CN106752627A - A kind of preparation method and applications of silicon-based hybrid material coating - Google Patents
A kind of preparation method and applications of silicon-based hybrid material coating Download PDFInfo
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- CN106752627A CN106752627A CN201611131157.3A CN201611131157A CN106752627A CN 106752627 A CN106752627 A CN 106752627A CN 201611131157 A CN201611131157 A CN 201611131157A CN 106752627 A CN106752627 A CN 106752627A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
- C09D151/08—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/12—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes
- C08F283/124—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes on to polysiloxanes having carbon-to-carbon double bonds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/11—Anti-reflection coatings
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/18—Coatings for keeping optical surfaces clean, e.g. hydrophobic or photo-catalytic films
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Abstract
The invention belongs to organic-inorganic nano hybrid composite material field, more particularly to a kind of preparation method and applications of silicon-based hybrid material coating.The invention provides a kind of preparation method of silicon-based hybrid material coating, it is：The mixing of step one, phenyltrimethoxysila,e and methyl allyl acyloxypropyl trimethoxysilane, is dissolved in solvent, stirs to obtain the first product；Step 2, the first product mix with phenoxyethyl acrylate and light trigger, obtain the second product；Step 3, the second product are layered on substrate, solidify to obtain product.A kind of application of the product obtained present invention also offers above-mentioned preparation method in optical coating art.Obtained product of the invention, surface forms the fold of size uniformity, the performance of micro-nano fexible film device can be tuned using microcosmic fold, and antireflection, the anti-fog and self-cleaning function material of optics for building environmental protection glass, liquid crystal display, solar cell and all kinds of optoelectronic devices may finally be applied to, have a extensive future.
Description
Technical field
The invention belongs to organic-inorganic nano hybrid composite material field, more particularly to a kind of silicon-based hybrid material coating
Preparation method and applications.
Background technology
Unnecessary light reflection can cause such as optical glass, liquid crystal display and camera lens to produce " ghost ", spuious
Optical phenomenon, and solar cell and the low problem of photovoltaic device light energy conversion efficiency.In urban construction, optical glass is used to
Used as building curtain wall, but due to the presence of light reflection, cause light pollution, given people life and bring puzzlement inconvenience.
Moreover, the cleaning of glass curtain wall takes and labor intensive material resources.Equally, mobile phone, camera and liquid crystal display screen are past
It is past that the phenomenons such as glare, veiling glare occur so that the visual experience of people is had a greatly reduced quality.Another important directions, solar energy
Cell power generation has obtained the support energetically of national governments as a kind of clean energy resource.Unit group important in solar energy utilization system
It is solar energy glass cover plate into part, solar energy glass cover plate easily causes various problems in complicated external environment, such as ash
Dustiness contaminates, glass surface easily atomization etc..
Fold is a kind of natural phenomena being widely present, and the skin from mountains and rivers landforms to animals and plants is ubiquitous.Fold is very
Already recognized by the mankind, but research work has been focused into negative effect aspect, and the appearance of such as fold imply that Ministry of worker's part
Fatigue and fracture.In recent years, it has been realized that fold inhales ripple or anti-on flexible electronic, surface optical element, surface
Penetrating the aspects such as structure has huge potential use.The folding of such as different scale film surface is different.Macro-scale is thin
Negative interaction is played the fold on film surface, such as the fold on high-precision large space membrane structure surface more, its shape will be directly affected
The dynamic characteristics of face precision, load transmission and structure.Conversely, positive interaction is played the fold on micro/nano film surface more, such as
The flexible solar battery that polyester film is made, the microcosmic fold on its surface can increase the generated energy of battery, significantly improve too
The power output of positive energy battery；The microcosmic fold of graphenic surface, can change the conductance of material, influence material translucency and
Scattered power.
The method for generating fold mainly has two kinds, plavini and outer force method, and plavini includes thermal induction and solvent-induced, outward
Force method includes stretching and compresses.Ordinary circumstance, in the system of flexible subserate dura mater, the choice of dura mater is than larger, Hen Duowu
Machine film, polymer film, metal etc. can serve as its material.The technique for preparing flexible subserate dura mater system can be divided into from mechanism
Physical method and chemical method, the metalloid such as gold, silver and bronze material and oxygen are prepared frequently with being evaporated in vacuo with the method for sputtering sedimentation
Compound dura mater.But for some high polymers, the modified method in surface is relatively conventional.Other situations, are similar to viscosity
Film, can as needed combine physical method and chemical method.But, efficiently prepare with scale pleated pattern material list
The method in face still needs further development badly.Ultraviolet light polymerization is a kind of technological means of highly effective.In addition, silsesquioxane
Used as a kind of organosilicon functional compounds, with good heat-resistant stability, mechanical strength and compatibility, its chemical constitution can root
According to needing to carry out MOLECULE DESIGN with synthesis.
