CN106752627B - 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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- CN106752627B CN106752627B CN201611131157.3A CN201611131157A CN106752627B CN 106752627 B CN106752627 B CN 106752627B CN 201611131157 A CN201611131157 A CN 201611131157A CN 106752627 B CN106752627 B CN 106752627B
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- 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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- C08F283/12—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes
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- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
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- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
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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 present invention provides a kind of preparation method of silicon-based hybrid material coating, are as follows: Step 1: phenyltrimethoxysila,e and methyl allyl acyloxypropyl trimethoxysilane mixing, are dissolved in solvent, stir to obtain the first product；Step 2: the first product is mixed with phenoxyethyl acrylate and photoinitiator, the second product is obtained；Step 3: the second product is layered on substrate, solidify to obtain product.The present invention also provides a kind of product that above-mentioned preparation method obtains optical coating art application.Product produced by the present 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 environmental protection glass for building, liquid crystal display, solar battery and all kinds of optoelectronic devices may finally be applied to, it has 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 coatings
Preparation method and applications.
Background technique
The reflection of unnecessary light will cause such as optical glass, liquid crystal display and camera lens generate " ghost ", spuious
The problems such as optical phenomenon and solar battery low with photovoltaic device light energy conversion efficiency.In urban construction, optical glass is used to
It is used as building curtain wall, but due to the presence of light reflection, causes light pollution, it is inconvenient to bring puzzlement to people's life.
Moreover, the cleaning of glass curtain wall is time-consuming and spends human and material resources.Equally, mobile phone, camera and liquid crystal display screen are past
Past phenomena such as will appear glare, stray light, 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.Important unit group in solar energy utilization system
At being partially solar energy glass cover board, solar energy glass cover board easily causes various problems in complicated external environment, such as grey
Dustiness contaminates, and glass surface is easily atomized 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, as the appearance of fold implies Ministry of worker's part
Fatigue and fracture.In recent years, it has been realized that fold inhales wave or anti-on flexible electronic, surface optical element, surface
Penetrating structure etc. has huge potential use.Such as the folding of different scale film surface is different.Macro-scale is thin
The fold of film surface is multiple to wave negative interaction, such as the fold on high-precision large space membrane structure surface, will directly affect its shape
The dynamic characteristics of face precision, load transmission and structure.On the contrary, the fold on micro/nano film surface is multiple to wave positive interaction, such as
Flexible solar battery made of polyester film, the microcosmic fold on surface can increase the generated energy of battery, significantly improve too
The output power of positive energy battery；The microcosmic fold of graphene surface, can be changed material conductivity, influence material translucency and
Scattered power.
There are mainly two types of the methods for generating fold, plavini and outer force method, and plavini includes thermal induction and solvent-induced, outside
Force method includes stretching and compressing.Ordinary circumstance, in the system of flexible subserate dura mater, the choice of dura mater is bigger, Hen Duowu
Machine film, polymer film, metal etc. all 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 prepare the metalloids such as gold, silver and bronze material and oxygen with the method for sputtering sedimentation frequently with being evaporated in vacuo
Compound dura mater.But for some high polymers, the modified method in surface is relatively conventional.Other situations, similar viscosity
Film can according to need in conjunction with physical method and chemical method.But efficiently prepare with scale pleated pattern material table
The method in face still needs further to develop.Ultraviolet light solidify be a kind of highly effective technological means.In addition, silsesquioxane
As a kind of organosilicon functional compounds, there is good heat-resistant stability, mechanical strength and compatibility, chemical structure can root
According to need to carry out MOLECULE DESIGN and synthesis.
Therefore, the preparation method and applications for developing a kind 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, have a extensive future.
Summary of the invention
In view of this, the present invention provides a kind of preparation method and applications of silicon-based hybrid material coating, utilization is 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 battery and all kinds of optoelectronic devices, anti-fog and self-cleaning function material.
The present invention provides a kind of preparation methods of silicon-based hybrid material coating, the preparation method is that:
Step 1: phenyltrimethoxysila,e and methyl allyl acyloxypropyl trimethoxysilane mixing, are dissolved in solvent,
Stir to obtain the first product；
Step 2: first product is mixed with phenoxyethyl acrylate and photoinitiator, the second product is obtained；
Step 3: second product is layered on substrate, solidify to obtain product.
Preferably, in terms of molar part, the phenyltrimethoxysila,e and methyl allyl acyloxypropyl trimethoxysilane
Feed ratio (1-9): (9~1).
Preferably, the solvent is selected from: one of tetrahydrofuran, methylene chloride and chloroform are a variety of.
