CN108238727A - The preparation method of earth silicon/titanic oxide nano-array antireflective coating - Google Patents
The preparation method of earth silicon/titanic oxide nano-array antireflective coating Download PDFInfo
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- CN108238727A CN108238727A CN201611216676.XA CN201611216676A CN108238727A CN 108238727 A CN108238727 A CN 108238727A CN 201611216676 A CN201611216676 A CN 201611216676A CN 108238727 A CN108238727 A CN 108238727A
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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
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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
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
-
- 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
- C03C2217/23—Mixtures
-
- 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
- C03C2217/40—Coatings comprising at least one inhomogeneous layer
- C03C2217/42—Coatings comprising at least one inhomogeneous layer consisting of particles only
-
- 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
- C03C2217/73—Anti-reflective coatings with specific characteristics
-
- 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
- C03C2217/76—Hydrophobic and oleophobic 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
-
- 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
Abstract
The invention discloses a kind of preparation methods of earth silicon/titanic oxide nano-array antireflective coating, include the following steps：(1) silica suspension is prepared using silica dioxide granule and absolute ethyl alcohol；(2) substrate of glass after cleaning is lifted, and made annealing treatment to obtain coarse membrana granulosa in silica suspension with certain rate of pulling；(3) using containing TiCl3Dilute hydrochloric acid solution, sodium chloride be mixed with saturation NaCl solution；(4) gained membrana granulosa slant setting is taken out after reacting a period of time in saturation NaCl solution, carrying out hydro-thermal reaction at a certain temperature, obtains the compound nano-wire array antireflective coating of earth silicon/titanic oxide.The structure of earth silicon/titanic oxide nano-wire array antireflective coating prepared by the present invention is the nano-array that single vertical nano wire is formed, with class lotus leaf and class moth eye surface pyramidal structure, the transmitance of the antireflective coating is high, hydrophobic and oleophobic contact angle is big, has excellent self-cleaning function.
Description
Technical field
The present invention relates to a kind of preparation methods of earth silicon/titanic oxide nano-array antireflective coating, belong to antireflective
Technical field of membrane.
Background technology
The antireflective coating glass used at present is generally all exposed in air, needs to be subjected to expose to the sun and rain, the evils such as high humility
The test of bad natural environment.Therefore antireflective coating also needs to reach self-cleaning performance under high transmittance requirement.It uses at present
Antireflective coating transmitance prepared by sol-gal process is high, but particle surface can be accompanied by a large amount of polar hydroxyl groups, easily inhale
Attached surface moisture and dirt cause glass surface to be difficult to keep the state of high transmittance, have violated the use original intention of antireflective coating.
Film layer is essentially consisted in super-hydrophobicity and oleophobic performance for the realization of self-cleaning function at present.Specific technology
There are two types of methods.The first is the modification that hydrophobization or oleophobic are carried out to film layer.Second of post processing skill for film layer
Art by way of being heat-treated after the heat treatment or immersion under certain atmosphere, improves the internal structure of film layer, reduces water suction and inhales
The probability of oil.The both of which is extremely difficult to while hydrophobic and oleophobic effect, and is improved by surface modification and located afterwards
The film layer of reason technological improvement under routine use environment over time, easily damage and fail by film layer, it is difficult to keep certainly
Cleaning effect.
To improve the self-cleaning performance of antireflective coating.By the way of surface roughening, lotus leaf and insect eyes are imitated
Hydrophobic mechanism, preferable hydrophobic and oleophobic effects can be played.Shaggy method is obtained at present to carve usually using ion
The method of erosion, ion etching can prepare nano dot, cone and line of marshalling etc. in film surface, can be good at increasing
Hydrophobic and oleophobic contact angle, but this method cost is very high, is only applicable in laboratory, for the preparation of scientific research and testing sample.
Invention content
The more than prior art is based on, the purpose of the present invention is to provide a kind of earth silicon/titanic oxide nano-arrays to subtract
The preparation method of reflectance coating arranges consistent, transmitance height, with super thin using the nano-array of antireflective coating prepared by this method
Aqueous and superoleophobic property, good weatherability.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of earth silicon/titanic oxide nano-array antireflective coating, includes the following steps：
(1) silica suspension is prepared using silica dioxide granule and absolute ethyl alcohol；
(2) substrate of glass after cleaning in the silica suspension with certain rate of pulling is lifted, gone forward side by side
Row annealing obtains coarse membrana granulosa；
(3) using containing TiCl3Dilute hydrochloric acid solution, sodium chloride be mixed with saturation NaCl solution；
(4) in the saturation NaCl solution for preparing the membrana granulosa slant setting prepared in step (2) in step (3), one
Determine to carry out hydro-thermal reaction at temperature, taken out after reacting a period of time, obtain the compound nano-wire array of earth silicon/titanic oxide
Antireflective coating.
