CN105826404A - Preparation method of doped polysiloxanes sol antireflection film based on interface modification - Google Patents
Preparation method of doped polysiloxanes sol antireflection film based on interface modification Download PDFInfo
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- CN105826404A CN105826404A CN201610178576.6A CN201610178576A CN105826404A CN 105826404 A CN105826404 A CN 105826404A CN 201610178576 A CN201610178576 A CN 201610178576A CN 105826404 A CN105826404 A CN 105826404A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- -1 polysiloxanes Polymers 0.000 title claims abstract description 25
- 230000004048 modification Effects 0.000 title abstract 2
- 238000012986 modification Methods 0.000 title abstract 2
- 229920001296 polysiloxane Polymers 0.000 title abstract 2
- 239000000758 substrate Substances 0.000 claims abstract description 42
- 239000008367 deionised water Substances 0.000 claims abstract description 28
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000006117 anti-reflective coating Substances 0.000 claims description 60
- 229910052681 coesite Inorganic materials 0.000 claims description 40
- 229910052906 cristobalite Inorganic materials 0.000 claims description 40
- 239000000377 silicon dioxide Substances 0.000 claims description 40
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 40
- 229910052682 stishovite Inorganic materials 0.000 claims description 40
- 229910052905 tridymite Inorganic materials 0.000 claims description 40
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 38
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 33
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims description 21
- 229920005591 polysilicon Polymers 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- 229910021529 ammonia Inorganic materials 0.000 claims description 19
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 17
- 239000002904 solvent Substances 0.000 claims description 15
- 238000013019 agitation Methods 0.000 claims description 14
- NASVITFAUKYCPM-UHFFFAOYSA-N ethanol;tetraethyl silicate Chemical compound CCO.CCO[Si](OCC)(OCC)OCC NASVITFAUKYCPM-UHFFFAOYSA-N 0.000 claims description 14
- 239000002346 layers by function Substances 0.000 claims description 13
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 12
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000011248 coating agent Substances 0.000 claims description 12
- 238000000576 coating method Methods 0.000 claims description 12
- 238000005286 illumination Methods 0.000 claims description 11
- 238000002791 soaking Methods 0.000 claims description 11
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 claims description 10
- 238000005516 engineering process Methods 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 7
- 239000000463 material Substances 0.000 abstract description 8
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 3
- 230000021715 photosynthesis, light harvesting Effects 0.000 abstract description 3
- 230000035699 permeability Effects 0.000 abstract description 2
- 238000007664 blowing Methods 0.000 abstract 1
- 230000001965 increasing effect Effects 0.000 abstract 1
- 238000005232 molecular self-assembly Methods 0.000 abstract 1
- 238000007781 pre-processing Methods 0.000 abstract 1
- 239000013557 residual solvent Substances 0.000 abstract 1
- 239000011521 glass Substances 0.000 description 38
- 239000000243 solution Substances 0.000 description 30
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 238000004140 cleaning Methods 0.000 description 10
- 238000001035 drying Methods 0.000 description 10
- 238000002834 transmittance Methods 0.000 description 8
- 230000005540 biological transmission Effects 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
- 239000002356 single layer Substances 0.000 description 5
- 230000003667 anti-reflective effect Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 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
- LVTJOONKWUXEFR-FZRMHRINSA-N protoneodioscin Natural products O(C[C@@H](CC[C@]1(O)[C@H](C)[C@@H]2[C@]3(C)[C@H]([C@H]4[C@@H]([C@]5(C)C(=CC4)C[C@@H](O[C@@H]4[C@H](O[C@H]6[C@@H](O)[C@@H](O)[C@@H](O)[C@H](C)O6)[C@@H](O)[C@H](O[C@H]6[C@@H](O)[C@@H](O)[C@@H](O)[C@H](C)O6)[C@H](CO)O4)CC5)CC3)C[C@@H]2O1)C)[C@H]1[C@H](O)[C@H](O)[C@H](O)[C@@H](CO)O1 LVTJOONKWUXEFR-FZRMHRINSA-N 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000004044 response Effects 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
-
- 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 present invention discloses a preparation method of a doped polysiloxanes sol antireflection film based on interface modification. After an antireflection film is grown on the surface of a substrate, the antireflection film is subjected to preprocessing, and it is ensured that a hydroxy group is formed on the antireflection film; the substrate with the antireflection film is immersed in the solution including sulfydryl, a single-molecule function layer including the sulfydryl is formed at the antireflection film through the molecular self-assembly mode; and finally, the single-molecule function layer is cleaned by deionized water, the residual solvent is removed, and the single-molecule function layer is dried by blowing. According to the invention, a single-molecule function layer is introduced to the antireflection film, the molecular chain of the materials of the single-molecule function layer is short and has a certain rigidness, and when the single-molecule function layer is uniformly covered at the surface of the materials, the vibration and the energy dissipation are sealed, the Van der Waals acting force between the molecular is small, the orderliness and the bulk density are low, therefore, the surface hardness of the antireflection film is effectively improved, the transmissivity of the antireflection film is enhanced, and the obvious permeability increasing effect is provided.