Therefore, a kind of preparation method and applications of silicon-based hybrid material coating are developed, can be adjusted using microcosmic fold
The performance of humorous micro-nano fexible film device, and optics environmental protection glass for building, liquid crystal display, the sun may finally be applied to
Antireflection, the anti-fog and self-cleaning function material of energy battery and all kinds of optoelectronic devices, have a extensive future.
The content of the invention
In view of this, the invention provides a kind of preparation method and applications of silicon-based hybrid material coating, using microcosmic
Fold can tune the performance of micro-nano fexible film device, and may finally be applied to optics environmental protection glass for building, liquid crystal
Display, the antireflection of solar cell and all kinds of optoelectronic devices, anti-fog and self-cleaning function material.
The invention provides a kind of preparation method of silicon-based hybrid material coating, the preparation method is：
The mixing of step one, phenyltrimethoxysila,e and methyl allyl acyloxypropyl trimethoxysilane, is dissolved in solvent,
Stir to obtain the first product；
Step 2, first product mix with phenoxyethyl acrylate and light trigger, obtain the second product；
Step 3, second product are layered on substrate, solidify to obtain product.
Preferably, in terms of molar part, the phenyltrimethoxysila,e and methyl allyl acyloxypropyl trimethoxysilane
Rate of charge (1-9):(9~1).
Preferably, the solvent is selected from：One or more in tetrahydrofuran, dichloromethane and chloroform.
Preferably, the step one is carried out under conditions of nitrogen protection, and the whipping temp described in step one is room temperature, step
The time stirred described in rapid one is 12~72h.
Preferably, the step one also needs the potassium carbonate and water of addition.
Preferably, in terms of molar part, the rate of charge of first product, phenoxyethyl acrylate and light trigger is
(1~5):(98~94):1.
Preferably, the light trigger is selected from：One kind in benzophenone, benzoin dimethylether and Irgacure-184 or
It is various.
Preferably, the substrate is glass chip bottom, and the method for the solidification is ultraviolet light polymerization.
Preferably, a length of 200~400nm of the ultraviolet light wave of the ultraviolet light polymerization, the time of the ultraviolet light polymerization is
40~180s.
Led in optical coating present invention also offers a kind of product obtained including one preparation method of any of the above
The application in domain.
In sum, the invention provides a kind of preparation method of silicon-based hybrid material coating, the preparation method is：Step
Rapid one, phenyltrimethoxysila,e and methyl allyl acyloxypropyl trimethoxysilane mix, and are dissolved in solvent, stir first
Product；Step 2, first product mix with phenoxyethyl acrylate and light trigger, obtain the second product；Step 3,
Second product is layered on substrate, solidifies to obtain product.The product obtained present invention also offers a kind of above-mentioned preparation method is in light
Learn the application of coatings art.Can be obtained through measuring, the obtained product of the present invention, surface forms the fold of size uniformity, profit
The performance of micro-nano fexible film device can be tuned with microcosmic fold, and optics environmental protection glass for building may finally be applied to
The antireflection of glass, liquid crystal display, solar cell and all kinds of optoelectronic devices, anti-fog and self-cleaning function material.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
The accompanying drawing to be used needed for having technology description is briefly described, it should be apparent that, drawings in the following description are only this
Inventive embodiment, for those of ordinary skill in the art, on the premise of not paying creative work, can also basis
The accompanying drawing of offer obtains other accompanying drawings.
A kind of preparation principle schematic diagram of the preparation method of silicon-based hybrid material coating that Fig. 1 is provided for the present invention；
Fig. 2 is sample optical reflectivity prepared by embodiment 3 and transmission measurement result.
Specific embodiment
The invention provides a kind of preparation method and applications of silicon-based hybrid material coating, can be adjusted using microcosmic fold
The performance of humorous micro-nano fexible film device, and optics environmental protection glass for building, liquid crystal display, the sun may finally be applied to
Antireflection, the anti-fog and self-cleaning function material of energy battery and all kinds of optoelectronic devices.
The technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, this area is common
The every other embodiment that technical staff is obtained under the premise of creative work is not made, belongs to the model of present invention protection
Enclose.
In order to the present invention is described in more detail, with reference to a kind of silicon-based hybrid material coating that embodiment is provided the present invention
Preparation method and applications, be specifically described.
Embodiment 1
The present embodiment is the specific embodiment that product 1 is prepared using above-mentioned preparation method.
