CN106892576A - A kind of hollow array antireflective coating of multi-layer nano and preparation method thereof - Google Patents
A kind of hollow array antireflective coating of multi-layer nano and preparation method thereof Download PDFInfo
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- CN106892576A CN106892576A CN201510958545.8A CN201510958545A CN106892576A CN 106892576 A CN106892576 A CN 106892576A CN 201510958545 A CN201510958545 A CN 201510958545A CN 106892576 A CN106892576 A CN 106892576A
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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
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
- C03C17/3417—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials all coatings being oxide coatings
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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
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Abstract
The invention discloses hollow array antireflective coating of a kind of multi-layer nano and preparation method thereof.The inside of the antireflective coating is that the multilayer film with hole-closing structure for constituting alternately is superimposed by the fine and close nano-hollow ball individual layer silica of marshalling and titanium dioxide, and the number of plies is 2-30 layers, and outermost layer is the silica coating of fine and close closing.Its preparation method is comprised the following steps：With tetraethyl orthosilicate, deionized water, acid catalyst, absolute ethyl alcohol as raw material, Sol A is prepared, be added thereto to granules of polystyrene and obtain suspension C；With butyl titanate, deionized water, absolute ethyl alcohol, diethanol amine as raw material, sol B is prepared, be added thereto to granules of polystyrene and obtain suspension D；Glass after cleaning is carried out lifting plated film after annealing in suspension C, then coated glass is carried out lifting plated film after annealing in suspension D, repeat operation 1-25 times；Lifting after annealing is finally carried out in Sol A, surface-closed, the antireflective coating of internal nano-hollow array structure is obtained.
Description
Technical field
The present invention relates to hollow array antireflective coating of a kind of multi-layer nano and preparation method thereof, belong to collosol and gel
Method plated film and antireflective coating technical field.
Background technology
By abundant reacted glue be plated on matrix plurality of liquid material by collosol and gel film plating process, it
Advantage be that composition is uniform after multiple material hybrid reaction, can guarantee that the uniformity of film, can be by adjustment
The proportioning of raw material changes the performance of film.Collosol and gel film plating process can also adjust film thickness and
Refractive index, so as to change the transmitance of antireflective coating, is prepared using sol-gal process on the glass substrate at present
Antireflective coating can will transmit through rate lifting 2-7%, while use sol-gal process to lift antireflective coating film having
Have the advantages that low cost, it is two-sided while plated film, therefore be widely used in photovoltaic solar and light heat solar row
Industry.
At present the antireflective coating that uses substantially all in atmospheric environment, it is necessary to sustain expose to the sun and rain,
The test of the extreme natural environments such as high/low temperature, high humility.Therefore antireflective coating must have following features just may be used
Use：High transmittance, hardness are big, weather resistance is good.Antireflective prepared by the sol-gal process for using at present
Film transmitance is high, but particle surface can be accompanied by a large amount of polar hydroxyl groups, and internal pore structure is in perforate
State, film easily absorbs the hydrone and organic matter in humid air, and transmitance will be with time drop
Low, antireflective coating weatherability is poor, it is impossible to used in wet environment.The perforated membrane of hole-closing structure can be prevented
Hydrone enters in hole, has cut off adsorption approach of the silica to hydrone.Therefore can solve porous
The weather-proof sex chromosome mosaicism that the film moisture absorption causes.
During closed pore antireflective coating is prepared at present, the antireflective coating prepared is due to the original of thicknesses of layers
Cause, differ problem in the aperture for often causing hole accumulation to cause, and causes the unstable of transmitance.While closed pore
Antireflective coating is made up of hollow ball, the same moisture understood in absorption air in the space caused between ball and ball, is made
Into the attenuating of transmitance.
The content of the invention
Based on this, it is an object of the invention to provide a kind of hollow array antireflective coating of multi-layer nano, the anti-reflection
Film is penetrated for closed cell, porous films, nano-pore is consistent in array arrangement, aperture, and transmitance is high, good stability.
