CN107555807A - A kind of method for preparing rub resistance hydrophobic silica anti-reflection film - Google Patents
A kind of method for preparing rub resistance hydrophobic silica anti-reflection film Download PDFInfo
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- CN107555807A CN107555807A CN201710734585.3A CN201710734585A CN107555807A CN 107555807 A CN107555807 A CN 107555807A CN 201710734585 A CN201710734585 A CN 201710734585A CN 107555807 A CN107555807 A CN 107555807A
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Abstract
The invention belongs to SiO2Thin film technique field, and in particular to one kind prepares the hydrophobic SiO of rub resistance2The method of anti-reflection film.Concretely comprise the following steps：By tetraethyl orthosilicate（TEOS）, VTES, absolute ethyl alcohol, distilled water and ammoniacal liquor in mass ratio 8.0 15.6：1.0‑7.6：120‑150：1‑10：0.1 5.5 be added in closed vial be well mixed, 25 60 DEG C of h of temperature constant magnetic stirring 0.5 24, it is aged 3 30 days at room temperature afterwards, with dip-coating method by the colloidal sol of preparation homogeneous film formation on a glass substrate, then film layer is soaked with containing hydrogen silicone oil/n-hexane/catalyst mixed liquid that mass fraction is 0.5 20%, it is rear to take out heat treatment.The method can be realized to adjacent S iO2The chemical crosslinking of particle, it is made and has rub resistance and hydrophobic SiO concurrently2Anti-reflection film.
Description
Technical field
The invention belongs to SiO2Thin film technique field, and in particular to one kind prepares the hydrophobic SiO of rub resistance2The method of anti-reflection film.
Background technology
With the quickening of Chinese society doctrine modernization, national energy faces a severe challenge.Develop clean energy resource
As the main direction of China's Energy restructuring.Solar energy is as a kind of new energy, because its is renewable and clean environment firendly spy
Property, by the extensive attention of various countries.Solar cell needs packaged glass to protect；But its reflection of packaged glass surface to light
It is a key factor for influenceing electricity conversion.Therefore anti-reflection film is coated with packaging glass of solar cell can be effective
The loss of light is reduced, improves the photoelectric transformation efficiency of solar cell.However, SiO2Between anti-reflection film surface great amount of hydroxy group and particle
The presence of abundant hole so that SiO2It is strong that anti-reflection film is faced with water imbibition, film optical property is impaired etc. it is environment resistant the problems such as.Together
When, use environment and artificial cleaning condition due to solar cell, it is desirable to which the anti-reflection film on its packaged glass surface has preferable
Crocking resistance.Under the conditions of base catalysis, the glomerate SiO of raw material teos hydrolysis polycondensation shape2Particle, in its film layer
Intermolecular force is weak, and the rub resistance of film is poor.In order to improve SiO2The problems such as environment resistant and rub resistance of anti-reflection film,
Method proposes being co-precursor with VTES and tetraethyl orthosilicate, pass through the two cohydrolysis-polycondensation
Journey, hydrophobic vinyl group is incorporated into SiO2On particle, SiO is reduced2The polar group on anti-reflection film surface, then uses Silicon Containing Hydrogen
Oil meter face is modified, and is crosslinked the vinyl double bond of introducing, so as to greatly improve its environment resistant and rub resistance, the novel letter of the method
Just it is efficient.
The content of the invention
It is an object of the invention to provide one kind to prepare the hydrophobic SiO of rub resistance2The method of anti-reflection film, method simple and effective,
Its application out of doors is widened while the environment resistant and rub resistance of anti-reflection film is improved.
To achieve these goals.The technical scheme is that：
One kind prepares the hydrophobic SiO of rub resistance2The method of anti-reflection film comprises the following steps that：
（1）Prepare SiO2Colloidal sol：By tetraethyl orthosilicate（TEOS）, VTES, absolute ethyl alcohol, distilled water and ammonia
Water 8.0-15.6 in mass ratio：1.0-7.6：120-150：1-10：0.1-5.5 is added in closed vial and is well mixed,
Temperature constant magnetic stirring, it is aged at room temperature afterwards；
（2）Plated film：Using dipping-pulling method, by the colloidal sol of preparation in glass substrate surface homogeneous film formation；
（3）Anti-reflection film crosslinking curing：The glass substrate for being coated with film is placed in containing hydrogen silicone oil/n-hexane/catalyst and soaked, then
It is heat-treated.
Wherein step（1）Constant temperature whipping temp be 25-60 DEG C, the time is 0.5-24 h.
Wherein step（1）Room temperature digestion time be 3-30 days.
Wherein step（2）Pull rate be 50-300 mm/min.
Wherein step（3）Containing hydrogen silicone oil quality be relative to n-hexane quality 0.05-20%, soak time 2-
36 h。
Wherein step（3）Catalyst be Kastredt catalyst or dibutyl tin laurate, the concentration of catalyst is pressed
30-500 ppm are calculated as according to the quality of added containing hydrogen silicone oil.
