy concentrate on visible light near infrared region, but
Be it is very high in infrared band transmitance due to silicon, using seldom, therefore 400-800nm is focused on to the anti-reflection of solar battery
Range.Antireflective coating used at present is substantially exposed in atmospheric environment, is needed to sustain and is exposed to the sun and rain, is high damp and hot etc. severe
The test of environment.Therefore a kind of to have a high transmittance in 400-800nm, while have very much must for the exploitation of the antireflective coating of good weatherability
It wants.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of surface layers to have meso-hole structure with hole sealing structure internal layer
Antireflecting silicon dioxide film, the anti-reflection film have high transmittance, while good weatherability in 400~800nm range.
Anti-reflection film surface produced by the present invention is the SiO of hole-closing structure2Film can prevent hydrone from entering in hole, cut
Silica broken to the adsorption approach of hydrone, to efficiently solve porous SiO2Weatherability caused by the film moisture absorption is asked
Topic.
A kind of surface layer has the antireflecting silicon dioxide film of meso-hole structure with hole sealing structure internal layer, and the anti-reflection film is upper and lower
Double membrane structure, upper layer SiO2SiO in film2Nano particle densification arrangement, lower layer SiO2SiO in film2Nano particle arrangement shape
At multiple nano aperture structures, the aperture of described hole structure is 2~50nm.
Above-mentioned surface layer has the preparation method of the antireflecting silicon dioxide film of meso-hole structure with hole sealing structure internal layer, including such as
Lower operating procedure:
Step 1, Sol A is prepared: by ethyl orthosilicate, ethyl alcohol, deionized water, acid catalyst and polyoxyethylene polyoxypropylene
Ether block copolymers are mixed with certain molar ratio, obtained Sol A after aged；
Step 2, it prepares sol B: ethyl orthosilicate, ethyl alcohol, deionized water and acid catalyst is mixed with certain molar ratio
It closes, obtained sol B after aged；
Step 3, it will immerse by pretreated substrate in the Sol A of step 1, plated in substrate using dip-coating method
SiO2Film；Wherein, the rate of pulling is 50~200mm/min；
Step 4, SiO will be coated with2The substrate of film is put into the sol B of step 2, is plated in substrate using dip-coating method
SiO2Film is made annealing treatment after plated film, to obtain surface layer closing, the double layer antireflection coating that internal layer is meso-hole structure.
Wherein, in step 1 and step 2, the acid catalyst is one of hydrochloric acid, acetic acid or nitric acid.
Wherein, in step 1, ethyl orthosilicate, ethyl alcohol, deionized water, acid catalyst and polyoxyethylene poly-oxygen propylene aether are embedding
The molar ratio of section copolymer is 1: 20-60: 2-8: 0.01-0.1: 0.002-0.1.
Wherein, in step 2, ethyl orthosilicate, ethyl alcohol, deionized water and acid catalyst addition molar ratio be 1: 20-60:
2-8∶0.01-0.1。
Wherein, in step 3, the pretreatment of the substrate refers to substrate is put into washing lotion sufficiently washing after, then use respectively
Dehydrated alcohol and deionized water are sufficiently washed through ultrasonic wave, with being dried with nitrogen and drying after washing, are finally set the substrate of drying
It is spare in drier.
Wherein, in step 4, the rate of pulling of dip-coating method is 50~200mm/min.
Wherein, in step 4, annealing temperature is 400~700 DEG C, and annealing time is 60~120min.
Silicon dioxide film prepared by the present invention, surface are hole sealing structure silicon dioxide film, the mesoporous silica films of bottom
It for reticular structure, is tightly combined between silica condensation polymer in surface layer, thus fine and close two for keeping upper layer porosity very low
Silicon oxide film, since surface layer is hole-closing structure, hydrone be cannot be introduced into film hole, so that anti-reflection film has excellent environment
Stability and weatherability.