Description
[technical field]
The invention belongs to field of photovoltaic technology, relate to a kind of nanometer antireflective coating, particularly relate to a kind of modifying interface method of nanometer antireflective coating, the present invention.
[background technology]
In area of solar cell, can effectively promote focus and the difficult point of the conversion efficiency of solaode, always industry research by improving the light transmission rate of substrate of glass.Coated with antireflection film in the substrate of glass of solaode, can reduce reflectance to greatest extent, increases transmitance.There is in developing solaode response spectral range the photovoltaic nanometer antireflective coating glass of high permeability, can equal extent raising conversion efficiency of solar cell, reduce cost of electricity-generating, promote the market competitiveness of solar cell power generation, shorten the period of cost recovery generated electricity by way of merging two or more grid systems, there is extraordinary economic outlook.
Photovoltaic antireflective coating is mainly used in the cover plate materials of photovoltaic cell, it is typically mounted under outdoor environment, the most also can be in areas such as the more extreme desert of weather, wastelands, therefore it is required that product not only to have high transmitance, but also require that film layer to withstand hot and humid condition and have the mechanical performance such as good hardness and damage resistant abrasion-resistant ability.But in existing product, antireflective coating case hardness is not high enough, damage resistant abrasion-resistant ability, the most easily scratches, thus affects performance and the life-span of product.
Based on this, patent of the present invention provides the preparation method of the antireflective coating that a kind of hardness based on modifying interface is high, damage resistant ability is strong and transmitance is high.
[summary of the invention]
The present invention provides a kind of method that antireflective coating prepared by doped poly silicon oxygen alkane colloidal sol based on modifying interface, unimolecule functional layer is introduced by molecular self-assembling, the case hardness of antireflective coating can be effectively improved and there is obvious antireflective effect, and then obtaining the antireflective coating that hardness is high, damage resistant ability is strong and transmitance is high.
The present invention is by the following technical solutions:
A kind of preparation method of doped poly silicon oxygen alkane colloidal sol antireflective coating based on modifying interface, after substrate surface growth antireflective coating, this antireflective coating is carried out pretreatment, ensure to be formed on antireflective coating oh group, growth then has the substrate of antireflective coating immerse in the solution containing sulfydryl, by the way of molecular self-assembling, the unimolecule functional layer containing sulfydryl is formed at antireflective coating, finally with deionized water rinsing, remove the solvent of residual, dry up.
Preferably, described pretreatment refers to ultra violet lamp, and wherein, intensity of illumination is 100-200mw/cm2。
Preferably, the described solution containing sulfydryl refers to the mixed liquor that super dry toluene solution or chlorobenzene solution are formed with 3-mercaptopropyl trimethoxysilane.
Preferably, described 3-mercaptopropyl trimethoxysilane is 0.5～3% with the volume ratio of super dry toluene solution or chlorobenzene solution.
Preferably, described substrate immerses in the solution containing sulfydryl, and soak time is 0.5～1h.
Preferably, described antireflective coating utilizes lifting coating technique to be grown in substrate surface, its specifically comprises the processes of: preparation SiO2Colloidal sol, after being cleaned by substrate, is immersed in SiO2In colloidal sol, lifting after soaking 30～60s, the speed of lifting plated film is 120-190mm/min, is finally sintered.
Preferably, before lifting plated film, by alkalescence SiO2Colloidal sol uses polysiloxane-modified technology to be modified, wherein, and doped poly silicon oxygen alkane and SiO2The volume ratio of colloidal sol is 2%-16%.