Preparation side another object of the present invention is to provide a kind of hollow array antireflective coating of multi-layer nano
Method, using the method prepare antireflective coating have hardness concurrently, film adhesion is big the characteristics of.
To achieve the above object, the present invention uses following technical scheme：
A kind of hollow array antireflective coating of multi-layer nano, the inside of the antireflective coating is fine and close by marshalling
Nano-hollow ball individual layer silica and the titanium dioxide multilayer film with hole-closing structure that alternately superposition is constituted,
The number of plies is 2-30 layers, and outermost layer is the silica coating of fine and close closing.
Preferably, the aperture of the hole-closing structure is 2-20nm.
A kind of preparation method of the hollow array antireflective coating of the multi-layer nano, comprises the following steps：
(1) with tetraethyl orthosilicate, deionized water, acid catalyst, absolute ethyl alcohol as raw material, Sol A is prepared；
(2) with butyl titanate, deionized water, absolute ethyl alcohol, diethanol amine as raw material, sol B is prepared
(3) by granules of polystyrene addition Sol A, mixing is stirred, obtains suspension C；
(4) by granules of polystyrene addition sol B, mixing is stirred, obtains suspension D；
(5) glass after cleaning is carried out lifting plated film after annealing in suspension C；
(6) coated glass after the completion of step (5) is carried out in suspension D lifting plated film after annealing；
(7) repeat step (5) and step (6) 1-15 times are continued cycling through；
(8) by repeatedly lifting annealing glass lifting after annealing is carried out in Sol A, obtain surface-closed,
The antireflective coating of internal nano-hollow array structure.
The hollow array antireflective coating of multi-layer nano obtained using the above method, its boring structure is come from
Step (3) and step (4) prepare the polystyrene nanoparticles in the suspension for being formed, silica list
The arrangement of layer nano-hollow array is formed by suspension C lifting annealing, titanium dioxide individual layer nano-hollow array by
Suspension D lifting annealing is formed, and the silica and titanium dioxide of individual layer are alternately constituted and arranges fine and close neat
Multi-layer nano hollow ball array structure, it is structurally characterized in that：Surface apertures are consistent, hole proper alignment, hole point
Cloth is homogeneous, is emerged from the test of later stage antireflective coating mean transmissivity, shows as transmitance change small
Advantage；And multi-layer nano hollow ball array structure makes hydrone cannot be introduced into being adsorbed in hole.Step
(8) purpose is to form one layer of compacted zone on surface, further keeps the closure of film layer.
In the above-mentioned methods, the acid catalyst is selected from the one kind in acetic acid, hydrochloric acid, nitric acid.The polyphenyl
The particle size of ethene particle is 2-20nm.
In step (1), between tetraethyl orthosilicate, deionized water, acid catalyst, absolute ethyl alcohol mole
Than being 1: (1-10): (0.01-0.1): (10-70), by tetraethyl orthosilicate, deionized water, acid catalyst, anhydrous second
Sol A is obtained after persistently stirring 1-24 hours after alcohol mixing.
In step (2), between butyl titanate, deionized water, absolute ethyl alcohol, diethanol amine mole
Than being 1: (1.5-3): (0.2-0.4): (500-750), by butyl titanate, deionized water, absolute ethyl alcohol, diethyl
Be aged after persistently being stirred 1-24 hour after hydramine mixing more than 2 hours to sol B.
In step (3) and step (4) between granules of polystyrene and tetraethyl orthosilicate, butyl titanate
Mol ratio be respectively 1-5: 1, respectively by particle diameter for 2-20nm polystyrene add Sol A and sol B
In, obtain suspension C and suspension D after persistently stirring 1-2 hours.
In step (5)-(8), the rate of pulling is 10-40cm/min, and annealing region is 250 DEG C -700
DEG C, the time is 5-60min.
The glass is plate glass or tubular glass.Its cleaning method is：First by deionized water and electricity
Sub- industrial cleaning agent cleans to glass surface without dirt glass surface；Secondly the glass that washing process is crossed is put
Enter in absolute ethyl alcohol and acetone, ultrasonic wave cleans each 30min.
