CN111548732A - Super-hydrophilic silicon nano-microstructure anti-reflection coating and preparation and use methods thereof - Google Patents
Super-hydrophilic silicon nano-microstructure anti-reflection coating and preparation and use methods thereof Download PDFInfo
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- C09D183/16—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers in which all the silicon atoms are connected by linkages other than oxygen atoms
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- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/16—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers in which all the silicon atoms are connected by linkages other than oxygen atoms
Abstract
The invention discloses a super-hydrophilic silicon nano-microstructure anti-reflection coating and a preparation method and a use method thereof. The super-hydrophilic silicon nano-microstructure anti-reflection coating comprises the following raw materials in parts by weight: 1-20 parts of polymer microspheres, 5-30 parts of polysilazane and 50-94 parts of organic solvent. According to the invention, the coating is coated on the surface of a substrate, and a super-hydrophilic silicon nano microstructure anti-reflection coating is obtained after high-temperature sintering hole making, and the coating has the excellent performances of lower hydrophilic angle, better hardness, higher light transmittance, aging resistance, acid and alkali resistance, wear resistance and the like; by changing the particle size of the polymer microspheres, coating materials with different hydrophilic effects and anti-reflection effects can be obtained, and the coating materials can be suitable for the fields of self-cleaning, anti-fogging, anti-fouling, oil-water separation, optics, semiconductor electronics and the like; the preparation process is simple and is beneficial to realizing industrial continuous production.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to a super-hydrophilic silicon nano microstructure anti-reflection coating and a preparation method and a use method thereof.
Background
Stronger interaction force exists between the super-hydrophilic coating and water, the water drops can be observed to be completely spread in a short time by dropping the water drops on the surface of the coating, so that the contact angle of the water is equal to or close to 0 degree, and the coating has a very wide application prospect in the fields of self-cleaning, antifogging, antifouling, oil-water separation and the like.
The current methods for realizing the super-hydrophilicity of the coating mainly comprise two main types: firstly, structuring roughness on the surface of a high-surface-energy substance to realize super-hydrophilicity, and secondly, realizing super-hydrophilicity by photoinduced light; the main preparation method of the super-hydrophilic coating comprises the following steps: such as sol-gel methods, vapor deposition methods, templating methods, phase separation methods, and layer-by-layer self-assembly methods.
The super-hydrophilic coating is still limited by a plurality of factors in the practical application process, and mainly comprises the following aspects: firstly, the preparation process of the conventional super-hydrophilic coating is complex, the equipment is expensive, and the preparation of the large-area super-hydrophilic coating is difficult to realize; secondly, the super-hydrophilic coating is greatly influenced by external environment (such as light, heat, oxygen and the like), and the hydrophilic performance is gradually deteriorated after long-term use; the long-lasting property of the super-hydrophilic coating is an important factor for limiting the popularization and the application of the super-hydrophilic coating, and the super-hydrophilic coating has higher surface energy and is easy to convert to a low surface energy direction to reach a stable state, so that the hydrophilic property of the super-hydrophilic coating is lost; the super-hydrophilic surface has poor wear resistance, which is another important factor restricting the popularization and application.
Disclosure of Invention
The invention aims to provide a super-hydrophilic silicon nano-microstructure anti-reflection coating and a preparation method and a using method thereof, so as to solve the technical problems.
In order to achieve the purpose, the technical scheme of the invention is as follows:
in a first aspect, the super-hydrophilic silicon nano microstructure anti-reflection coating provided by the invention comprises the following raw materials in parts by weight: 1-20 parts of polymer microspheres, 5-30 parts of polysilazane and 50-94 parts of organic solvent.
Preferably, the polymer microspheres are selected from one or more of polystyrene microspheres, polymethyl methacrylate microspheres and carbon black microspheres.
Preferably, the average particle size of the polymer microspheres is 0.01-5.0 μm.
Further preferably, the average particle size of the polymer microspheres is 0.01-1.0 μm.
Preferably, the amount of the polymer microspheres in the super-hydrophilic silicon nano-microstructure anti-reflection coating is 5-15 parts.
Preferably, the polysilazane is selected from one or more of inorganic polysilazane, organic polysilazane, and modified polysilazane.
Further preferably, the inorganic polysilazane is perhydropolysilazane; the organic polysilazane is selected from one or more of methyl polysilazane, dimethyl polysilazane and methyl vinyl polysilazane; the modified polysilazane is selected from one or more of vinyl silicone oil modified polysilazane, fluorine-containing modified polysilazane, boron modified polysilazane and transition metal element modified polysilazane.
Preferably, the amount of polysilazane in the super-hydrophilic silicon nano-microstructure antireflection coating is 5-25 parts.