Preferably, 20-40min is sintered at being sintered in 480-520 DEG C.
Preferably, described SiO2The preparation method of colloidal sol is: magnetic agitation tetraethyl orthosilicate ethanol solution, then the solution of dehydrated alcohol, deionized water and ammonia is added dropwise in tetraethyl orthosilicate ethanol solution, continue magnetic agitation to after uniformly, seal and be aged at ambient temperature.
Preferably, tetraethyl orthosilicate: dehydrated alcohol: deionized water: the mol ratio of ammonia is 1:(20-80): (1-10): 0.1.
Compared with prior art, the present invention at least has the advantages that the present invention is after substrate surface growth antireflective coating, this antireflective coating is carried out pretreatment, ensure to be formed on antireflective coating oh group, growth then has the substrate of antireflective coating immerse in the solution containing sulfydryl, by the way of molecular self-assembling, the unimolecule functional layer containing sulfydryl is formed at antireflective coating, finally with deionized water rinsing, remove the solvent of residual, dry up.The present invention is to introduce unimolecule functional layer on antireflective coating surface, the strand of unimolecule functional layer material is shorter, there is 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 less, order and bulk density are low, and then can be effectively improved the case hardness of antireflective coating, and improve the absorbance of antireflective coating, there is obvious antireflective effect.
[accompanying drawing explanation]
In order to make present disclosure be more likely to be clearly understood, below according to the specific embodiment of the present invention and combine accompanying drawing, the present invention is further detailed explanation, wherein
Fig. 1 is to add the wavelength-transmittance graph of 3-mercaptopropyl trimethoxysilane that volume ratio is 0%；
Fig. 2 is to add the wavelength-transmittance graph of 3-mercaptopropyl trimethoxysilane that volume ratio is 0.5%；
Fig. 3 is to add the wavelength-transmittance graph of 3-mercaptopropyl trimethoxysilane that volume ratio is 1.5%；
Fig. 4 is to add the wavelength-transmittance graph of 3-mercaptopropyl trimethoxysilane that volume ratio is 3%.
[detailed description of the invention]
A kind of method that antireflective coating prepared by doped poly silicon oxygen alkane colloidal sol based on modifying interface, including step:
(1) configuration SiO2Colloidal sol: with tetraethyl orthosilicate, dehydrated alcohol, deionized water and ammonia as raw material, preparation alkalescence SiO2Colloidal sol, wherein tetraethyl orthosilicate: dehydrated alcohol: deionized water: the mol ratio of ammonia is 1:(20-80): (1-10): 0.1.Preparation alkalescence SiO2The method of colloidal sol is: after magnetic agitation tetraethyl orthosilicate ethanol solution 3-10min, the solution of dehydrated alcohol, deionized water and ammonia is added dropwise in tetraethyl orthosilicate ethanol solution, continue magnetic agitation to after uniformly, seal and be aged 5d at ambient temperature.
(2)SiO2Sol-gel modified process: by alkalescence SiO2Colloidal sol uses polysiloxane-modified technology to be modified, and obtains coating liquid.Wherein doped poly silicon oxygen alkane and SiO2The volume ratio of colloidal sol can be adjusted between 2%-16%.
(3) cleaning glass substrate, the glass substrate after cleaning is immersed in colloidal sol, lifts after soak time 30-60s, lifts coating speed 120-190mm/min.
(4) putting in drying baker by the glass substrate after lifting plated film, under the conditions of 180-220 DEG C, baking is dried 5-15min；Put in Muffle furnace after drying and be sintered, at 480-520 DEG C, sinter 20-40min, form antireflective coating.
(5) being placed under uviol lamp by antireflective coating glass substrate, carry out UV illumination pretreatment, wherein intensity of illumination is 100-200mw/cm2, light application time is 30-60s；Oh group (-OH) can be formed on antireflective coating glass substrate after UV illumination pretreatment.The compound C of structure shown in a kind of structure formula I is added in the super dry toluene solution of solvent or chlorobenzene solution6H16O3SSi (3-mercaptopropyl trimethoxysilane), described compound is 0.5%-3% with the volume ratio of super dry solvent benzol solution, is sufficiently mixed.After UV illumination pretreatment, being immersed in above-mentioned mixed solution by antireflective coating glass substrate, soak time is 30 minutes to 1 hour, forms unimolecule functional layer.