The advantage of the invention is that：
The porous mode of production that the present invention is accumulated using individual layer, can form orderly, marshalling, aperture one
The multilayer film of cause, and dense film is added on the surface of multilayer film, hydrone can be further prevented in film layer
The diffusion in portion, plays the second layer effect of hydrone obstruction so that the antireflective coating of preparation has excellent resistance to
Hou Xing.Antireflective coating hardness of the invention is big, adhesive force strong, the effect with broadband anti-reflection film.The anti-reflection
Compact film of the outer surface rich in hydroxyl for penetrating film causes water contact angle to be less than 5 ° so that antireflective coating has super
Hydrophilic self-cleaning function, the solar energy optical-thermal photoelectricity under extraneous natural environment is exposed to for antireflective coating
Field is significant.
The glass of antireflective coating of the invention mean transmissivity in 250-2500nm spectral regions is coated with to be more than
96%, increased 3~5% than the bare glass without plated film.The color of prepared glass surface inteferometer coating according to
Film thickness difference can be light blue, light blue violet and pale purple coppery, can effectively improve solar thermal collector,
The sun light transmission rate such as photovoltaic module, Solar use efficiency can be significantly improved.
Specific embodiment
With reference to embodiment, the present invention will be further described, but embodiments of the present invention not limited to this.
Embodiment 1
Carried out during absolute ethyl alcohol and acetone will be put into after sheet or tubular glass wash clean first ultrasonically treated each
30min, the glass sample drying that will be cleaned up；
By 0.1mol tetraethyl orthosilicates, 0.8mol deionized waters, 0.005mol hydrochloric acid, 2.4mol absolute ethyl alcohols
Sol A is obtained after persistently being stirred 12 hours at normal temperatures after mixing；
By 0.4mol butyl titanates, 0.6mol deionized waters, 0.08mol absolute ethyl alcohols, 200mol diethyls
Ageing obtains sol B in 2 hours after persistently being stirred 24 hours after hydramine mixing；
After 2mol particle diameters are added in Sol A for the polystyrene of 5nm, it is stirred 2 hours, obtains
Suspension C；
After 2mol particle diameters are added in sol B for the polystyrene of 5nm, it is stirred 2 hours, obtains
Suspension D；
Glass after cleaning is lifted in suspension C, the rate of pulling is 8cm/min, lifting is completed
After be placed in the 30min that annealed at 500 DEG C in annealing furnace.
Glass after annealing is lifted in suspension D, the rate of pulling is 8cm/min, lifting is completed
After be placed in the 30min that annealed at 500 DEG C in annealing furnace.
Glass after the completion of annealing is continued to be alternately repeated lifting in C and D suspension and annealed, circulation altogether
Repeat to lift and anneal 5 times.
The coated glass of completion is lifted in Sol A, the rate of pulling is 5cm/min, lifting is completed
After be placed in annealing furnace at 500 DEG C anneal 1 hour.
By detection, mean transmissivity reaches in the antireflective coating 250-2500nm spectral regions that the present embodiment is obtained
To 96%.With 5 samples are prepared under embodiment, sample average transmitance phase difference is 0.1%.The antireflective
(place under film outside atmosphere environment：Beijing) annual aging experiment and 48 hours environmental experiments of steady damp heat
(GB-T2423.3-2006) after, transmitance is all unchanged；Pencil hardness is more than 3H, the attachment of cross-hatching film layer
Power test film layer comes off (5B grades) without any；Characterized using field emission scanning electron microscope (FESEM),
By film layer Cross Section Morphology it can be seen that closed pore aperture about 5nm.