Preferably, the number average molecular weight of the polysilazane is 150-150000 g/moL.
Preferably, the organic solvent is selected from one or more of ethyl acetate, toluene, xylene, D40 solvent oil, butyl acetate, n-octane, cyclohexane, methylcyclohexane, n-butyl ether and tetrahydrofuran;
preferably, the super-hydrophilic siliceous nano-microstructure antireflection coating further comprises an organic auxiliary agent, wherein the organic auxiliary agent is one or two of a leveling agent and a dispersing agent.
Preferably, the amount of the leveling agent in the super-hydrophilic silicon nano-microstructure anti-reflection coating is 0.1-10 parts.
More preferably, the amount of the leveling agent in the super-hydrophilic silicon nano-microstructure antireflection coating is 0.1-5 parts.
Further preferably, the leveling agent is selected from one or more of a leveling agent BYK-333, a leveling agent BYK-306 and a leveling agent Tego-450.
Preferably, the amount of the dispersing agent in the super-hydrophilic silicon nano-microstructure antireflection coating is 0.1-10 parts.
More preferably, the amount of the dispersing agent in the super-hydrophilic silicon nano-microstructure antireflection coating is 0.1-5 parts.
Further preferably, the dispersant is selected from one or more of dispersant BYK-130, dispersant BYK-170, dispersant BYK-P104S and dispersant BYK-2009.
Preferably, the super-hydrophilic silicon nano-microstructure anti-reflection coating comprises the following raw materials in parts by weight: 6-8 parts of polystyrene microspheres, 5-20 parts of fluorine-containing modified polysilazane, 74-87 parts of organic solvent, 0.15 part of flatting agent and 0.3 part of dispersing agent.
Preferably, the super-hydrophilic silicon nano-microstructure anti-reflection coating comprises the following raw materials in parts by weight: 8 parts of polymethyl methacrylate microspheres, 10-20 parts of vinyl silicone oil modified polysilazane, 72-82 parts of organic solvent, 0.1 part of flatting agent and 0.3 part of dispersing agent.
Preferably, the super-hydrophilic silicon nano-microstructure anti-reflection coating comprises the following raw materials in parts by weight: 8-10 parts of carbon black microspheres, 15-20 parts of dimethyl polysilazane, 70-77 parts of organic solvent, 0.2 part of flatting agent and 0.25 part of dispersing agent.
In a second aspect, the invention provides a preparation method of the super-hydrophilic silicon nano-microstructure anti-reflection coating according to the first aspect, which includes the following steps:
and mixing and dispersing the polymer microspheres, the polysilazane, the organic solvent and the organic auxiliary agent uniformly to obtain the polymer microsphere.
Preferably, the mixing and dispersing method is one or more selected from a mechanical stirring method, an ultrasonic dispersing method and a ball milling dispersing method.
Preferably, the mixing and dispersing time is 15-60 min.
In a third aspect, the invention provides a method for using the super-hydrophilic silicon nano-microstructure anti-reflection coating as described in the first aspect, which includes the following steps:
coating the super-hydrophilic silicon nano-microstructure anti-reflection coating on the surface of a substrate, baking and curing at 120-200 ℃, and finally removing the polymer microspheres through high-temperature sintering to obtain the super-hydrophilic silicon nano-microstructure anti-reflection coating.
Preferably, the coating method is selected from one or more of dip coating, curtain coating, wipe coating, blade coating, roll coating and spray coating.
Further preferably, the coating method is spray coating.
Preferably, the substrate is selected from one or more of glass, optical lens, marble, stainless steel and tinplate.
Preferably, the baking and curing temperature is 150 ℃, and the curing time is 1-3 h;
preferably, the high-temperature sintering temperature of the polymer microspheres is 400-500 ℃, and the time is 1-2 h.
Compared with the prior art, the invention has the beneficial effects that:
(1) the super-hydrophilic silicon nano-microstructure anti-reflection coating provided by the invention is mainly prepared from polymer microspheres, polysilazane and an organic solvent, the coating is coated on the surface of a substrate, and a super-hydrophilic silicon nano-microstructure anti-reflection coating is obtained after high-temperature sintering hole making, and the coating has excellent performances of lower hydrophilic angle, better hardness, higher light transmittance, aging resistance, acid and alkali resistance, wear resistance and the like; by changing the particle size of the polymer microspheres, coating materials with different hydrophilic effects and anti-reflection effects can be obtained, and the coating materials can be suitable for the fields of self-cleaning, anti-fogging, anti-fouling, oil-water separation, optics, semiconductor electronics and the like;
(2) the super-hydrophilic silicon nano-microstructure anti-reflection coating disclosed by the invention is simple in preparation process and beneficial to realizing industrial continuous production.
