CN105826404B - A kind of preparation method of the doped poly silicon oxygen alkane colloidal sol antireflective coating based on modifying interface - Google Patents
A kind of preparation method of the doped poly silicon oxygen alkane colloidal sol antireflective coating based on modifying interface Download PDFInfo
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- CN105826404B CN105826404B CN201610178576.6A CN201610178576A CN105826404B CN 105826404 B CN105826404 B CN 105826404B CN 201610178576 A CN201610178576 A CN 201610178576A CN 105826404 B CN105826404 B CN 105826404B
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- 239000006117 anti-reflective coating Substances 0.000 title claims abstract description 67
- -1 silicon oxygen alkane Chemical class 0.000 title claims abstract description 26
- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 22
- 229920005591 polysilicon Polymers 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000758 substrate Substances 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000008367 deionised water Substances 0.000 claims abstract description 24
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 24
- 239000002904 solvent Substances 0.000 claims abstract description 17
- 239000002346 layers by function Substances 0.000 claims abstract description 9
- 229910052681 coesite Inorganic materials 0.000 claims description 35
- 229910052906 cristobalite Inorganic materials 0.000 claims description 35
- 239000000377 silicon dioxide Substances 0.000 claims description 35
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 35
- 229910052682 stishovite Inorganic materials 0.000 claims description 35
- 229910052905 tridymite Inorganic materials 0.000 claims description 35
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 18
- NASVITFAUKYCPM-UHFFFAOYSA-N ethanol;tetraethyl silicate Chemical compound CCO.CCO[Si](OCC)(OCC)OCC NASVITFAUKYCPM-UHFFFAOYSA-N 0.000 claims description 14
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 12
- 238000013019 agitation Methods 0.000 claims description 12
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000005286 illumination Methods 0.000 claims description 11
- 238000005516 engineering process Methods 0.000 claims description 10
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical class CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 8
- 238000000576 coating method Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 2
- 230000007062 hydrolysis Effects 0.000 claims description 2
- 238000006460 hydrolysis reaction Methods 0.000 claims description 2
- 229910000077 silane Inorganic materials 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 8
- 239000002356 single layer Substances 0.000 abstract description 6
- 230000003667 anti-reflective effect Effects 0.000 abstract description 5
- 230000021715 photosynthesis, light harvesting Effects 0.000 abstract description 3
- 239000011521 glass Substances 0.000 description 38
- 239000000243 solution Substances 0.000 description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 238000002834 transmittance Methods 0.000 description 9
- 239000010410 layer Substances 0.000 description 8
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000007654 immersion Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 238000002203 pretreatment Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000004879 molecular function Effects 0.000 description 2
- 230000036755 cellular response Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000013082 photovoltaic technology Methods 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0216—Coatings
- H01L31/02161—Coatings for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/02167—Coatings for devices characterised by at least one potential jump barrier or surface barrier for solar cells
- H01L31/02168—Coatings for devices characterised by at least one potential jump barrier or surface barrier for solar cells the coatings being antireflective or having enhancing optical properties for the solar cells
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- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Engineering & Computer Science (AREA)
- Electromagnetism (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Sustainable Energy (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Surface Treatment Of Optical Elements (AREA)
- Paints Or Removers (AREA)
- Laminated Bodies (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
The invention discloses a kind of preparation method of the doped poly silicon oxygen alkane colloidal sol antireflective coating based on modifying interface, after substrate surface grows antireflective coating, the antireflective coating is pre-processed, ensure to form oh group on antireflective coating, then immerse the substrate that growth has antireflective coating in the solution containing sulfydryl, by way of molecular self-assembling, the unimolecule functional layer containing sulfydryl is formed in antireflective coating, deionized water rinsing is finally used, removes the solvent of residual, is dried up.The present invention is to introduce unimolecule functional layer on antireflective coating surface, the strand of unimolecule functional layer material is shorter, with certain rigidity, when monolayer is uniformly covered on the surface of material, vibration and energy dissipation can be closed, and intermolecular model ylid bloom action power is smaller, order and bulk density are low, and then the case hardness of antireflective coating can be effectively improved, and the transmissivity of antireflective coating is improved, there is obvious antireflective effect.