Compared with prior art, technical solution of the present invention has the beneficial effect that
Anti-reflection film prepared by the present invention mean transmissivity in 400-800nm spectral region is greater than 98%, than no plated film
Bare glass increase 5%-7% (K9 glass) (bare glass in 400-800nm spectral region mean transmissivity be 91%)；This
The color of invention film can be rendered as light blue, crocus, bluish violet, can effectively improve too according to the difference of film thickness
The sun light transmission rate of positive energy heat collector, photovoltaic module etc., capacity usage ratio are remarkably improved.
Antireflective coating steady damp heat environmental experiment (GB-T2423.3-2006) prepared by the present invention penetrates after 72 hours
Rate does not change.The broadband anti-reflection film can be used for a long time under the climatic environment of the complexity such as high temperature and humidity, and weather resistance is good.This
Invent the antireflective coating product of preparation, substrate of glass is without corroding pre-treatment, low manufacture cost, simple process, scratch-resistant, resistance to
The features such as time property is good is suitble to industrial production and application.
Detailed description of the invention
Fig. 1 is the transmission electron microscope picture of Sol A, and the silica in colloid is in mesopore network shape；
Fig. 2 is the transmission electron microscope picture of sol B, and silica chain combination obtains closely；
Fig. 3 is the scanning electron microscope (SEM) photograph after Sol A plated film, and silica chain is orderly aligned, is rendered as meso-hole structure；
Fig. 4 is duplicature surface scan electron microscope, and the sour glue film of surface covering combines fine and close；
Fig. 5 is the surface chart of duplicature produced by the present invention, is tightly combined between double-layer films, interface is unobvious；
Fig. 6 is the refractive index curve after Sol A plated film, refractive index 1.173；
Fig. 7 is the refractive index curve of closed pore duplicature, refractive index 1.222；
Fig. 8 is the transmittance curve of double-deck closed pore SiO2 antireflective coating and K9 substrate produced by the present invention, and anti-reflection film is can
Light-exposed region mean transmissivity reaches 98.97% or more.
Specific embodiment
Technical solution of the present invention is described further in the following with reference to the drawings and specific embodiments.
A kind of surface layer has the preparation method of the antireflecting silicon dioxide film of meso-hole structure with hole sealing structure internal layer, specific to wrap
Include following operating procedure:
Step 1, the ethyl orthosilicate by molar ratio for 1: 0.03: 0.04: 5: 41, polyoxyethylene polyoxypropylene block copolymerization
Object, concentrated hydrochloric acid, deionized water and dehydrated alcohol mixing, obtain mixed solution X, after mixed solution X is stirred 12 hours, in stabilizing ring
Seven days or so are stood under border, obtains the very big acid catalysis SiO of porosity2Sol A；The mass percentage concentration of Sol A is 3%；On
It states in reaction system, concentrated hydrochloric acid is catalyst, and ethyl orthosilicate is silicon source, and dehydrated alcohol is solvent, polyoxyethylene polyoxypropylene
For template；The mass percentage concentration of concentrated hydrochloric acid is 36.5%；
Step 2, ethyl orthosilicate, concentrated hydrochloric acid, deionized water and dehydrated alcohol that molar ratio is 1: 0.04: 4: 120 are mixed
It closes, obtains mixed solution Y and stand seven days or so after mixed solution Y is stirred 12 hours in stable environment, obtain porosity very
Small acid catalysis SiO2Sol B；The mass percentage concentration of sol B is 1%；In above-mentioned reaction system, concentrated hydrochloric acid is catalyst, just
Silester is silicon source, and dehydrated alcohol is solvent；
Step 3, in the environment of relative ambient humidity < 50%, the Sol A of step 1 will be immersed by pretreated substrate
In, the very big SiO of a layer porosity is first plated in substrate using lifting coating method2Film, pull rate 150mm/min；Lifting
After will be coated with SiO2The substrate of film stands 5min, then the sol B that will plate substrate with the membrane immersion step 2 under clean room environment
In, second layer SiO is plated using the pull rate of 100mm/min2Film；Finally, two layers of SiO will be coated with2The substrate of film is in Muffle
It is heat-treated 2 hours in furnace；The temperature of heat treatment is 700 DEG C.