Wherein, in the step (1), the average particle size of silica dioxide granule is 5-30nm.Titanium dioxide in the suspension
Silicon and absolute ethyl alcohol weight ratio are 1: 100-1: 200.
In the step (2), rate of pulling 1-5cm/min, annealing temperature is 300-600 DEG C.
Contain TiCl in the step (3)3Dilute hydrochloric acid solution in TiCl3∶HCl∶H2O molar ratios are 0.03-0.13: 0.02-
0.14∶4.1-5.2。
Hydrothermal temperature in the step (4) is 50-100 DEG C, the hydro-thermal reaction time 1-2h.
The film layer structure of the antireflective coating is the nano-array that single vertical nano wire is formed, and nano-wire array height is
100-200nm, line spacing are 5-50nm.
The substrate of glass is plate glass or tubular glass, and the cleaning method of the substrate of glass is：First using going
Ionized water and cleaning agent for electronic industry clean glass surface to glass surface without dirt；Secondly the glass that washing process is crossed is put
Enter in absolute ethyl alcohol and acetone, each 30min of ultrasonic cleaning.
The method that the present invention prepares nano-oxide array using the ripe hydro-thermal of current technique, prepares titanium dioxide
The nano-wire array of silicon/titanium dioxide, it is neat, high transmittance which can adjust acquisition surface according to process conditions
Class lotus leaf and class moth eye surface pyramidal structure.The class pyramidal structure on surface has superoleophobic and super-hydrophobic self-cleaning performance；Film
Layer is formed by stacking by silica and titanium dioxide, has broad-band transparence-increased effect, and therefore, the transmitance of antireflective coating is high, thin
Water and oleophobic contact angle are big, have excellent self-cleaning function.
Specifically, the present invention is used as the kind of nano-wire array by depositing silica dioxide granule film on the glass substrate
Son can achieve the effect that broad-band transparence-increased after silica and titanium dioxide are compound.After hydro-thermal reaction, silica/titanium dioxide
Titanium is in composite Nano linear array structure, and nano wire is arranged vertically, marshalling, nano wire gap uniformity.Pass through hydro-thermal reaction
The diameter and length of the vertical nano-wire of time and temperature control nano-wire array.Control length meets the film of antireflective coating needs
Layer thickness requirement, passes through the refractive index of diameter and clearance control antireflective coating.Suitable nanowire height, diameter and gap make to subtract
Reflectance coating has high transmitance.The surface texture of nano-wire array is class lotus leaf and class moth eye surface pyramidal structure, is had super
Hydrophobicity and superoleophobic property.
The advantage of the invention is that：
The glass for being coated with antireflective coating prepared by the method for the present invention is average saturating in 250-2500nm spectral regions
The bare glass that rate is crossed than no plated film increases 3~5%.The color of the glass surface antireflection film of preparation is according to nano-array height
It can be light blue, light blue violet and pale purple coppery to spend (thicknesses of layers) difference, can effectively improve solar thermal collector, photovoltaic group
The sun light transmission rate of part etc., the efficiency of solar energy utilization can be significantly improved.Antireflective coating outdoor environment prepared by the present invention
One annual aging test and the environmental experiment of steady damp heat 48 hours (GB-T2423.3-2006) after, transmitance changing value is less than
0.5%.Prepared glass antireflective coating oil contact angle and water contact angle are more than 150 °.Illustrate that the antireflective coating has automatically cleaning
Function, which can be widely applied to the fields such as solar energy glass, building glass and touched panel glass.
Specific embodiment
With reference to embodiment, the embodiment of the present invention is furthur described in detail.
Embodiment 1
It will be put into absolute ethyl alcohol and acetone after sheet or tubular glass wash clean first and carry out being ultrasonically treated each 30min,
The glass sample cleaned up is dried；
The silica dioxide granule that 2g average particle sizes are 5nm is placed in 200g absolute ethyl alcohols and prepares silica dioxide granule suspension
Liquid；
Glass is slowly lifted from silica-particle suspension with 1cm/min rates, after the completion of lifting at 300 DEG C
It anneals, prepares shaggy silica dioxide granule film；
TiCl3∶HCl∶H2The solution that O molar ratios are 0.03: 0.02: 4.1 adds in NaCl until saturation, and solution is put
In reaction kettle, and the silica dioxide granule film inclination prepared is placed in solution, continues 1h at 50 DEG C；
The sample of preparation using deionized water is rinsed, obtains earth silicon/titanic oxide nano-wire array antireflective coating,
Linear array height is about 100nm, and line spacing is 5nm.By detection, the antireflective coating that the present embodiment obtains is in 250-2500nm spectrum
In the range of mean transmissivity reach 96%.With 5 samples are prepared under embodiment, sample average transmitance phase difference is 0.1%.It dredges
Oily contact angle is 155 °, and hydrophobic contact angle is 162 °.