Description
【Technical field】
The invention belongs to field of photovoltaic technology, is related to a kind of nanometer antireflective coating, more particularly to a kind of nanometer antireflective coating
Modifying interface method, the present invention.
【Background technology】
In area of solar cell, the light transmission rate by improving substrate of glass can effectively lift turning for solar cell
Efficiency is changed, is always the focus and difficult point of industry research.The coated with antireflection film in the substrate of glass of solar cell, can maximum limit
Degree ground reduces reflectivity, increases transmitance.Developing has the solar energy of high transmittance in solar cell response spectral range
Photovoltaic nanometer antireflective coating glass, can equal extent raising conversion efficiency of solar cell, reduce cost of electricity-generating, lifting too
The market competitiveness of positive energy cell power generation, shortens the period of cost recovery to generate electricity by way of merging two or more grid systems, has extraordinary economic prospect.
Photovoltaic is mainly used in the cover plate materials of photovoltaic cell with antireflective coating, is typically mounted under outdoor environment,
Sometimes can also in areas such as the more extreme desert of weather, wastelands, therefore it is required that product will not only have high transmitance, but also
It is required that film layer will withstand hot and humid condition and have the mechanical performance such as good hardness and damage resistant abrasion-resistant ability.So
And in existing product, antireflective coating case hardness is not high enough, damage resistant abrasion-resistant ability, easily draws in use
Wound, so as to influence the performance of product and life-span.
Based on this, patent of the present invention provides a kind of hardness height based on modifying interface, damage resistant ability by force and transmitance
The preparation method of high antireflective coating.
【The content of the invention】
The present invention provides a kind of method that doped poly silicon oxygen alkane colloidal sol based on modifying interface prepares antireflective coating, by dividing
Sub- self assembly introduces unimolecule functional layer, can be effectively improved the case hardness of antireflective coating and have obvious antireflective effect, enter
And obtain hardness height, the antireflective coating that damage resistant ability is strong and transmitance is high.
The present invention uses following technical scheme：
A kind of preparation method of the doped poly silicon oxygen alkane colloidal sol antireflective coating based on modifying interface, subtract in substrate surface growth
After reflectance coating, the antireflective coating is pre-processed, ensures to form oh group on antireflective coating, growth is then had into antireflective
The substrate of film is immersed in the solution containing sulfydryl, and by way of molecular self-assembling, single point containing sulfydryl is formed in antireflective coating
Subfunction layer, finally with deionized water rinsing, the solvent of residual is removed, is dried up.
Preferably, described pretreatment refers to ultra violet lamp, wherein, intensity of illumination 100-200mw/cm2。
Preferably, the solution containing sulfydryl refers to super dry toluene solution or chlorobenzene solution and 3- mercapto propyl trimethoxies
The mixed liquor that silane is formed.
Preferably, the volume ratio of described 3- mercaptopropyl trimethoxysilanes and super dry toluene solution or chlorobenzene solution is
0.5~3%.
Preferably, described substrate is immersed in the solution containing sulfydryl, and soak time is 0.5~1h.
Preferably, described antireflective coating is grown in substrate surface using coating technique is lifted, and its concrete technology is：Prepare
SiO2Colloidal sol, after substrate is cleaned, it is immersed in SiO2In colloidal sol, lifted after soaking 30~60s, the speed for lifting plated film is
120-190mm/min, finally it is sintered.
Preferably, before lifting plated film, by alkaline SiO2Colloidal sol is modified using polysiloxane-modified technology, wherein,
Doped poly silicon oxygen alkane and SiO2The volume ratio of colloidal sol is 2%-16%.
Preferably, it is sintered at 480-520 DEG C and sinters 20-40min.
