CN106630668A - Method for preparing SiO2 antireflection film with controllable refractive index by using propyltriethoxysilane - Google Patents
Method for preparing SiO2 antireflection film with controllable refractive index by using propyltriethoxysilane Download PDFInfo
- Publication number
- CN106630668A CN106630668A CN201610888398.6A CN201610888398A CN106630668A CN 106630668 A CN106630668 A CN 106630668A CN 201610888398 A CN201610888398 A CN 201610888398A CN 106630668 A CN106630668 A CN 106630668A
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- Prior art keywords
- refractive index
- propyl
- reflection film
- sio
- triethoxysilicane
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Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/23—Oxides
- C03C17/25—Oxides by deposition from the liquid phase
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/213—SiO2
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/111—Deposition methods from solutions or suspensions by dipping, immersion
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Laminated Bodies (AREA)
- Surface Treatment Of Optical Elements (AREA)
- Surface Treatment Of Glass (AREA)
Abstract
The invention provides a method for preparing a SiO2 antireflection film with controllable refractive index by using propyltriethoxysilane. The method comprises the following concrete steps: mixing tetraethoxysilane, propyltriethoxysilane, absolute ethyl alcohol and ammonia water according to a mass ratio of (11.0-15.6): (1-8): (130-200): (3.6-6.6), adding the mixture into an airtight glass container, carrying out magnetic stirring at 25 to 50 DEG C for 0.5 to 12 h, and carrying out aging at a constant temperature of 20 to 40 DEG C for 3 to 30 days; and coating on a film on a substrate by adopting an impregnation-pulling method so as to obtain a film layer, i.e., the SiO2 antireflection film with a certain refractive index. The method provided by the invention has simple and highly-efficient process and lays a foundation for preparation of broadband multilayer antireflection films.
Description
Technical field
The invention belongs to prepare the controllable SiO of refractive index2Anti-reflection technical field of membrane, and in particular to one kind ethoxy of propyl group three
Base silane prepares the controllable SiO of refractive index2The method of anti-reflection film.
Background technology
The SiO of individual layer2Anti-reflection film can only realize higher transmitance in a certain specific wavelength, but in actual applications,
Such as in solar-energy photo-voltaic cell or high energy laser system, large range of high transmission is generally required.Multilayer SiO2Anti-reflection film can
To realize the transmission on a large scale of light, central is by different refractivity SiO2What anti-reflection film was combined.So, prepare different foldings
Penetrate the SiO of rate2Anti-reflection film is design wideband SiO2The key of anti-reflection film.It is general to adjust SiO by introducing template2Anti-reflection film
Porosity, finally prepare the SiO of different refractivity2Anti-reflection film, but the method is more complicated, also to be removed by methods such as calcinings
Remove template.The controllable SiO of refractive index is prepared with propyl-triethoxysilicane and tetraethyl orthosilicate2Anti-reflection film, the method need not
Template is introduced, method is easy, effect is significant.
The content of the invention
The purpose of the present invention aims to provide a kind of propyl-triethoxysilicane and prepares the controllable SiO of refractive index2Anti-reflection film
Method, provides basis to design wideband anti-reflection film, the method need not introduce template, method simplicity, effect is significant.
To achieve these goals, the technical scheme is that：
A kind of controllable SiO of refractive index2The preparation method of anti-reflection film is comprised the following steps that：
（1）SiO2The preparation of colloidal sol：By tetraethyl orthosilicate, propyl-triethoxysilicane, absolute ethyl alcohol and ammoniacal liquor in mass ratio
11.0-15.6：1-8：130-200：3.6-6.6 is added in closed glass container, in 25-50 DEG C of magnetic agitation 0.5-12
H, is then aged 3-30 days in 20-40 DEG C of constant temperature.
（2）The plated film that dipping-pulling method adopted with certain pull rate on substrate, the film layer of gained is certain refraction
The SiO of rate2Anti-reflection film.
A kind of controllable SiO of refractive index obtained in method as mentioned2Anti-reflection film, the speed of dipping-lifting is 50-200
mm/min。
The remarkable advantage of the present invention：Prior art adjusts SiO generally by template is introduced2The hole of anti-reflection film
Rate, finally prepares the SiO of different refractivity2Anti-reflection film, but the method is more complicated, also to remove template by methods such as calcinings
Agent.The present invention prepares the controllable SiO of refractive index with propyl-triethoxysilicane and tetraethyl orthosilicate2Anti-reflection film, the method need not
Template is introduced, method is easy, effect is significant.
Specific embodiment
Present invention following experiments example is come the further present invention, but protection scope of the present invention is not limited to following experiments
Example.
Embodiment 1
（1）In mass ratio it is 14.2 by tetraethyl orthosilicate, propyl-triethoxysilicane, absolute ethyl alcohol, ammoniacal liquor：1.88：130：3.6
In being added to closed glass container, in 25 DEG C of h of magnetic agitation 2,20 DEG C of constant temperature are aged 5 days.
（2）Dipping-pulling method is adopted with 50 mm/min pull rate plated films on substrate.
Embodiment 2
（1）In mass ratio it is 13 by tetraethyl orthosilicate, propyl-triethoxysilicane, absolute ethyl alcohol, ammoniacal liquor：3.45：130：3.6 add
Enter in closed glass container, in 35 DEG C of h of magnetic agitation 12,30 DEG C of constant temperature are aged 30 days.