Hydroxyl is formed after UV illumination pretreatment, in super dry toluene solvant or chlorobenzene solvent, hydrolysis is there is in described hydroxyl with the trimethoxy silane containing sulfydryl, and then on antireflective coating surface by the way of molecular self-assembling, form the unimolecule functional layer containing sulfydryl, and then improve the case hardness of antireflective coating, and having obvious antireflective effect, relevant unimolecule functional layer formation mechenism is as follows.
The molecular self-assembling material that the present invention is claimed carries out modifying interface to antireflective coating surface, it is to introduce monolayer on antireflective coating surface, the strand of monolayer material is shorter, there is 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 less, order and bulk density are low, and then the case hardness of antireflective coating can be effectively improved, and improve the absorbance of antireflective coating, there is obvious antireflective effect.
The volume ratio of 3-mercaptopropyl trimethoxysilane and super dry toluene solvant is limited between 0.5%-3%, when volume ratio is too low be less than 0.5% time, 3-mercaptopropyl trimethoxysilane compound is because concentration is too low cannot form monolayer；When volume ratio is too high be more than 3% time, what 3-mercaptopropyl trimethoxysilane compound was formed because of excessive concentration is polymolecular layer.
(6) the anti reflection glass film deionized water rinsing after soaking, removes the solvent of other residuals；Dry up with nitrogen.
Detailed description of the invention:
Embodiment 1
(1) configuration SiO2Colloidal sol: with tetraethyl orthosilicate, dehydrated alcohol, deionized water and ammonia as raw material, preparation alkalescence SiO2Colloidal sol, wherein tetraethyl orthosilicate: dehydrated alcohol: deionized water: the mol ratio of ammonia is 1:45:3:0.1.Preparation alkalescence SiO2The method of colloidal sol is: after magnetic agitation tetraethyl orthosilicate ethanol solution 3-10min, the solution of dehydrated alcohol, deionized water and ammonia is added dropwise in tetraethyl orthosilicate ethanol solution, after continuing magnetic agitation 2h, seal and be aged 5d at ambient temperature.
(2)SiO2Sol-gel modified process: by alkalescence SiO2Colloidal sol uses polysiloxane-modified technology to be modified, and obtains coating liquid.Wherein doped poly silicon oxygen alkane and SiO2The volume ratio of colloidal sol is 8%.
(3) cleaning glass substrate, the glass substrate after cleaning is immersed in colloidal sol, lifts after soak time 30s, lifts coating speed 190mm/min.
(4) putting in drying baker by the glass substrate after lifting plated film, under the conditions of 180 DEG C, baking is dried 10min；Put in Muffle furnace after drying and be sintered, at 500 DEG C, sinter 30min, form antireflective coating.
(5) being placed under uviol lamp by antireflective coating glass substrate, carry out UV illumination, the time is 30s；After photo-irradiation treatment, sample is put into the C that volume ratio is 0%6H16O3Soaking in SSi and super dry solvent toluene mixture, the time is 30min, forms unimolecule functional layer；
(6) the anti reflection glass film deionized water rinsing after soaking, removes the solvent of other residuals；Dry up with nitrogen.
Result shows, anti reflection glass film hardness prepared by the present embodiment is 3H, and on a glass substrate, sample peak transmission reaches 89.36%, and wavelength-transmittance graph is as shown in Figure 1.
Embodiment 2
(1) configuration SiO2Colloidal sol: with tetraethyl orthosilicate, dehydrated alcohol, deionized water and ammonia as raw material, preparation alkalescence SiO2Colloidal sol, wherein tetraethyl orthosilicate: dehydrated alcohol: deionized water: the mol ratio of ammonia is 1:60:8:0.1.Preparation alkalescence SiO2The method of colloidal sol is: after magnetic agitation tetraethyl orthosilicate ethanol solution 3-10min, the solution of dehydrated alcohol, deionized water and ammonia is added dropwise in tetraethyl orthosilicate ethanol solution, continue magnetic agitation to after uniformly, seal and be aged 5d at ambient temperature.
(2)SiO2Sol-gel modified process: by alkalescence SiO2Colloidal sol uses polysiloxane-modified technology to be modified, and obtains coating liquid.Wherein doped poly silicon oxygen alkane and SiO2The volume ratio of colloidal sol is 12%.