Preferably, described SiO2The preparation method of colloidal sol is：Magnetic agitation tetraethyl orthosilicate ethanol solution, then
The solution of absolute ethyl alcohol, deionized water and ammoniacal liquor is added dropwise in tetraethyl orthosilicate ethanol solution, continues magnetic force and stirs
Mix to uniformly after, sealing be aged at ambient temperature.
Preferably, tetraethyl orthosilicate：Absolute ethyl alcohol：Deionized water：The mol ratio of ammoniacal liquor is 1:(20-80):(1-10):
0.1。
Compared with prior art, the present invention at least has the advantages that：The present invention grows antireflective in substrate surface
After film, the antireflective coating is pre-processed, ensures to form oh group on antireflective coating, growth is then had into antireflective coating
Substrate is immersed in the solution containing sulfydryl, and by way of molecular self-assembling, the unimolecule work(containing sulfydryl is formed in antireflective coating
Ergosphere, finally with deionized water rinsing, the solvent of residual is removed, is dried up.The present invention is to introduce unimolecule on antireflective coating surface
Functional layer, the strand of unimolecule functional layer material is shorter, has certain rigidity, when monolayer is uniformly covered on material
Surface when, vibration and energy dissipation can be closed, and intermolecular model ylid bloom action power is smaller, and order and bulk density are low,
And then the case hardness of antireflective coating can be effectively improved, and the transmissivity of antireflective coating is improved, there is obvious anti-reflection effect
Fruit.
【Brief description of the drawings】
In order that present disclosure is more likely to be clearly understood, specific embodiment and combination below according to the present invention
Accompanying drawing, the present invention is further detailed explanation, wherein
Fig. 1 be add volume ratio 0% 3- mercaptopropyl trimethoxysilanes wavelength-transmittance graph；
Fig. 2 be add volume ratio 0.5% 3- mercaptopropyl trimethoxysilanes wavelength-transmittance graph；
Fig. 3 be add volume ratio 1.5% 3- mercaptopropyl trimethoxysilanes wavelength-transmittance graph；
Fig. 4 be add volume ratio 3% 3- mercaptopropyl trimethoxysilanes wavelength-transmittance graph.
【Embodiment】
A kind of method that doped poly silicon oxygen alkane colloidal sol based on modifying interface prepares antireflective coating, including step：
(1) SiO is configured2Colloidal sol：Using tetraethyl orthosilicate, absolute ethyl alcohol, deionized water and ammoniacal liquor as raw material, alkalescence is prepared
SiO2Colloidal sol, wherein tetraethyl orthosilicate：Absolute ethyl alcohol：Deionized water：The mol ratio of ammoniacal liquor is 1:(20-80):(1-10):0.1.
Prepare alkaline SiO2The method of colloidal sol is：After magnetic agitation tetraethyl orthosilicate ethanol solution 3-10min, by anhydrous second
The solution of alcohol, deionized water and ammoniacal liquor is added dropwise in tetraethyl orthosilicate ethanol solution, continues magnetic agitation to uniform
Afterwards, sealing is aged 5d at ambient temperature.
(2)SiO2Sol-gel modified processing：By alkaline SiO2Colloidal sol is modified using polysiloxane-modified technology, is plated
Film liquid.Wherein doped poly silicon oxygen alkane and SiO2The volume ratio of colloidal sol can be adjusted between 2%-16%.
(3) glass substrate is cleaned, the glass substrate after cleaning is immersed in colloidal sol, carried after soak time 30-60s
Draw, lifting coating speed 120-190mm/min.
(4) glass substrate after lifting plated film is put into drying box, is toasted under the conditions of 180-220 DEG C and dry 5-
15min；It is put into Muffle furnace and is sintered after drying, 20-40min is sintered at 480-520 DEG C, forms antireflective coating.