（2）Dipping-pulling method is adopted with 100 mm/min pull rate plated films on substrate.
Embodiment 3
（1）In mass ratio it is 11.12 by tetraethyl orthosilicate, propyl-triethoxysilicane, absolute ethyl alcohol, ammoniacal liquor：5.92：130：
3.6 are added in closed glass container, and in 50 DEG C of h of magnetic agitation 0.5,40 DEG C of constant temperature are aged 3 days.
（2）Dipping-pulling method is adopted with 200 mm/min pull rate plated films on substrate.
SiO under the raw material of the different quality ratio of table 12The centre wavelength of anti-reflection film, maximum transmission and refractive index
Obtained SiO of the invention2The modification scope of anti-reflection film refractive index is 1.10-1.23.
The foregoing is only presently preferred embodiments of the present invention, all impartial changes done according to scope of the present invention patent with
Modification, should all belong to the covering scope of the present invention.
Claims (6)
1. a kind of propyl-triethoxysilicane prepares the controllable SiO of refractive index2The method of anti-reflection film, it is characterised in that use propyl group
Triethoxysilane prepares SiO with tetraethyl orthosilicate2Anti-reflection film.
2. propyl-triethoxysilicane according to claim 1 prepares the controllable SiO of refractive index2The method of anti-reflection film, its
It is characterised by, comprises the following steps that：
（1）The preparation of colloidal sol：In mass ratio it is 11.0- by tetraethyl orthosilicate, propyl-triethoxysilicane, absolute ethyl alcohol, ammoniacal liquor
15.6：1-8：130-200：3.6-6.6 is mixed to join in closed glass container, in 25-50 DEG C of magnetic agitation 0.5-12
H, 20-40 DEG C of constant temperature is aged 3-30 days；
（2）Using dipping-pulling method on substrate plated film, the film layer of gained is the SiO of certain refractive index2Anti-reflection film.
3. propyl-triethoxysilicane according to claim 2 prepares the controllable SiO of refractive index2The method of anti-reflection film, its
It is characterised by, tetraethyl orthosilicate：Propyl-triethoxysilicane：Absolute ethyl alcohol：Ammoniacal liquor mass ratio is 14.2：1.88：130：3.6.
4. propyl-triethoxysilicane according to claim 2 prepares the controllable SiO of refractive index2The method of anti-reflection film, its
It is characterised by, the temperature of stirring is 25 DEG C, and the time is 2 h.
5. propyl-triethoxysilicane according to claim 2 prepares the controllable SiO of refractive index2The method of anti-reflection film, its
It is characterised by, the constant temperature digestion time of mixed sols is 5 days, and thermostat temperature is 20 DEG C.
6. propyl-triethoxysilicane according to claim 2 prepares the controllable SiO of refractive index2The method of anti-reflection film, its
It is characterised by, step（2）The speed of middle plated film is 50-200 mm/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610888398.6A CN106630668A (en) | 2016-10-12 | 2016-10-12 | Method for preparing SiO2 antireflection film with controllable refractive index by using propyltriethoxysilane |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610888398.6A CN106630668A (en) | 2016-10-12 | 2016-10-12 | Method for preparing SiO2 antireflection film with controllable refractive index by using propyltriethoxysilane |
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| CN106630668A true CN106630668A (en) | 2017-05-10 |
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| CN201610888398.6A Pending CN106630668A (en) | 2016-10-12 | 2016-10-12 | Method for preparing SiO2 antireflection film with controllable refractive index by using propyltriethoxysilane |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107540241A (en) * | 2017-08-24 | 2018-01-05 | 福建农林大学 | A kind of method that the controllable hydrophobic silica anti-reflection film of refractive index is prepared with phenyl triethoxysilane |
| CN107942414A (en) * | 2017-12-27 | 2018-04-20 | 福建农林大学 | A kind of bottom is the double-deck wideband anti-reflection film of organic inorganic hybridization film |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104230178A (en) * | 2014-09-09 | 2014-12-24 | 中国科学院上海光学精密机械研究所 | Preparation method of modified porous silicon dioxide anti-reflection coating |
| CN105130205A (en) * | 2015-08-25 | 2015-12-09 | 杭州绿梦纳米材料有限公司 | Preparation method of film-plating liquid for antireflection film of high anti-weathering type photovoltaic glass |
-
2016
- 2016-10-12 CN CN201610888398.6A patent/CN106630668A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104230178A (en) * | 2014-09-09 | 2014-12-24 | 中国科学院上海光学精密机械研究所 | Preparation method of modified porous silicon dioxide anti-reflection coating |
| CN105130205A (en) * | 2015-08-25 | 2015-12-09 | 杭州绿梦纳米材料有限公司 | Preparation method of film-plating liquid for antireflection film of high anti-weathering type photovoltaic glass |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107540241A (en) * | 2017-08-24 | 2018-01-05 | 福建农林大学 | A kind of method that the controllable hydrophobic silica anti-reflection film of refractive index is prepared with phenyl triethoxysilane |
| CN107942414A (en) * | 2017-12-27 | 2018-04-20 | 福建农林大学 | A kind of bottom is the double-deck wideband anti-reflection film of organic inorganic hybridization film |
| CN107942414B (en) * | 2017-12-27 | 2019-10-29 | 福建农林大学 | A kind of bottom is the double-deck wideband anti-reflection film of organic-inorganic hybrid film |
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Application publication date: 20170510 |