(3) cleaning glass substrate, the glass substrate after cleaning is immersed in colloidal sol, lifts after soak time 60s, lifts coating speed 150mm/min.
(4) putting in drying baker by the glass substrate after lifting plated film, under the conditions of 200 DEG C, baking is dried 10min；Put in Muffle furnace after drying and be sintered, at 520 DEG C, sinter 40min, form antireflective coating.
(5) being placed under uviol lamp by antireflective coating glass substrate, carry out UV illumination, the time is 50s；After photo-irradiation treatment, sample is put into the C that volume ratio is 0.5%6H16O3Soaking in SSi and super dry solvent toluene mixture, the time is 30min, forms unimolecule functional layer；
(6) the anti reflection glass film deionized water rinsing after soaking, removes the solvent of other residuals；Dry up with nitrogen.
Result shows, anti reflection glass film hardness prepared by the present embodiment can reach 5H, and on a glass substrate, sample peak transmission reaches 93.06%, has significant broad-band transparence-increased effect, and wavelength-transmittance graph is as shown in Figure 2.
Embodiment 3
(1) configuration SiO2Colloidal sol: with tetraethyl orthosilicate, dehydrated alcohol, deionized water and ammonia as raw material, preparation alkalescence SiO2Colloidal sol, wherein tetraethyl orthosilicate: dehydrated alcohol: deionized water: the mol ratio of ammonia is 1:80:1:0.1.Preparation alkalescence SiO2The method of colloidal sol is: after magnetic agitation tetraethyl orthosilicate ethanol solution 3-10min, the solution of dehydrated alcohol, deionized water and ammonia is added dropwise in tetraethyl orthosilicate ethanol solution, continue magnetic agitation to after uniformly, seal and be aged 5d at ambient temperature.
(2)SiO2Sol-gel modified process: by alkalescence SiO2Colloidal sol uses polysiloxane-modified technology to be modified, and obtains coating liquid.Wherein doped poly silicon oxygen alkane and SiO2The volume ratio of colloidal sol is 2%.
(3) cleaning glass substrate, the glass substrate after cleaning is immersed in colloidal sol, lifts after soak time 30s, lifts coating speed 120mm/min.
(4) putting in drying baker by the glass substrate after lifting plated film, under the conditions of 220 DEG C, baking is dried 15min；Put in Muffle furnace after drying and be sintered, at 500 DEG C, sinter 20min, form antireflective coating.
(5) being placed under uviol lamp by antireflective coating glass substrate, carry out UV illumination, the time is 60s；After photo-irradiation treatment, sample is put into the C that volume ratio is 1.5%6H16O3Soaking in SSi and super dry solvent toluene mixture, the time is 60min, forms unimolecule functional layer；
(6) the anti reflection glass film deionized water rinsing after soaking, removes the solvent of other residuals；Dry up with nitrogen.
Result shows, anti reflection glass film hardness prepared by the present embodiment can reach 5H, and on a glass substrate, sample peak transmission reaches 97.43%, has significant broad-band transparence-increased effect, and wavelength-transmittance graph is as shown in Figure 3.
Embodiment 4
(1) configuration SiO2Colloidal sol: with tetraethyl orthosilicate, dehydrated alcohol, deionized water and ammonia as raw material, preparation alkalescence SiO2Colloidal sol, wherein tetraethyl orthosilicate: dehydrated alcohol: deionized water: the mol ratio of ammonia is 1:20:10:0.1.Preparation alkalescence SiO2The method of colloidal sol is: after magnetic agitation tetraethyl orthosilicate ethanol solution 3-10min, the solution of dehydrated alcohol, deionized water and ammonia is added dropwise in tetraethyl orthosilicate ethanol solution, continue magnetic agitation to after uniformly, seal and be aged 5d at ambient temperature.
(2)SiO2Sol-gel modified process: by alkalescence SiO2Colloidal sol uses polysiloxane-modified technology to be modified, and obtains coating liquid.Wherein doped poly silicon oxygen alkane and SiO2The volume ratio of colloidal sol is 16%.
(3) cleaning glass substrate, the glass substrate after cleaning is immersed in colloidal sol, lifts after soak time 30s, lifts coating speed 190mm/min.