(5) antireflective coating glass substrate is placed under uviol lamp, carries out UV illumination pretreatments, wherein intensity of illumination is 100-
200mw/cm2, light application time 30-60s；Can be in formation hydroxyl base on antireflective coating glass substrate after UV illumination pretreatments
Group (- OH).The compound of structure shown in a kind of structural formula (I) is added in the super dry toluene solution of solvent or chlorobenzene solution
C6H16O3SSi (3- mercaptopropyl trimethoxysilanes), the compound and the volume ratio of super dry solvent benzole soln are 0.5%-
3%, it is sufficiently mixed.After UV illumination pretreatments, antireflective coating glass substrate is immersed in above-mentioned mixed solution, soak time is
30 minutes to 1 hour, form unimolecule functional layer.
Hydroxyl is formed after UV illumination pretreatments, described hydroxyl is with the trimethoxy silane containing sulfydryl in super dry first
Hydrolysis occurs in benzene solvent or chlorobenzene solvent, and then on antireflective coating surface by way of molecular self-assembling, formation contains
The unimolecule functional layer of sulfydryl, and then the case hardness of antireflective coating is improved, and there is obvious antireflective effect, it is related single point
Subfunction layer formation mechenism is as follows.
Carry out modifying interface of the molecular self-assembling material that the present invention is claimed to antireflective coating surface, is in antireflective coating
Surface introduces monolayer, and the strand of monolayer material is shorter, has certain rigidity, when monolayer uniformly covers
On the surface of material, vibration and energy dissipation can be closed, and intermolecular model ylid bloom action power is smaller, order and bulk density
It is low, and then the case hardness of antireflective coating can be effectively improved, and the transmissivity of antireflective coating is improved, have obvious anti-reflection
Effect.
The volume ratio of 3- mercaptopropyl trimethoxysilanes and super dry toluene solvant is limited between 0.5%-3%, works as volume
Than it is too low be less than 0.5% when, 3- mercaptopropyl trimethoxysilanes compound is because concentration is too low can not form monolayer；Work as body
Product than it is too high be more than 3% when, what 3- mercaptopropyl trimethoxysilanes compound was formed by excessive concentration is polymolecular layer.
(6) by the anti reflection glass film deionized water rinsing after immersion, other solvents remained are removed；Blown with nitrogen
It is dry.
Embodiment：
Embodiment 1
(1) SiO is configured2Colloidal sol：Using tetraethyl orthosilicate, absolute ethyl alcohol, deionized water and ammoniacal liquor as raw material, alkalescence is prepared
SiO2Colloidal sol, wherein tetraethyl orthosilicate：Absolute ethyl alcohol：Deionized water：The mol ratio of ammoniacal liquor is 1:45:3:0.1.Prepare alkalescence
SiO2The method of colloidal sol is：After magnetic agitation tetraethyl orthosilicate ethanol solution 3-10min, by absolute ethyl alcohol, go from
The solution of sub- water and ammoniacal liquor is added dropwise in tetraethyl orthosilicate ethanol solution, after continuing magnetic agitation 2h, is sealed in room
5d is aged under the conditions of temperature.
(2)SiO2Sol-gel modified processing：By alkaline SiO2Colloidal sol is modified using polysiloxane-modified technology, is plated
Film liquid.Wherein doped poly silicon oxygen alkane and SiO2The volume ratio of colloidal sol is 8%.
(3) glass substrate is cleaned, the glass substrate after cleaning is immersed in colloidal sol, lifted after soak time 30s,
Lift coating speed 190mm/min.
(4) glass substrate after lifting plated film is put into drying box, is toasted under the conditions of 180 DEG C and dry 10min；It is dry
It is put into Muffle furnace and is sintered after dry, 30min is sintered at 500 DEG C, forms antireflective coating.
(5) antireflective coating glass substrate is placed under uviol lamp, carries out UV illumination, time 30s；, will after photo-irradiation treatment
Sample is put into the C that volume ratio is 0%6H16O3SSi in super dry solvent toluene mixture with soaking, time 30min, forms single point
Subfunction layer；
(6) by the anti reflection glass film deionized water rinsing after immersion, other solvents remained are removed；Blown with nitrogen
It is dry.