Embodiment 2
It will be put into absolute ethyl alcohol and acetone after sheet or tubular glass wash clean first and carry out being ultrasonically treated each 30min,
The glass sample cleaned up is dried；
The silica dioxide granule that 2g average particle sizes are 30nm is placed in and prepares silica dioxide granule in 200g absolute ethyl alcohols and hangs
Supernatant liquid；
Glass is slowly lifted from silica-particle suspension with 5cm/min rates, after the completion of lifting at 600 DEG C
It anneals, prepares shaggy silica dioxide granule film；
TiCl3∶HCl∶H2The solution that O molar ratios are 0.10: 0.12: 4.9 adds in NaCl until saturation, and solution is put
In reaction kettle, and the silica dioxide granule film inclination prepared is placed in solution, continues 2h at 100 DEG C；
The sample of preparation using deionized water is rinsed, obtains earth silicon/titanic oxide nano-wire array antireflective coating,
Linear array height is about 120nm, and line spacing is 10nm.By detection, the antireflective coating that the present embodiment obtains is in 250-2500nm light
Mean transmissivity reaches 96% in spectral limit.With 5 samples are prepared under embodiment, sample average transmitance phase difference is 0.3%.
Oleophobic contact angle is 152 °, and hydrophobic contact angle is 164 °.
Embodiment 3
It will be put into absolute ethyl alcohol and acetone after sheet or tubular glass wash clean first and carry out being ultrasonically treated each 30min,
The glass sample cleaned up is dried；
The silica dioxide granule that 1.5g average particle sizes are 15nm is placed in 150g absolute ethyl alcohols and prepares silica dioxide granule
Suspension；
Glass is slowly lifted from silica-particle suspension with 3cm/min rates, after the completion of lifting at 450 DEG C
It anneals, prepares shaggy silica dioxide granule film；
TiCl3∶HCl∶H2The solution that O molar ratios are 0.05: 0.12: 4.3 adds in NaCl until saturation, and solution is put
In reaction kettle, and the silica dioxide granule film inclination prepared is placed in solution, continues 1.5h at 75 DEG C；
The sample of preparation using deionized water is rinsed, obtains earth silicon/titanic oxide nano-wire array antireflective coating,
Linear array height is about 150nm, and line spacing is 20nm.By detection, the antireflective coating that the present embodiment obtains is in 250-2500nm light
Mean transmissivity reaches 96% in spectral limit.With 5 samples are prepared under embodiment, sample average transmitance phase difference is 0.1%.
Oleophobic contact angle is 157 °, and hydrophobic contact angle is 158 °.
Embodiment 4
It will be put into absolute ethyl alcohol and acetone after sheet or tubular glass wash clean first and carry out being ultrasonically treated each 30min,
The glass sample cleaned up is dried；
The silica dioxide granule that 1g average particle sizes are 20nm is placed in and prepares silica dioxide granule in 100g absolute ethyl alcohols and hangs
Supernatant liquid；
Glass is slowly lifted from silica-particle suspension with 3cm/min rates, after the completion of lifting at 500 DEG C
It anneals, prepares shaggy silica dioxide granule film；
TiCl3∶HCl∶H2The solution that O molar ratios are 0.06: 0.08: 4.7 adds in NaCl until saturation, and solution is put
In reaction kettle, and the silica dioxide granule film inclination prepared is placed in solution, continues 1.8h at 75 DEG C；
The sample of preparation using deionized water is rinsed, obtains earth silicon/titanic oxide nano-wire array antireflective coating,
Linear array height is about 170nm, and line spacing is 25nm.By detection, the antireflective coating that the present embodiment obtains is in 250-2500nm light
Mean transmissivity reaches 96% in spectral limit.With 5 samples are prepared under embodiment, sample average transmitance phase difference is 0.1%.
Oleophobic contact angle is 158 °, and hydrophobic contact angle is 168 °.
Embodiment 5
It will be put into absolute ethyl alcohol and acetone after sheet or tubular glass wash clean first and carry out being ultrasonically treated each 30min,
The glass sample cleaned up is dried；
The silica dioxide granule that 2g average particle sizes are 5nm is placed in 200g absolute ethyl alcohols and prepares silica dioxide granule suspension
Liquid；
Glass is slowly lifted from silica-particle suspension with 1cm/min rates, after the completion of lifting at 300 DEG C
It anneals, prepares shaggy silica dioxide granule film；
TiCl3∶HCl∶H2The solution that O molar ratios are 0.13: 0.14: 5.2 adds in NaCl until saturation, and solution is put
In reaction kettle, and the silica dioxide granule film inclination prepared is placed in solution, continues 1h at 100 DEG C；
The sample of preparation using deionized water is rinsed, obtains earth silicon/titanic oxide nano-wire array antireflective coating,
Linear array height is about 200m, and line spacing is 50nm.By detection, the antireflective coating that the present embodiment obtains is in 250-2500nm spectrum
In the range of mean transmissivity reach 96%.With 5 samples are prepared under embodiment, sample average transmitance phase difference is 0.1%.It dredges
Oily contact angle is 151 °, and hydrophobic contact angle is 152 °.