Preferably, the step 1 carries out under conditions of nitrogen protection, and whipping temp described in step 1 is room temperature, step
The time of a rapid stirring is 12~72h.
Preferably, the step 1 also needs the potassium carbonate and water of addition.
Preferably, in terms of molar part, the feed ratio of first product, phenoxyethyl acrylate and photoinitiator is
(1~5): (98~94): 1.
Preferably, the photoinitiator is selected from: one of benzophenone, benzoin dimethylether and Irgacure-184 or
It is a variety of.
Preferably, the substrate is glass sheet substrate, and the cured method is ultraviolet light solidification.
Preferably, a length of 200~400nm of the cured ultraviolet light wave of the ultraviolet light, the ultraviolet light cured time is
40~180s.
The present invention also provides a kind of products obtained including one preparation method of any of the above to lead in optical coating
The application in domain.
In conclusion the present invention provides a kind of preparation methods of silicon-based hybrid material coating, and the preparation method is that: step
Rapid one, phenyltrimethoxysila,e and methyl allyl acyloxypropyl trimethoxysilane mixing, be dissolved in solvent, stir first
Product；Step 2: first product is mixed with phenoxyethyl acrylate and photoinitiator, the second product is obtained；Step 3:
Second product is layered on substrate, solidifies to obtain product.The present invention also provides a kind of products that above-mentioned preparation method obtains in light
Learn the application of coatings art.It can be obtained through measuring, product produced by the present invention, surface forms the fold of size uniformity, benefit
The performance of micro-nano fexible film device can be tuned with microcosmic fold, and may finally be applied to optics environmental protection glass for building
Glass, liquid crystal display, solar battery and all kinds of optoelectronic devices antireflection, anti-fog and self-cleaning function material.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 is a kind of preparation principle schematic diagram of the preparation method of silicon-based hybrid material coating provided by the invention；
Fig. 2 is sample optical reflectivity and transmission measurement result prepared by embodiment 3.
Specific embodiment
The present 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 embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
In order to which the present invention is described in more detail, below with reference to embodiment to a kind of silicon-based hybrid material coating provided by the 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,e, 0.16mol methyl allyl acyloxypropyl trimethoxysilane and 0.2g
Potassium carbonate mixing is added 2ml distilled water to mixed system, is dissolved in 40ml solvents tetrahydrofurane, stirs under room temperature for 24 hours,
Obtain the first product 1.In this step, stirring carries out under conditions of nitrogen protection.
According to 3:96:1 mass ratio, it is light-initiated to weigh the first product of 0.3g 1,9.6g phenoxyethyl acrylate and 0.1g
Agent mixing, obtains the second product 1.In this step, photoinitiator Irgacure-184.
Second product 1 is spread on the glass substrate, is solidified 80s with the ultraviolet light that wavelength is 365nm, is obtained product 1.
With the surface texture of electron microscope observation product 1, product 1 can be observed and form fold group flower surface, gained
The size of fold is more uniform.It can be obtained through scanning electron microscope observation and dimension analysis measurement, the size statistic of 1 fold of product
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,e, 0.24mol methyl allyl acyloxypropyl trimethoxysilane and 0.2g
Potassium carbonate mixing is added 2ml distilled water to mixed system, is dissolved in 40ml solvents tetrahydrofurane, stirs under room temperature for 24 hours,
Obtain the first product 2.In this step, stirring carries out under conditions of nitrogen protection.
According to 2:97:1 mass ratio, it is light-initiated to weigh the first product of 0.2g 2,9.7g phenoxyethyl acrylate and 0.1g
Agent mixing, obtains the second product 2.In this step, photoinitiator Irgacure-184.
Second product 1 is spread on the glass substrate, is solidified 80s with the ultraviolet light that wavelength is 365nm, is obtained product 1.
With the surface texture of electron microscope observation product 2, product 2 can be observed and form fold group flower surface, gained
The size of fold is more uniform.It can be obtained through scanning electron microscope observation and dimension analysis measurement, the size statistic of 2 fold of product
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,e, 0.16mol methyl allyl acyloxypropyl trimethoxysilane and 0.2g
Potassium carbonate mixing is added 2ml distilled water to mixed system, is dissolved in 40ml solvents tetrahydrofurane, stirs under room temperature for 24 hours,
Obtain the first product 3.In this step, stirring carries out under conditions of nitrogen protection.
According to 1:98:1 mass ratio, it is light-initiated to weigh the first product of 0.1g 3,9.8g phenoxyethyl acrylate and 0.1g
Agent mixing, obtains the second product 3.In this step, photoinitiator Irgacure-184.