Embodiment 2
Carried out during absolute ethyl alcohol and acetone will be put into after sheet or tubular glass wash clean first ultrasonically treated each
30min, the glass sample drying that will be cleaned up；
By 0.1mol tetraethyl orthosilicates, 0.2mol deionized waters, 0.005mol hydrochloric acid, 2.4mol absolute ethyl alcohols
Sol A is obtained after persistently being stirred 24 hours at normal temperatures after mixing；
By 0.4mol butyl titanates, 0.6mol deionized waters, 0.10mol absolute ethyl alcohols, 250mol diethyls
Ageing obtains sol B in 2 hours after persistently being stirred 24 hours after hydramine mixing；
After 0.5mol particle diameters are added in Sol A for the polystyrene of 5nm, it is stirred 2 hours, obtains
Suspension C；
After 2mol particle diameters are added in sol B for the polystyrene of 5nm, it is stirred 2 hours, obtains
Suspension D；
Glass after cleaning is lifted in suspension C, the rate of pulling is 9cm/min, lifting is completed
After be placed in the 30min that annealed at 500 DEG C in annealing furnace.
Glass after annealing is lifted in suspension D, the rate of pulling is 9cm/min, lifting is completed
After be placed in the 30min that annealed at 500 DEG C in annealing furnace.
Glass after the completion of annealing is continued to be alternately repeated lifting in C and D suspension and annealed, circulation altogether
Repeat to lift and anneal 5 times.
The coated glass of completion is lifted in Sol A, the rate of pulling is 5cm/min, lifting is completed
After be placed in annealing furnace at 500 DEG C anneal 1 hour.
By detection, mean transmissivity reaches in the antireflective coating 250-2500nm spectral regions that the present embodiment is obtained
To 96%.With 5 samples are prepared under embodiment, sample average transmitance phase difference is 0.1%.The antireflective
(place under film outside atmosphere environment：Beijing) annual aging experiment and 48 hours environmental experiments of steady damp heat
(GB-T2423.3-2006) after, transmitance is all unchanged；Pencil hardness is more than 3H, the attachment of cross-hatching film layer
Power test film layer comes off (5B grades) without any；Characterized using field emission scanning electron microscope (FESEM),
By film layer Cross Section Morphology it can be seen that closed pore aperture about 5nm.
Embodiment 3
Carried out during absolute ethyl alcohol and acetone will be put into after sheet or tubular glass wash clean first ultrasonically treated each
30min, the glass sample drying that will be cleaned up；
By 0.1mol tetraethyl orthosilicates, 0.2mol deionized waters, 0.005mol hydrochloric acid, 2.4mol absolute ethyl alcohols
Sol A is obtained after persistently being stirred 24 hours at normal temperatures after mixing；
By 0.4mol butyl titanates, 0.6mol deionized waters, 0.08mol absolute ethyl alcohols, 200mol diethyls
Ageing obtains sol B in 2 hours after persistently being stirred 24 hours after hydramine mixing；
After 0.5mol particle diameters are added in Sol A for the polystyrene of 5nm, it is stirred 2 hours, obtains
Suspension C；
After 2mol particle diameters are added in sol B for the polystyrene of 5nm, it is stirred 2 hours, obtains
Suspension D；
Glass after cleaning is lifted in suspension C, the rate of pulling is 8cm/min, lifting is completed
After be placed in the 30min that annealed at 600 DEG C in annealing furnace.
Glass after annealing is lifted in suspension D, the rate of pulling is 8cm/min, lifting is completed
After be placed in the 30min that annealed at 600 DEG C in annealing furnace.
Glass after the completion of annealing is continued to be alternately repeated lifting in C and D suspension and annealed, circulation altogether
Repeat to lift and anneal 10 times.
The coated glass of completion is lifted in Sol A, the rate of pulling is 5cm/min, lifting is completed
After be placed in annealing furnace at 600 DEG C anneal 1 hour.
By detection, mean transmissivity reaches in the antireflective coating 250-2500nm spectral regions that the present embodiment is obtained
To 96%.With 5 samples are prepared under embodiment, sample average transmitance phase difference is 0.1%.The antireflective
(place under film outside atmosphere environment：Beijing) annual aging experiment and 48 hours environmental experiments of steady damp heat
(GB-T2423.3-2006) after, transmitance is all unchanged；Pencil hardness is more than 3H, the attachment of cross-hatching film layer
Power test film layer comes off (5B grades) without any；Characterized using field emission scanning electron microscope (FESEM),
By film layer Cross Section Morphology it can be seen that closed pore aperture about 5nm.