Substrate is silicon wafer or tubulose, foliated glass substrate, and the pretreatment of substrate, which refers to for substrate to be put into washing lotion, sufficiently washes
It after washing, then is sufficiently washed with dehydrated alcohol and deionized water through ultrasonic wave respectively, with being dried with nitrogen after washing, is put into baking oven drying
Afterwards, it is placed in spare in drier.
After testing, the anti-reflection film that the method for the present invention obtains, mean transmissivity reaches in 400~800nm spectral region
98% or more.With 5 samples of preparation under embodiment.Sample average transmitance difference 0.1%.The anti-reflection film is in steady damp heat environment
After 72 hours, transmitance does not change lower experiment (GB-T2423.3-2006)；Pencil hardness is greater than 3H, and cross-hatching coating is attached
Put forth effort to test no any fall off (5B grades)；It is characterized using field emission scanning electron microscope (FESEM), it can be seen that film surface
Mesoporous pattern.The double-deck mesoporous anti-reflection film transmitance is high, hardness is big, adhesive force is strong.
The present invention is prepared for the weathering for having excellent using mesopore silicon dioxide nano material as raw material, using lifting coating method
The durable surface closed pore broadband anti-reflection film of performance and mechanical stability, using calcining after the second layer surface closed pore anti-reflection film deposition
(calcining is to form porous structure in order to which template is burnt up to reduce the refractive index of film, while calcining can allow to annealing
Film and substrate glasses combine even closer).The mesoporous anti-reflection film of single layer, highest transmitance is 97.90%, in visible light
Mean transmissivity in range is 95.93%, and due to surface porosity, pollutant and steam are easily entered in anti-reflection film
Portion, to seriously reduce the transmitance and environmental stability of anti-reflection film；The highest transmitance of single layer acid glue film is 94.28%,
Mean transmissivity is 93.40% within the scope of 400-800nm, and antireflective effect is very limited；Jie of surface-sealing prepared by the present invention
The highest transmitance of hole duplicature is 99.98%, and the transmitance within the scope of 400-800nm is 98.97%, and due to surface
It is hole sealing structure, substantially increases the ability that anti-reflection film resists pollutant and steam；Meanwhile sour glue film plays and reconciles monofilm folding
The effect for penetrating rate improves the broad-band transparence-increased effect of duplicature.
The present invention covers the gap of bottom mesopore surfaces using acid catalysis silica membrane, to prevent water point and pollution
Object penetrates into anti-reflection film, so that film be made to have inherent durability, and then improves the environmental reliability of film；Due to acid catalysis
SiO2The addition of colloidal sol (sol B), so that (internal layer) SiO2It is connected with each other, is obtained with toughness and bridging property between nano particle
Skeleton, so that anti-reflection film be made to show excellent mechanical strength；Finally, a small amount of acid catalyzed silicon dioxide gel (sol B)
It penetrates into the opening hole of meso-hole structure, the refractive index of adjustable anti-reflection film, significantly improves the whole transmitance of anti-reflection film.
The present invention can be by accurately controlling the thickness of mesoporous layer and compacted zone acid glue film, and the broad-band transparence-increased performance of film obtains
It significantly improves.Broadband anti-reflection film of the present invention can be used in solar energy acquisition and optical instrument field under harsh conditions.
Claims (8)
1. the antireflecting silicon dioxide film that a kind of surface layer has meso-hole structure with hole sealing structure internal layer, it is characterised in that: the increasing
Permeable membrane is Dual-layer membrane structure, upper layer SiO2SiO in film2Nano particle densification arrangement, lower layer SiO2SiO in film2Nanometer
Particle arranges to form multiple nano aperture structures, and the aperture of described hole structure is 2~50nm.