(4) putting in drying baker by the glass substrate after lifting plated film, under the conditions of 200 DEG C, baking is dried 5min；Put in Muffle furnace after drying and be sintered, at 480 DEG C, sinter 30min, form antireflective coating.
(5) being placed under uviol lamp by antireflective coating glass substrate, carry out UV illumination, the time is 30s；After photo-irradiation treatment, sample is put into the C that volume ratio is 3%6H16O3Soaking in SSi and super dry solvent toluene mixture, the time is 30min, forms unimolecule functional layer；
(6) the anti reflection glass film deionized water rinsing after soaking, removes the solvent of other residuals；Dry up with nitrogen.
Result shows, anti reflection glass film hardness prepared by the present embodiment can reach 5H, and on a glass substrate, sample peak transmission reaches 93.60%, has significant broad-band transparence-increased effect, and wavelength-transmittance graph is as shown in Figure 4.
Claims (10)
1. the preparation method of a doped poly silicon oxygen alkane colloidal sol antireflective coating based on modifying interface, it is characterized in that: after substrate surface growth antireflective coating, this antireflective coating is carried out pretreatment, ensure to be formed on antireflective coating oh group, growth then has the substrate of antireflective coating immerse in the solution containing sulfydryl, by the way of molecular self-assembling, the unimolecule functional layer containing sulfydryl is formed at antireflective coating, finally with deionized water rinsing, remove the solvent of residual, dry up.
The preparation method of a kind of doped poly silicon oxygen alkane colloidal sol antireflective coating based on modifying interface the most according to claim 1, it is characterised in that: described pretreatment refers to ultra violet lamp, and wherein, intensity of illumination is 100-200mw/cm2。
The preparation method of a kind of doped poly silicon oxygen alkane colloidal sol antireflective coating based on modifying interface the most according to claim 1, it is characterised in that: the described solution containing sulfydryl refers to the mixed liquor that super dry toluene solution or chlorobenzene solution are formed with 3-mercaptopropyl trimethoxysilane.
The preparation method of a kind of doped poly silicon oxygen alkane colloidal sol antireflective coating based on modifying interface the most according to claim 3, it is characterised in that: described 3-mercaptopropyl trimethoxysilane is 0.5～3% with the volume ratio of super dry toluene solution or chlorobenzene solution.
5. according to the preparation method of a kind of based on modifying interface the doped poly silicon oxygen alkane colloidal sol antireflective coating described in claim 1 or 3 or 4, it is characterised in that: described substrate immerses in the solution containing sulfydryl, and soak time is 0.5～1h.
The preparation method of a kind of doped poly silicon oxygen alkane colloidal sol antireflective coating based on modifying interface the most according to claim 1, it is characterised in that: described antireflective coating utilizes lifting coating technique to be grown in substrate surface, its specifically comprises the processes of: preparation SiO2Colloidal sol, after being cleaned by substrate, is immersed in SiO2In colloidal sol, lifting after soaking 30～60s, the speed of lifting plated film is 120-190mm/min, is finally sintered.
The preparation method of a kind of doped poly silicon oxygen alkane colloidal sol antireflective coating based on modifying interface the most according to claim 6, it is characterised in that: before lifting plated film, by alkalescence SiO2Colloidal sol uses polysiloxane-modified technology to be modified, wherein, and doped poly silicon oxygen alkane and SiO2The volume ratio of colloidal sol is 2%-16%.
The preparation method of a kind of doped poly silicon oxygen alkane colloidal sol antireflective coating based on modifying interface the most according to claim 6, it is characterised in that: sinter 20-40min at being sintered in 480-520 DEG C.
The preparation method of a kind of doped poly silicon oxygen alkane colloidal sol antireflective coating based on modifying interface the most according to claim 6, it is characterised in that: described SiO2The preparation method of colloidal sol is: magnetic agitation tetraethyl orthosilicate ethanol solution, then the solution of dehydrated alcohol, deionized water and ammonia is added dropwise in tetraethyl orthosilicate ethanol solution, continue magnetic agitation to after uniformly, seal and be aged at ambient temperature.
The preparation method of a kind of doped poly silicon oxygen alkane colloidal sol antireflective coating based on modifying interface the most according to claim 9, it is characterised in that: tetraethyl orthosilicate: dehydrated alcohol: deionized water: the mol ratio of ammonia is 1:(20-80): (1-10): 0.1.
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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 |
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