Embodiment 4
Carried out during absolute ethyl alcohol and acetone will be put into after sheet or tubular glass wash clean first ultrasonically treated each
30min, the glass sample drying that will be cleaned up；
By 0.1mol tetraethyl orthosilicates, 0.2mol deionized waters, 0.005mol hydrochloric acid, 2.4mol absolute ethyl alcohols
Sol A is obtained after persistently being stirred 24 hours at normal temperatures after mixing；
By 0.4mol butyl titanates, 0.6mol deionized waters, 0.08mol absolute ethyl alcohols, 200mol diethyls
Ageing obtains sol B in 2 hours after persistently being stirred 24 hours after hydramine mixing；
After 0.5mol particle diameters are added in Sol A for the polystyrene of 10nm, it is stirred 2 hours, obtains
To suspension C；
After 4mol particle diameters are added in sol B for the polystyrene of 10nm, it is stirred 2 hours, obtains
Suspension D；
Glass after cleaning is lifted in suspension C, the rate of pulling is 8cm/min, lifting is completed
After be placed in the 30min that annealed at 500 DEG C in annealing furnace.
Glass after annealing is lifted in suspension D, the rate of pulling is 8cm/min, lifting is completed
After be placed in the 30min that annealed at 500 DEG C in annealing furnace.
Glass after the completion of annealing is continued to be alternately repeated lifting in C and D suspension and annealed, circulation altogether
Repeat to lift and anneal 5 times.
The coated glass of completion is lifted in Sol A, the rate of pulling is 5cm/min, lifting is completed
After be placed in annealing furnace at 500 DEG C anneal 1 hour.
By detection, mean transmissivity reaches in the antireflective coating 250-2500nm spectral regions that the present embodiment is obtained
To 96%.With 5 samples are prepared under embodiment, sample average transmitance phase difference is 0.1%.The antireflective
(place under film outside atmosphere environment：Beijing) annual aging experiment and 48 hours environmental experiments of steady damp heat
(GB-T2423.3-2006) after, transmitance is all unchanged；Pencil hardness is more than 3H, the attachment of cross-hatching film layer
Power test film layer comes off (5B grades) without any；Characterized using field emission scanning electron microscope (FESEM),
By film layer Cross Section Morphology it can be seen that closed pore aperture about 10nm.
Embodiment 5
Carried out during absolute ethyl alcohol and acetone will be put into after sheet or tubular glass wash clean first ultrasonically treated each
30min, the glass sample drying that will be cleaned up；
By 0.1mol tetraethyl orthosilicates, 0.2mol deionized waters, 0.005mol hydrochloric acid, 2.4mol absolute ethyl alcohols
Sol A is obtained after persistently being stirred 24 hours at normal temperatures after mixing；
By 0.3mol butyl titanates, 0.5mol deionized waters, 0.08mol absolute ethyl alcohols, 200mol diethyls
Ageing obtains sol B in 2 hours after persistently being stirred 24 hours after hydramine mixing；
After 0.5mol particle diameters are added in Sol A for the polystyrene of 5nm, it is stirred 2 hours, obtains
Suspension C；
After 2mol particle diameters are added in sol B for the polystyrene of 5nm, it is stirred 2 hours, obtains
Suspension D；
Glass after cleaning is lifted in suspension C, the rate of pulling is 8cm/min, lifting is completed
After be placed in the 45min that annealed at 500 DEG C in annealing furnace.
Glass after annealing is lifted in suspension D, the rate of pulling is 8cm/min, lifting is completed
After be placed in the 45min that annealed at 500 DEG C in annealing furnace.
Glass after the completion of annealing is continued to be alternately repeated lifting in C and D suspension and annealed, circulation altogether
Repeat to lift and anneal 5 times.