As a result show, anti reflection glass film hardness manufactured in the present embodiment is 3H, on a glass substrate, sample peak transmission
Rate reaches 89.36%, and wavelength-transmittance graph is as shown in Figure 1.
Embodiment 2
(1) SiO is configured2Colloidal sol：Using tetraethyl orthosilicate, absolute ethyl alcohol, deionized water and ammoniacal liquor as raw material, alkalescence is prepared
SiO2Colloidal sol, wherein tetraethyl orthosilicate：Absolute ethyl alcohol：Deionized water：The mol ratio of ammoniacal liquor is 1:60:8:0.1.Prepare alkalescence
SiO2The method of colloidal sol is：After magnetic agitation tetraethyl orthosilicate ethanol solution 3-10min, by absolute ethyl alcohol, go from
The solution of sub- water and ammoniacal liquor is added dropwise in tetraethyl orthosilicate ethanol solution, continue magnetic agitation to uniformly after, sealing
5d is aged at ambient temperature.
(2)SiO2Sol-gel modified processing：By alkaline SiO2Colloidal sol is modified using polysiloxane-modified technology, is plated
Film liquid.Wherein doped poly silicon oxygen alkane and SiO2The volume ratio of colloidal sol is 12%.
(3) glass substrate is cleaned, the glass substrate after cleaning is immersed in colloidal sol, lifted after soak time 60s,
Lift coating speed 150mm/min.
(4) glass substrate after lifting plated film is put into drying box, is toasted under the conditions of 200 DEG C and dry 10min；It is dry
It is put into Muffle furnace and is sintered after dry, 40min is sintered at 520 DEG C, forms antireflective coating.
(5) antireflective coating glass substrate is placed under uviol lamp, carries out UV illumination, time 50s；, will after photo-irradiation treatment
Sample is put into the C that volume ratio is 0.5%6H16O3SSi in super dry solvent toluene mixture with soaking, time 30min, is formed single
Molecular function layer；
(6) by the anti reflection glass film deionized water rinsing after immersion, other solvents remained are removed；Blown with nitrogen
It is dry.
As a result showing, anti reflection glass film hardness manufactured in the present embodiment can reach 5H, on a glass substrate, sample peak value
Transmissivity reaches 93.06%, has significant broad-band transparence-increased effect, wavelength-transmittance graph is as shown in Figure 2.
Embodiment 3
(1) SiO is configured2Colloidal sol：Using tetraethyl orthosilicate, absolute ethyl alcohol, deionized water and ammoniacal liquor as raw material, alkalescence is prepared
SiO2Colloidal sol, wherein tetraethyl orthosilicate：Absolute ethyl alcohol：Deionized water：The mol ratio of ammoniacal liquor is 1:80:1:0.1.Prepare alkalescence
SiO2The method of colloidal sol is：After magnetic agitation tetraethyl orthosilicate ethanol solution 3-10min, by absolute ethyl alcohol, go from
The solution of sub- water and ammoniacal liquor is added dropwise in tetraethyl orthosilicate ethanol solution, continue magnetic agitation to uniformly after, sealing
5d is aged at ambient temperature.
(2)SiO2Sol-gel modified processing：By alkaline SiO2Colloidal sol is modified using polysiloxane-modified technology, is plated
Film liquid.Wherein doped poly silicon oxygen alkane and SiO2The volume ratio of colloidal sol is 2%.
(3) glass substrate is cleaned, the glass substrate after cleaning is immersed in colloidal sol, lifted after soak time 30s,
Lift coating speed 120mm/min.
(4) glass substrate after lifting plated film is put into drying box, is toasted under the conditions of 220 DEG C and dry 15min；It is dry
It is put into Muffle furnace and is sintered after dry, 20min is sintered at 500 DEG C, forms antireflective coating.