Second product 3 is spread on the glass substrate, is solidified 80s with the ultraviolet light that wavelength is 365nm, is obtained product 3.
With the surface texture of electron microscope observation product 3, product 3 can be observed and form fold group flower surface, gained
The size of fold is more uniform.It can be obtained through scanning electron microscope observation and dimension analysis measurement, the size statistic of 1 fold of product
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% mention to
98%, reflectivity is down to 3% by 8%, has 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,e, 0.04mol methyl allyl acyloxypropyl trimethoxysilane and 0.2g
Potassium carbonate mixing is added 2ml distilled water to mixed system, is dissolved in 40ml solvents tetrahydrofurane, stirs under room temperature for 24 hours,
Obtain the first product 4.In this step, stirring carries out under conditions of nitrogen protection.
According to 5:94:1 mass ratio, it is light-initiated to weigh the first product of 0.5g 4,9.4g phenoxyethyl acrylate and 0.1g
Agent mixing, obtains the second product 4.In this step, photoinitiator Irgacure-184.
Second product 1 is spread on the glass substrate, is solidified 80s with the ultraviolet light that wavelength is 365nm, is obtained 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,e, 0.08mol methyl allyl acyloxypropyl trimethoxysilane and 0.2g
Potassium carbonate mixing is added 2ml distilled water to mixed system, is dissolved in 40ml solvents tetrahydrofurane, stirs under room temperature for 24 hours,
Obtain the first product 5.In this step, stirring carries out under conditions of nitrogen protection.
According to 4:95:1 mass ratio, it is light-initiated to weigh the first product of 0.4g 5,9.5g phenoxyethyl acrylate and 0.1g
Agent mixing, obtains the second product 5.In this step, photoinitiator Irgacure-184.
Second product 1 is spread on the glass substrate, is solidified 80s with the ultraviolet light that wavelength is 365nm, is obtained product 5.
In conclusion the present invention provides a kind of preparation methods of silicon-based hybrid material coating, and the preparation method is that: step
Rapid one, phenyltrimethoxysila,e and methyl allyl acyloxypropyl trimethoxysilane mixing, be dissolved in solvent, stir first
Product；Step 2: first product is mixed with phenoxyethyl acrylate and photoinitiator, the second product is obtained；Step 3:
Second product is layered on substrate, solidifies to obtain product.The present invention also provides a kind of products that above-mentioned preparation method obtains in light
Learn the application of coatings art.It can be obtained through measuring, product produced by the present invention, surface forms the fold of size uniformity, benefit
The performance of micro-nano fexible film device can be tuned with microcosmic fold, and may finally be applied to optics environmental protection glass for building
Glass, liquid crystal display, solar battery and all kinds of optoelectronic devices antireflection, anti-fog and self-cleaning function material.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of silicon-based hybrid material coating, which is characterized in that the preparation method is that:
Step 1: phenyltrimethoxysila,e and methyl allyl acyloxypropyl trimethoxysilane mixing, are dissolved in solvent, stir
Obtain the first product；
Step 2: first product is mixed with phenoxyethyl acrylate and photoinitiator, the second product is obtained；
Step 3: second product is layered on substrate, solidify to obtain product.
2. preparation method according to claim 1, which is characterized in that in terms of molar part, the phenyltrimethoxysila,e
Feed ratio with methyl allyl acyloxypropyl trimethoxysilane is (1~9): (9~1).
3. preparation method according to claim 1, which is characterized in that the solvent is selected from: tetrahydrofuran, methylene chloride and
One of chloroform is a variety of.
4. preparation method according to claim 1, which is characterized in that the step 1 under conditions of nitrogen protection into
It goes, whipping temp described in step 1 is room temperature, and the time of stirring described in step 1 is 12~72h.
5. preparation method according to claim 1, which is characterized in that the step 1 also needs the potassium carbonate and water of addition.
6. preparation method according to claim 1, which is characterized in that in terms of mass parts, first product, phenoxy group second
The feed ratio of base acrylate and photoinitiator is (1~5): (98~94): 1.
7. preparation method according to claim 1, which is characterized in that the photoinitiator is selected from: benzophenone, styrax
One of double methyl ethers and Irgacure-184 are a variety of.
8. preparation method according to claim 1, which is characterized in that the substrate is glass sheet substrate, described cured
Method is ultraviolet light solidification.
9. preparation method according to claim 8, which is characterized in that the cured ultraviolet light wave of ultraviolet light a length of 200
~400nm, the ultraviolet light cured time is 40~180s.
10. a kind of product obtained including preparation method described in claim 1 to 9 any one answering in optical coating art
With.
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