Weigh 0.24mol phenyltrimethoxysila,es, 0.16mol methyl allyl acyloxypropyl trimethoxysilanes and 0.2g
Potassium carbonate mixes, and 2ml distilled water is added to mixed system, is dissolved in 40ml solvents tetrahydrofuranes, and 24h is stirred under room temperature condition,
Obtain the first product 1.In this step, stirring is carried out under conditions of nitrogen protection.
According to 3:96:1 mass ratio, weighs the first products of 0.3g 1,9.6g phenoxyethyl acrylates and 0.1g is light-initiated
Agent mixes, and obtains the second product 1.In this step, light trigger is Irgacure-184.
Second product 1 spreads on the glass substrate, with the ultraviolet light polymerization 80s that wavelength is 365nm, obtains product 1.
With the surface texture of electron microscope observation product 1, product 1 can be observed and forms fold group flower surface, gained
The size of fold is more homogeneous.Scanned electron microscope observation and dimension analysis measurement can be obtained, the size statistic of the fold of product 1
Average data is 31 ± 1nm.
Embodiment 2
The present embodiment is the specific embodiment that product 2 is prepared using above-mentioned preparation method.
Weigh 0.16mol phenyltrimethoxysila,es, 0.24mol methyl allyl acyloxypropyl trimethoxysilanes and 0.2g
Potassium carbonate mixes, and 2ml distilled water is added to mixed system, is dissolved in 40ml solvents tetrahydrofuranes, and 24h is stirred under room temperature condition,
Obtain the first product 2.In this step, stirring is carried out under conditions of nitrogen protection.
According to 2:97:1 mass ratio, weighs the first products of 0.2g 2,9.7g phenoxyethyl acrylates and 0.1g is light-initiated
Agent mixes, and obtains the second product 2.In this step, light trigger is Irgacure-184.
Second product 1 spreads on the glass substrate, with the ultraviolet light polymerization 80s that wavelength is 365nm, obtains product 1.
With the surface texture of electron microscope observation product 2, product 2 can be observed and forms fold group flower surface, gained
The size of fold is more homogeneous.Scanned electron microscope observation and dimension analysis measurement can be obtained, the size statistic of the fold of product 2
Average data is 24 ± 1nm.
Embodiment 3
The present embodiment is the specific embodiment that product 3 is prepared using above-mentioned preparation method.
Weigh 0.24mol phenyltrimethoxysila,es, 0.16mol methyl allyl acyloxypropyl trimethoxysilanes and 0.2g
Potassium carbonate mixes, and 2ml distilled water is added to mixed system, is dissolved in 40ml solvents tetrahydrofuranes, and 24h is stirred under room temperature condition,
Obtain the first product 3.In this step, stirring is carried out under conditions of nitrogen protection.
According to 1:98:1 mass ratio, weighs the first products of 0.1g 3,9.8g phenoxyethyl acrylates and 0.1g is light-initiated
Agent mixes, and obtains the second product 3.In this step, light trigger is Irgacure-184.
Second product 3 spreads on the glass substrate, with the ultraviolet light polymerization 80s that wavelength is 365nm, obtains product 3.
With the surface texture of electron microscope observation product 3, product 3 can be observed and forms fold group flower surface, gained
The size of fold is more homogeneous.Scanned electron microscope observation and dimension analysis measurement can be obtained, the size statistic of the fold of product 1
Average data is 28 ± 1nm.
Fig. 2 reflectivity and light transmittance test result show, the product can by the light transmittance of glass substrate by 92% carry to
98%, reflectivity is down to 3% by 8%, with the excellent anti-reflection performance of antireflection, can be in optics building glass and solar energy
Field of batteries is applied.
Embodiment 4
The present embodiment is the specific embodiment that product 4 is prepared using above-mentioned preparation method.
Weigh 0.36mol phenyltrimethoxysila,es, 0.04mol methyl allyl acyloxypropyl trimethoxysilanes and 0.2g
Potassium carbonate mixes, and 2ml distilled water is added to mixed system, is dissolved in 40ml solvents tetrahydrofuranes, and 24h is stirred under room temperature condition,
Obtain the first product 4.In this step, stirring is carried out under conditions of nitrogen protection.
According to 5:94:1 mass ratio, weighs the first products of 0.5g 4,9.4g phenoxyethyl acrylates and 0.1g is light-initiated
Agent mixes, and obtains the second product 4.In this step, light trigger is Irgacure-184.
Second product 1 spreads on the glass substrate, with the ultraviolet light polymerization 80s that wavelength is 365nm, obtains product 4.