(5) antireflective coating glass substrate is placed under uviol lamp, carries out UV illumination, time 60s；, will after photo-irradiation treatment
Sample is put into the C that volume ratio is 1.5%6H16O3SSi in super dry solvent toluene mixture with soaking, time 60min, is formed single
Molecular function layer；
(6) by the anti reflection glass film deionized water rinsing after immersion, other solvents remained are removed；Blown with nitrogen
It is dry.
As a result showing, anti reflection glass film hardness manufactured in the present embodiment can reach 5H, on a glass substrate, sample peak value
Transmissivity reaches 97.43%, has significant broad-band transparence-increased effect, wavelength-transmittance graph is as shown in Figure 3.
Embodiment 4
(1) SiO is configured2Colloidal sol：Using tetraethyl orthosilicate, absolute ethyl alcohol, deionized water and ammoniacal liquor as raw material, alkalescence is prepared
SiO2Colloidal sol, wherein tetraethyl orthosilicate：Absolute ethyl alcohol：Deionized water：The mol ratio of ammoniacal liquor is 1:20:10:0.1.Prepare alkalescence
SiO2The method of colloidal sol is：After magnetic agitation tetraethyl orthosilicate ethanol solution 3-10min, by absolute ethyl alcohol, go from
The solution of sub- water and ammoniacal liquor is added dropwise in tetraethyl orthosilicate ethanol solution, continue magnetic agitation to uniformly after, sealing
5d is aged at ambient temperature.
(2)SiO2Sol-gel modified processing：By alkaline SiO2Colloidal sol is modified using polysiloxane-modified technology, is plated
Film liquid.Wherein doped poly silicon oxygen alkane and SiO2The volume ratio of colloidal sol is 16%.
(3) glass substrate is cleaned, the glass substrate after cleaning is immersed in colloidal sol, lifted after soak time 30s,
Lift coating speed 190mm/min.
(4) glass substrate after lifting plated film is put into drying box, is toasted under the conditions of 200 DEG C and dry 5min；It is dry
It is put into Muffle furnace and is sintered after dry, 30min is sintered at 480 DEG C, forms antireflective coating.
(5) antireflective coating glass substrate is placed under uviol lamp, carries out UV illumination, time 30s；, will after photo-irradiation treatment
Sample is put into the C that volume ratio is 3%6H16O3SSi in super dry solvent toluene mixture with soaking, time 30min, forms single point
Subfunction layer；
(6) by the anti reflection glass film deionized water rinsing after immersion, other solvents remained are removed；Blown with nitrogen
It is dry.
As a result showing, anti reflection glass film hardness manufactured in the present embodiment can reach 5H, on a glass substrate, sample peak value
Transmissivity reaches 93.60%, has significant broad-band transparence-increased effect, wavelength-transmittance graph is as shown in Figure 4.
Claims (10)
- A kind of 1. preparation method of the doped poly silicon oxygen alkane colloidal sol antireflective coating based on modifying interface, it is characterised in that：In substrate After superficial growth antireflective coating, the antireflective coating is pre-processed, ensures to form oh group on antireflective coating, then will be raw Substrate with antireflective coating is immersed in the solution containing sulfydryl, and with the solution containing sulfydryl hydrolysis occurs for hydroxyl, and then The list functional layer containing sulfydryl is formed by way of molecular self-assembling on antireflective coating surface, finally with deionized water rinsing, Remove the solvent of residual, drying.
- A kind of 2. preparation side of doped poly silicon oxygen alkane colloidal sol antireflective coating based on modifying interface according to claim 1 Method, it is characterised in that：Described pretreatment refers to ultra violet lamp, wherein, intensity of illumination 100-200mw/cm2。
- A kind of 3. preparation side of doped poly silicon oxygen alkane colloidal sol antireflective coating based on modifying interface according to claim 1 Method, it is characterised in that：The described solution containing sulfydryl refers to super dry toluene solution or chlorobenzene solution and 3- mercapto propyl trimethoxies The mixed liquor that silane is formed.