The coated glass of completion is lifted in Sol A, the rate of pulling is 7cm/min, lifting is completed
After be placed in annealing furnace at 500 DEG C anneal 30 hours.
By detection, mean transmissivity reaches in the antireflective coating 250-2500nm spectral regions that the present embodiment is obtained
To 96%.With 5 samples are prepared under embodiment, sample average transmitance phase difference is 0.1%.The antireflective
(place under film outside atmosphere environment：Beijing) annual aging experiment and 48 hours environmental experiments of steady damp heat
(GB-T2423.3-2006) after, transmitance is all unchanged；Pencil hardness is more than 3H, the attachment of cross-hatching film layer
Power test film layer comes off (5B grades) without any；Characterized using field emission scanning electron microscope (FESEM),
By film layer Cross Section Morphology it can be seen that closed pore aperture about 5nm.
Embodiment 6
Carried out during absolute ethyl alcohol and acetone will be put into after sheet or tubular glass wash clean first ultrasonically treated each
30min, the glass sample drying that will be cleaned up；
By 0.1mol tetraethyl orthosilicates, 0.2mol deionized waters, 0.005mol hydrochloric acid, 2.4mol absolute ethyl alcohols
Mixing obtains Sol A after persistently stirring 12 hours；
By 0.4mol butyl titanates, 0.6mol deionized waters, 0.08mol absolute ethyl alcohols, 200mol diethyls
Ageing obtains sol B in 1 hour after persistently being stirred 12 hours after hydramine mixing；
After 0.2mol particle diameters are added in Sol A for the polystyrene of 5nm, it is stirred 2 hours, obtains
Suspension C；
After 2mol particle diameters are added in sol B for the polystyrene of 5nm, it is stirred 2 hours, obtains
Suspension D；
Glass after cleaning is lifted in suspension C, the rate of pulling is 6cm/min, lifting is completed
After be placed in the 30min that annealed at 500 DEG C in annealing furnace.
Glass after annealing is lifted in suspension D, the rate of pulling is 6cm/min, lifting is completed
After be placed in the 30min that annealed at 500 DEG C in annealing furnace.
Glass after the completion of annealing is continued to be alternately repeated lifting in C and D suspension and annealed, circulation altogether
Repeat to lift and anneal 5 times.
The coated glass of completion is lifted in Sol A, the rate of pulling is 10cm/min, lifting is completed
After be placed in annealing furnace at 500 DEG C anneal 1 hour.
By detection, mean transmissivity reaches in the antireflective coating 250-2500nm spectral regions that the present embodiment is obtained
To 96%.With 5 samples are prepared under embodiment, sample average transmitance phase difference is 0.1%.The antireflective
(place under film outside atmosphere environment：Beijing) annual aging experiment and 48 hours environmental experiments of steady damp heat
(GB-T2423.3-2006) after, transmitance is all unchanged；Pencil hardness is more than 3H, the attachment of cross-hatching film layer
Power test film layer comes off (5B grades) without any；Characterized using field emission scanning electron microscope (FESEM),
By film layer Cross Section Morphology it can be seen that closed pore aperture about 5nm.
Claims (10)
1. the hollow array antireflective coating of a kind of multi-layer nano, it is characterised in that：The inside of the antireflective coating is that the multilayer film with hole-closing structure for constituting alternately is superimposed by the fine and close nano-hollow ball individual layer silica of marshalling and titanium dioxide, and the number of plies is 2-30 layers, and outermost layer is the silica coating of fine and close closing.
2. the hollow array antireflective coating of multi-layer nano according to claim 1, it is characterised in that：The aperture of the hole-closing structure is 2-20nm.