Wherein step（3）Heat treatment temperature be 120 ~ 300 DEG C, heat treatment time is 1 ~ 5 h
The remarkable advantage of the present invention：The vinyl for being available for crosslinking is introduced to silica particle surface by hybrid inorganic-organic,
And crosslinking curing is further carried out to the anti-reflection film containing vinyl by containing hydrogen silicone oil, improve that its is hydrophobic simultaneously, carry again
Its high rub resistance, method are novel simple efficient.
Brief description of the drawings
Fig. 1 is SiO in embodiment2The contact angle figure of anti-reflection film.
Embodiment
The present invention further illustrates the present invention with following experiments example, but protection scope of the present invention is not limited to following reality
Test example.
Comparative example
（1）By tetraethyl orthosilicate（TEOS）, VTES, absolute ethyl alcohol, distilled water and ammoniacal liquor in mass ratio
15.6：0：137.4：4：0.91 is added in closed vial well mixed, 30 DEG C of h of temperature constant magnetic stirring 2, afterwards in room
The lower ageing of temperature 9 days.
（2）With dipping-pulling method with 100 mm/min pull rate by the colloidal sol of preparation film forming on a glass substrate.
（3）The glass substrate for plating film layer is put in 2 h drying, rear natural cooling in 160 DEG C.
Embodiment 1
（1）By tetraethyl orthosilicate（TEOS）, VTES, absolute ethyl alcohol, distilled water and ammoniacal liquor in mass ratio
13.90：2.54：137.4：4：0.91 is added in closed vial well mixed, 30 DEG C of h of temperature constant magnetic stirring 2, afterwards
It is aged 6 days at room temperature.
（2）With dipping-pulling method with 150 mm/min pull rate by the colloidal sol of preparation film forming on a glass substrate.
（3）Configure in containing hydrogen silicone oil/n-hexane/mixed liquor that containing hydrogen silicone oil mass concentration is 5%, and add relative to containing
The ppm of hydrogen silicone oil quality meter 50 Kastredt catalyst；The glass substrate for being coated with film is placed in above-mentioned mixed liquor after 22 h
Take out, 1 h is heat-treated at a temperature of 120 DEG C.
Embodiment 2
（1）By tetraethyl orthosilicate（TEOS）, VTES, absolute ethyl alcohol, distilled water and ammoniacal liquor in mass ratio
11.9：4.34：137.4：4：0.91 is added in closed vial well mixed, 25 DEG C of h of temperature constant magnetic stirring 2, afterwards
It is aged 9 days at room temperature.
（2）With dipping-pulling method with 200 mm/min pull rate by the colloidal sol of preparation film forming on a glass substrate.
（3）Containing hydrogen silicone oil/n-hexane mixed liquor that containing hydrogen silicone oil mass concentration is 5% is prepared, and is added relative to Silicon Containing Hydrogen
The oily ppm of gauge 500 catalyst dibutyltin dilaurylate；The glass substrate for being coated with film is placed in above-mentioned mixed liquor
Taken out after soaking 5 h, 3 h are heat-treated at a temperature of 160 DEG C.
Embodiment 3
（1）By tetraethyl orthosilicate（TEOS）, VTES, absolute ethyl alcohol, distilled water and ammoniacal liquor in mass ratio
9.27：6.78：137.4：4：0.91 is added in closed vial well mixed, 30 DEG C of h of temperature constant magnetic stirring 5, afterwards
It is aged 12 days at room temperature.
（2）With dipping-pulling method with 100 mm/min pull rate by the colloidal sol of preparation film forming on a glass substrate.
（3）Containing hydrogen silicone oil/n-hexane mixed liquor that containing hydrogen silicone oil mass concentration is 8% is prepared, and is added relative to Silicon Containing Hydrogen
The oily ppm of gauge 100 Kastredt catalyst；The glass substrate for being coated with film is placed in above-mentioned mixed liquor and soaks 36 h
After take out, 3 h are heat-treated at a temperature of 300 DEG C.
The transmitance suppression ratio of table 1 compared with
Table 1 is that the transmitance being wiped repeatedly with non-dust cloth before and after 100 times compares.As seen from the above table, comparative example transmitance declines
4.84%, the transmitance of anti-reflection film declines seldom in each embodiment, declines 1.58%, 0.55%, 0.56% respectively, rub resistance obtains
To raising largely, the reason is that the surface modification of containing hydrogen silicone oil causes adjacent S iO2Particle is chemically crosslinked,
So as to substantially increase intermolecular force.
From Fig. 1 it can be found that the anti-reflection film of comparative example is non-modified, it shows good hydrophilicity, through Silicon Containing Hydrogen
The VTES of oil meter face modification is modified the SiO prepared2Anti-reflection film, hydrophobic performance greatly enhance, in embodiment 2
Contact angle reached 126.1 °.
Claims (8)
1. one kind prepares the hydrophobic SiO of rub resistance2The method of anti-reflection film, it is characterised in that：With VTES and positive silicon
Acetoacetic ester is co-precursor, and Nano-meter SiO_2 is obtained after hydrolysis and copolymerization2Vinyl is contained on particle, its surface；Pass through Silicon Containing Hydrogen again
Oil-Si -- H bond and SiO2Addition reaction occurs for the vinyl of particle surface, realizes to adjacent S iO2The chemical crosslinking of particle, system
Rub resistance and hydrophobic SiO must be had concurrently2Anti-reflection film.