- A kind of 4. preparation side of doped poly silicon oxygen alkane colloidal sol antireflective coating based on modifying interface according to claim 3 Method, it is characterised in that：Described 3- mercaptopropyl trimethoxysilanes are 0.5 with the volume ratio of super dry toluene solution or chlorobenzene solution ~3%.
- A kind of 5. system of doped poly silicon oxygen alkane colloidal sol antireflective coating based on modifying interface according to claim 1 or 3 or 4 Preparation Method, it is characterised in that：Described substrate is immersed in the solution containing sulfydryl, and soak time is 0.5~1h.
- A kind of 6. preparation side of doped poly silicon oxygen alkane colloidal sol antireflective coating based on modifying interface according to claim 1 Method, it is characterised in that：Described antireflective coating is grown in substrate surface using coating technique is lifted, and its concrete technology is：Prepare SiO2Colloidal sol, after substrate is cleaned, it is immersed in SiO2In colloidal sol, lifted after soaking 30~60s, the speed for lifting plated film is 120-190mm/min, finally it is sintered.
- A kind of 7. preparation side of doped poly silicon oxygen alkane colloidal sol antireflective coating based on modifying interface according to claim 6 Method, it is characterised in that：Before lifting plated film, by alkaline SiO2Colloidal sol is modified using polysiloxane-modified technology, wherein, mix Heteropolysiloxane and SiO2The volume ratio of colloidal sol is 2%-16%.
- A kind of 8. preparation side of doped poly silicon oxygen alkane colloidal sol antireflective coating based on modifying interface according to claim 6 Method, it is characterised in that：It is sintered at 480-520 DEG C and sinters 20-40min.
- A kind of 9. preparation side of doped poly silicon oxygen alkane colloidal sol antireflective coating based on modifying interface according to claim 6 Method, it is characterised in that：Described SiO2The preparation method of colloidal sol is：Magnetic agitation tetraethyl orthosilicate ethanol solution, then The solution of absolute ethyl alcohol, deionized water and ammoniacal liquor is added dropwise in tetraethyl orthosilicate ethanol solution, continues magnetic force and stirs Mix to uniformly after, sealing be aged at ambient temperature.
- A kind of 10. preparation side of doped poly silicon oxygen alkane colloidal sol antireflective coating based on modifying interface according to claim 9 Method, it is characterised in that：Tetraethyl orthosilicate：Absolute ethyl alcohol：Deionized water：The mol ratio of ammoniacal liquor is 1:(20-80):(1-10): 0.1。
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| CN103739794A (en) * | 2013-12-24 | 2014-04-23 | 太原理工大学 | Preparation method of hyperbranched polymer-modified nano-silicon dioxide hybrid material |
| CN104097295A (en) * | 2013-04-10 | 2014-10-15 | 鸿富锦精密工业（深圳）有限公司 | Die cavity and manufacturing method thereof |
| CN105399340A (en) * | 2015-12-14 | 2016-03-16 | 上海电力学院 | Super-hydrophobic high-transmittance SiO2 anti-reflecting thin film and preparation method thereof |
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| CN103311320A (en) * | 2012-03-14 | 2013-09-18 | 江苏新源动力有限公司 | Transparent conducting film for solar cell and preparation method thereof |
| CN104097295A (en) * | 2013-04-10 | 2014-10-15 | 鸿富锦精密工业（深圳）有限公司 | Die cavity and manufacturing method thereof |
| CN103739794A (en) * | 2013-12-24 | 2014-04-23 | 太原理工大学 | Preparation method of hyperbranched polymer-modified nano-silicon dioxide hybrid material |
| CN105399340A (en) * | 2015-12-14 | 2016-03-16 | 上海电力学院 | Super-hydrophobic high-transmittance SiO2 anti-reflecting thin film and preparation method thereof |
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