3. a kind of preparation method of the hollow array antireflective coating of multi-layer nano described in claim 1 or 2, it is characterised in that：Comprise the following steps：
(1) with tetraethyl orthosilicate, deionized water, acid catalyst, absolute ethyl alcohol as raw material, Sol A is prepared；
(2) with butyl titanate, deionized water, absolute ethyl alcohol, diethanol amine as raw material, sol B is prepared
(3) by granules of polystyrene addition Sol A, mixing is stirred, obtains suspension C；
(4) by granules of polystyrene addition sol B, mixing is stirred, obtains suspension D；
(5) glass after cleaning is carried out lifting plated film after annealing in suspension C；
(6) coated glass after the completion of step (5) is carried out in suspension D lifting plated film after annealing；
(7) repeat step (5) and step (6) 1-15 times are continued cycling through；
(8) glass by repeatedly lifting annealing carries out lifting after annealing in Sol A, obtains surface-closed, the antireflective coating of internal nano-hollow array structure.
4. preparation method according to claim 3, it is characterised in that：The acid catalyst is selected from the one kind in acetic acid, hydrochloric acid, nitric acid.
5. preparation method according to claim 3, it is characterised in that：Mol ratio in step (1) between tetraethyl orthosilicate, deionized water, acid catalyst, absolute ethyl alcohol is 1: (1-10): (0.01-0.1): (10-70).
6. preparation method according to claim 3, it is characterised in that：Mol ratio in step (2) between butyl titanate, deionized water, absolute ethyl alcohol, diethanol amine is 1: (1.5-3): (0.2-0.4): (500-750).
7. preparation method according to claim 3, it is characterised in that：Mol ratio in step (3) and step (4) between granules of polystyrene and tetraethyl orthosilicate, butyl titanate is respectively 1-5: 1.
8. preparation method according to claim 3, it is characterised in that：The rate of pulling is 10-40cm/min.
9. preparation method according to claim 3, it is characterised in that：Annealing region is 250 DEG C -700 DEG C, and the time is 5-60min.
10. preparation method according to claim 3, it is characterised in that：The glass is plate glass or tubular glass.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109467317A (en) * | 2019-01-04 | 2019-03-15 | 中国工程物理研究院激光聚变研究中心 | 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 |
| CN110109200A (en) * | 2019-04-04 | 2019-08-09 | 深圳市华星光电技术有限公司 | A kind of display panel and preparation method thereof |
| CN110982325A (en) * | 2019-12-31 | 2020-04-10 | 上海特栎材料科技有限公司 | Antireflection, antistatic and super-hydrophilic coating composition, coating and product |
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| CN101786801A (en) * | 2009-01-22 | 2010-07-28 | 中国科学院理化技术研究所 | Super-hydrophilic anti-fog anti-reflection coating and preparation method and application thereof |
| CN101786803A (en) * | 2010-03-02 | 2010-07-28 | 常州龙腾太阳能热电设备有限公司 | Method for coating multiple compound high anti-reflection films on inner surface and outer surface of glass tube with length/aperture ratio greater than 30 |
| CN103288358A (en) * | 2012-02-22 | 2013-09-11 | 中国科学院理化技术研究所 | Super-hydrophilic self-cleaning antifogging antireflection coating and preparation method thereof |
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| CN101786801A (en) * | 2009-01-22 | 2010-07-28 | 中国科学院理化技术研究所 | Super-hydrophilic anti-fog anti-reflection coating and preparation method and application thereof |
| CN101786803A (en) * | 2010-03-02 | 2010-07-28 | 常州龙腾太阳能热电设备有限公司 | Method for coating multiple compound high anti-reflection films on inner surface and outer surface of glass tube with length/aperture ratio greater than 30 |
| CN103288358A (en) * | 2012-02-22 | 2013-09-11 | 中国科学院理化技术研究所 | Super-hydrophilic self-cleaning antifogging antireflection coating and preparation method thereof |
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| CN109467317A (en) * | 2019-01-04 | 2019-03-15 | 中国工程物理研究院激光聚变研究中心 | 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 |
| CN110109200A (en) * | 2019-04-04 | 2019-08-09 | 深圳市华星光电技术有限公司 | A kind of display panel and preparation method thereof |
| CN110982325A (en) * | 2019-12-31 | 2020-04-10 | 上海特栎材料科技有限公司 | Antireflection, antistatic and super-hydrophilic coating composition, coating and product |
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