2. the system that a kind of surface layer described in claim 1 has the antireflecting silicon dioxide film of meso-hole structure with hole sealing structure internal layer
Preparation Method, which is characterized in that including following operating procedure:
Step 1, Sol A is prepared: ethyl orthosilicate, ethyl alcohol, deionized water, acid catalyst and polyoxyethylene poly-oxygen propylene aether is embedding
Section copolymer is mixed with certain molar ratio, obtained Sol A after aged；
Step 2, it prepares sol B: ethyl orthosilicate, ethyl alcohol, deionized water and acid catalyst being mixed with certain molar ratio, warp
Sol B is made after ageing；
Step 3, it will be immersed by pretreated substrate in the Sol A of step 1, SiO plated in substrate using dip-coating method2It is thin
Film；Wherein, the rate of pulling is 50~200mm/min；
Step 4, SiO will be coated with2The substrate of film is put into the sol B of step 2, and SiO is plated in substrate using dip-coating method2
Film is made annealing treatment after plated film, to obtain surface layer closing, the double layer antireflection coating that internal layer is meso-hole structure.
3. the system that surface layer according to claim 2 has the antireflecting silicon dioxide film of meso-hole structure with hole sealing structure internal layer
Preparation Method, it is characterised in that: in step 1 and step 2, the acid catalyst is one of hydrochloric acid, acetic acid or nitric acid.
4. the system that surface layer according to claim 2 has the antireflecting silicon dioxide film of meso-hole structure with hole sealing structure internal layer
Preparation Method, it is characterised in that: in step 1, ethyl orthosilicate, ethyl alcohol, deionized water, acid catalyst and polyoxyethylene polyoxypropylene
The molar ratio of ether block copolymers is 1: 20-60: 2-8: 0.01-0.1: 0.002-0.1.
5. the system that surface layer according to claim 2 has the antireflecting silicon dioxide film of meso-hole structure with hole sealing structure internal layer
Preparation Method, it is characterised in that: in step 2, ethyl orthosilicate, ethyl alcohol, deionized water and acid catalyst addition molar ratio be 1:
20-60∶2-8∶0.01-0.1。
6. the system that surface layer according to claim 2 has the antireflecting silicon dioxide film of meso-hole structure with hole sealing structure internal layer
Preparation Method, it is characterised in that: in step 3, the pretreatment of the substrate refers to substrate is put into washing lotion sufficiently washing after, then divide
It is not washed sufficiently with dehydrated alcohol and deionized water through ultrasonic wave, with being dried with nitrogen and drying after washing, finally by the base of drying
Bottom is placed in spare in drier.
7. the system that surface layer according to claim 2 has the antireflecting silicon dioxide film of meso-hole structure with hole sealing structure internal layer
Preparation Method, it is characterised in that: in step 4, the rate of pulling of dip-coating method is 50~200mm/min.
8. the system that surface layer according to claim 2 has the antireflecting silicon dioxide film of meso-hole structure with hole sealing structure internal layer
Preparation Method, it is characterised in that: in step 4, annealing temperature is 400~700 DEG C, and annealing time is 60~120min.
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Cited By (4)
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| CN110237814A (en) * | 2019-06-21 | 2019-09-17 | 一重集团大连工程建设有限公司 | A kind of preparation method for the active carbon handling marine oil spill |
| CN110975624A (en) * | 2019-12-31 | 2020-04-10 | 中建材蚌埠玻璃工业设计研究院有限公司 | Silicon dioxide closed porous membrane and preparation method thereof |
| CN111381297A (en) * | 2020-04-07 | 2020-07-07 | 宁波材料所杭州湾研究院 | High-anti-reflection antireflection film and preparation method thereof |
| CN111849349A (en) * | 2020-08-04 | 2020-10-30 | 吴江南玻玻璃有限公司 | Antireflection coating liquid, preparation method thereof, antireflection coated glass and photovoltaic module |
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| CN111849349A (en) * | 2020-08-04 | 2020-10-30 | 吴江南玻玻璃有限公司 | Antireflection coating liquid, preparation method thereof, antireflection coated glass and photovoltaic module |
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Application publication date: 20190315 |