2. one kind according to claim 1 prepares the hydrophobic SiO of rub resistance2The method of anti-reflection film, it is characterised in that：Specific step
It is rapid as follows：
（1）Prepare SiO2Colloidal sol：By tetraethyl orthosilicate（TEOS）, VTES, absolute ethyl alcohol, distilled water and ammonia
Water 8.0-15.6 in mass ratio：1.0-7.6：120-150：1-10：0.1-5.5 is added in closed vial and is well mixed,
Temperature constant magnetic stirring, it is aged at room temperature afterwards；
（2）Plated film：Using dipping-pulling method, by the colloidal sol of preparation in glass substrate surface homogeneous film formation；
（3）Anti-reflection film crosslinking curing：The glass substrate for being coated with film is placed in containing hydrogen silicone oil/n-hexane/catalyst mixed solution
Middle immersion, then be heat-treated.
3. one kind according to claim 2 prepares the hydrophobic SiO of rub resistance2The method of anti-reflection film, it is characterised in that：Step（1）
Constant temperature whipping temp be 25-60 DEG C, the time is 0.5-24 h.
4. one kind according to claim 2 prepares the hydrophobic SiO of rub resistance2The method of anti-reflection film, it is characterised in that：Step（1）
Room temperature digestion time be 3-30 days.
5. one kind according to claim 2 prepares the hydrophobic SiO of rub resistance2The method of anti-reflection film, it is characterised in that：Step（2）
Pull rate be 50-300 mm/min.
6. one kind according to claim 2 prepares the hydrophobic SiO of rub resistance2The method of anti-reflection film, it is characterised in that：Step（3）
Containing hydrogen silicone oil quality be relative to n-hexane quality 0.05-20%, soak time is 2-36 h.
7. one kind according to claim 2 prepares the hydrophobic SiO of rub resistance2The method of anti-reflection film, it is characterised in that：Step（3）
Catalyst be Kastredt catalyst or dibutyl tin laurate, the concentration of catalyst according to added containing hydrogen silicone oil quality
It is calculated as 30-500 ppm.
8. one kind according to claim 2 prepares the hydrophobic SiO of rub resistance2The method of anti-reflection film, it is characterised in that：Step（3）
Heat treatment temperature be 120 ~ 300 DEG C, heat treatment time is 1 ~ 5 h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108395114A (en) * | 2018-03-09 | 2018-08-14 | 三峡大学 | A kind of anti-reflection hydrophobic film of broadband and preparation method thereof |
| CN110408070A (en) * | 2019-07-31 | 2019-11-05 | 中国工程物理研究院激光聚变研究中心 | A kind of basic frequency laser film of high threshold scratch-resistant high-transmission rate and preparation method thereof |
| CN112110654A (en) * | 2020-09-25 | 2020-12-22 | 常州大学 | Preparation method and application of optical anti-reflection antifogging film |
| CN115231835A (en) * | 2022-09-19 | 2022-10-25 | 江苏中新瑞光学材料有限公司 | Preparation method of UV (ultraviolet) curing super-hydrophobic material |
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| CN101885586A (en) * | 2009-05-14 | 2010-11-17 | 中国科学院宁波材料技术与工程研究所 | Preparation method of photovoltaic glass surface antireflection film |
| CN106800885A (en) * | 2016-12-21 | 2017-06-06 | 中国科学院兰州化学物理研究所 | A kind of large-scale preparation method of transparent hydrophobic/super-amphiphobic coating |
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| CN101885586A (en) * | 2009-05-14 | 2010-11-17 | 中国科学院宁波材料技术与工程研究所 | Preparation method of photovoltaic glass surface antireflection film |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108395114A (en) * | 2018-03-09 | 2018-08-14 | 三峡大学 | A kind of anti-reflection hydrophobic film of broadband and preparation method thereof |
| CN110408070A (en) * | 2019-07-31 | 2019-11-05 | 中国工程物理研究院激光聚变研究中心 | A kind of basic frequency laser film of high threshold scratch-resistant high-transmission rate and preparation method thereof |
| CN110408070B (en) * | 2019-07-31 | 2022-03-01 | 中国工程物理研究院激光聚变研究中心 | High-threshold-value scratch-resistant high-transmittance fundamental-frequency laser film and preparation method thereof |
| CN112110654A (en) * | 2020-09-25 | 2020-12-22 | 常州大学 | Preparation method and application of optical anti-reflection antifogging film |
| CN112110654B (en) * | 2020-09-25 | 2022-07-05 | 常州大学 | Preparation method and application of optical anti-reflection antifogging film |
| CN115231835A (en) * | 2022-09-19 | 2022-10-25 | 江苏中新瑞光学材料有限公司 | Preparation method of UV (ultraviolet) curing super-hydrophobic material |
| CN115231835B (en) * | 2022-09-19 | 2022-12-02 | 江苏中新瑞光学材料有限公司 | Preparation method of UV (ultraviolet) curing super-hydrophobic material |
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Application publication date: 20180109 |