Embodiment described above only expresses the several embodiments of the present invention, and description is more specific and detailed, but simultaneously
Cannot limiting the scope of the invention therefore be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect range.Therefore, protection scope of the present invention should be determined by the appended claims.
Claims (8)
1. a kind of preparation method of earth silicon/titanic oxide nano-array antireflective coating, includes the following steps：
(1) silica suspension is prepared using silica dioxide granule and absolute ethyl alcohol；
(2) substrate of glass after cleaning is lifted, and moved back in the silica suspension with certain rate of pulling
Fire processing obtains coarse membrana granulosa；
(3) using containing TiCl3Dilute hydrochloric acid solution, sodium chloride be mixed with saturation NaCl solution；
(4) in the saturation NaCl solution for preparing the membrana granulosa slant setting prepared in step (2) in step (3), in a constant temperature
Degree is lower to carry out hydro-thermal reaction, is taken out after reacting a period of time, obtains the compound nano-wire array anti-reflection of earth silicon/titanic oxide
Penetrate film.
2. preparation method according to claim 1, which is characterized in that in the step (1), silica dioxide granule is put down
Equal granularity is 5-30nm.
3. preparation method according to claim 1, which is characterized in that silica and absolute ethyl alcohol weight in the suspension
Amount is than being 1: 100-1: 200.
4. preparation method according to claim 1, which is characterized in that in the step (2), rate of pulling 1-5cm/
Min, annealing temperature are 300-600 DEG C.
5. preparation method according to claim 1, which is characterized in that contain TiCl in the step (3)3Dilute hydrochloric acid solution
Middle TiCl3∶HCl∶H2O molar ratios are 0.03-0.13: 0.02-0.14: 4.1-5.2..
6. preparation method according to claim 1, which is characterized in that the hydrothermal temperature in the step (4) is 50-
100 DEG C, the hydro-thermal reaction time 1-2h.
7. preparation method according to claim 1, which is characterized in that the film layer structure of the antireflective coating is single vertical
The nano-array that nano wire is formed, nano-wire array height are 100-200nm, and line spacing is 5-50nm.
8. preparation method according to claim 1, which is characterized in that the substrate of glass is plate glass or tubulose glass
Glass.
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| CN201611216676.XA CN108238727B (en) | 2016-12-23 | 2016-12-23 | Preparation method of silicon dioxide/titanium dioxide nano array antireflection film |
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Citations (5)
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|---|---|---|---|---|
| CN1289724A (en) * | 2000-10-16 | 2001-04-04 | 南京大学 | Ordinary-temp hydrolysis process for synthesizing nm-class rutile-type TiO2 with high specific surface area from TiCl4 |
| CN101649483A (en) * | 2008-08-12 | 2010-02-17 | 中国科学院理化技术研究所 | Method for preparing titanium dioxide nanorod array film |
| CN102532960A (en) * | 2010-12-30 | 2012-07-04 | 中国科学院理化技术研究所 | Reflection/transmittanceimproving coating and preparation method thereof |
| CN102951848A (en) * | 2011-08-29 | 2013-03-06 | 中国科学院理化技术研究所 | Preparation method of anti-reflection coating |
| CN103482885A (en) * | 2013-07-23 | 2014-01-01 | 北京纳琦环保科技有限公司 | Processing method for sintering and film-formation of self-cleaning glass with photocatalytic performance |
-
2016
- 2016-12-23 CN CN201611216676.XA patent/CN108238727B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1289724A (en) * | 2000-10-16 | 2001-04-04 | 南京大学 | Ordinary-temp hydrolysis process for synthesizing nm-class rutile-type TiO2 with high specific surface area from TiCl4 |
| CN101649483A (en) * | 2008-08-12 | 2010-02-17 | 中国科学院理化技术研究所 | Method for preparing titanium dioxide nanorod array film |
| CN102532960A (en) * | 2010-12-30 | 2012-07-04 | 中国科学院理化技术研究所 | Reflection/transmittanceimproving coating and preparation method thereof |
| CN102951848A (en) * | 2011-08-29 | 2013-03-06 | 中国科学院理化技术研究所 | Preparation method of anti-reflection coating |
| CN103482885A (en) * | 2013-07-23 | 2014-01-01 | 北京纳琦环保科技有限公司 | Processing method for sintering and film-formation of self-cleaning glass with photocatalytic performance |
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