Embodiment 5
The present embodiment is the specific embodiment that product 4 is prepared using above-mentioned preparation method.
Weigh 0.32mol phenyltrimethoxysila,es, 0.08mol methyl allyl acyloxypropyl trimethoxysilanes and 0.2g
Potassium carbonate mixes, and 2ml distilled water is added to mixed system, is dissolved in 40ml solvents tetrahydrofuranes, and 24h is stirred under room temperature condition,
Obtain the first product 5.In this step, stirring is carried out under conditions of nitrogen protection.
According to 4:95:1 mass ratio, weighs the first products of 0.4g 5,9.5g phenoxyethyl acrylates and 0.1g is light-initiated
Agent mixes, and obtains the second product 5.In this step, light trigger is Irgacure-184.
Second product 1 spreads on the glass substrate, with the ultraviolet light polymerization 80s that wavelength is 365nm, obtains product 5.
In sum, the invention provides a kind of preparation method of silicon-based hybrid material coating, the preparation method is：Step
Rapid one, phenyltrimethoxysila,e and methyl allyl acyloxypropyl trimethoxysilane mix, and are dissolved in solvent, stir first
Product；Step 2, first product mix with phenoxyethyl acrylate and light trigger, obtain the second product；Step 3,
Second product is layered on substrate, solidifies to obtain product.The product obtained present invention also offers a kind of above-mentioned preparation method is in light
Learn the application of coatings art.Can be obtained through measuring, the obtained product of the present invention, surface forms the fold of size uniformity, profit
The performance of micro-nano fexible film device can be tuned with microcosmic fold, and optics environmental protection glass for building may finally be applied to
The antireflection of glass, liquid crystal display, solar cell and all kinds of optoelectronic devices, anti-fog and self-cleaning function material.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of silicon-based hybrid material coating, it is characterised in that the preparation method is：
The mixing of step one, phenyltrimethoxysila,e and methyl allyl acyloxypropyl trimethoxysilane, is dissolved in solvent, stirs
Obtain the first product；
Step 2, first product mix with phenoxyethyl acrylate and light trigger, obtain the second product；
Step 3, second product are layered on substrate, solidify to obtain product.
2. preparation method according to claim 1, it is characterised in that in terms of molar part, the phenyltrimethoxysila,e
It is (1~9) with the rate of charge of methyl allyl acyloxypropyl trimethoxysilane:(9~1).
3. preparation method according to claim 1, it is characterised in that the solvent is selected from：Tetrahydrofuran, dichloromethane and
One or more in chloroform.
4. preparation method according to claim 1, it is characterised in that the step one is entered under conditions of nitrogen protection
OK, the whipping temp described in step one is room temperature, and the time of stirring described in step one is 12~72h.
5. preparation method according to claim 1, it is characterised in that the step one also needs the potassium carbonate and water of addition.
6. preparation method according to claim 1, it is characterised in that in terms of mass parts, first product, phenoxy group second
The rate of charge of base acrylate and light trigger is (1~5):(98~94):1.
7. preparation method according to claim 1, it is characterised in that the light trigger is selected from：Benzophenone, styrax
One or more in double methyl ethers and Irgacure-184.
8. preparation method according to claim 1, it is characterised in that the substrate is glass chip bottom, the solidification
Method is ultraviolet light polymerization.
9. preparation method according to claim 8, it is characterised in that the ultraviolet light wave a length of 200 of the ultraviolet light polymerization
~400nm, the time of the ultraviolet light polymerization is 40~180s.
10. a kind of product obtained including preparation method described in claim 1 to 9 any one in optical coating art should
With.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111978545A (en) * | 2020-09-10 | 2020-11-24 | 江西星火狮达科技有限公司 | Special waterproof and mildewproof resin for wood and preparation method thereof |
| WO2022022728A1 (en) * | 2020-07-31 | 2022-02-03 | 华为技术有限公司 | Patterning material and patterned film |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015190729A1 (en) * | 2014-06-13 | 2015-12-17 | (주)엘지하우시스 | High-refractive composition, anti-reflective film and production method thereof |
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- 2016-12-09 CN CN201611131157.3A patent/CN106752627B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015190729A1 (en) * | 2014-06-13 | 2015-12-17 | (주)엘지하우시스 | High-refractive composition, anti-reflective film and production method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022022728A1 (en) * | 2020-07-31 | 2022-02-03 | 华为技术有限公司 | Patterning material and patterned film |
| CN111978545A (en) * | 2020-09-10 | 2020-11-24 | 江西星火狮达科技有限公司 | Special waterproof and mildewproof resin for wood and preparation method thereof |
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