Detailed Description
The following further describes the embodiments of the present invention. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1
The preparation and application method of the super-hydrophilic silicon nano-microstructure antireflection coating provided by the embodiment comprises the following steps:
(1) weighing the following raw materials in parts by weight: 6 parts of polystyrene microspheres, 20 parts of fluorine-containing modified polysilazane, BYK-3330.15 parts of flatting agent, BYK-1300.3 parts of dispersant and 74 parts of butyl acetate, wherein the average particle size of the polystyrene microspheres is 0.1 mu m;
(2) adding polystyrene microspheres into butyl acetate, adding fluorine-containing modified polysilazane into the mixed solution, finally adding a leveling agent BYK-333 and a dispersing agent BYK-130, stirring for 30min at a stirring speed of 1000rpm by using a high-speed stirrer until the polystyrene microspheres are uniformly mixed and dispersed to obtain the super-hydrophilic silicon nano microstructure anti-reflection coating;
(3) spraying the super-hydrophilic silicon nano microstructure anti-reflection coating prepared in the step (2) on the surface of glass, and curing for 3 hours at the temperature of 150 ℃; and then cooling to room temperature, and finally sintering at the high temperature of 450 ℃ for 1h to obtain the super-hydrophilic silicon nano-microstructure anti-reflection coating.
Example 2
The preparation and application method of the super-hydrophilic silicon nano-microstructure antireflection coating provided by the embodiment comprises the following steps:
(1) weighing the following raw materials in parts by weight: 8 parts of polymethyl methacrylate microspheres, 20 parts of fluorine-containing modified polysilazane, BYK-3060.1 parts of flatting agent, BYK-1300.3 parts of dispersant and 72 parts of butyl acetate, wherein the average particle size of the polymethyl methacrylate microspheres is 0.1 mu m;
(2) adding polymethyl methacrylate microspheres into butyl acetate, then adding vinyl silicone oil modified polysilazane into the mixed solution, finally adding a leveling agent BYK-306 and a dispersing agent BYK-130, and stirring for 30min at a stirring speed of 1500rpm by using a high-speed stirrer until the polymethyl methacrylate microspheres are uniformly mixed and dispersed to obtain the super-hydrophilic silicon nano microstructure anti-reflection coating;
(3) spraying the super-hydrophilic silicon nano microstructure anti-reflection coating prepared in the step (2) on the surface of glass, and curing for 1h at 180 ℃; and then cooling to room temperature, and finally sintering at the high temperature of 500 ℃ for 1h to obtain the super-hydrophilic silicon nano-microstructure anti-reflection coating.
Example 3
The preparation and application method of the super-hydrophilic silicon nano-microstructure antireflection coating provided by the embodiment comprises the following steps:
(1) weighing the following raw materials in parts by weight: 10 parts of carbon black microspheres, 20 parts of dimethyl polysilazane, 20 parts of flatting agent Tego-4500.2 parts, 0.25 part of dispersant BYK-P104S 0.25 and 70 parts of butyl acetate, wherein the average particle size of the carbon black microspheres is 0.2 mu m;
(2) adding carbon black microspheres into butyl acetate, then adding dimethyl polysilazane into the mixed solution, finally adding a leveling agent Tego-450 and a dispersant BYK-P104S, and stirring for 30min at a stirring speed of 2500rpm by using a high-speed stirrer until the carbon black microspheres are uniformly mixed and dispersed to obtain the super-hydrophilic silicon nano microstructure anti-reflection coating;
(3) spraying the super-hydrophilic silicon nano microstructure anti-reflection coating prepared in the step (2) on the surface of glass, and curing for 3 hours at the temperature of 150 ℃; and then cooling to room temperature, and finally sintering at the high temperature of 500 ℃ for 1h to obtain the super-hydrophilic silicon nano-microstructure anti-reflection coating.
Example 4
The preparation and application method of the super-hydrophilic silicon nano-microstructure antireflection coating provided by the embodiment comprises the following steps:
(1) weighing the following raw materials in parts by weight: 8 parts of polystyrene microspheres, 5 parts of fluorine-containing modified polysilazane, BYK-3330.15 parts of flatting agent, BYK-1300.3 parts of dispersant and 87 parts of butyl acetate, wherein the average particle size of the polystyrene microspheres is 0.1 mu m;
(2) adding polystyrene microspheres into butyl acetate, adding fluorine-containing modified polysilazane into the mixed solution, finally adding a leveling agent BYK-333 and a dispersing agent BYK-130, stirring for 30min at a stirring speed of 1000rpm by using a high-speed stirrer until the polystyrene microspheres are uniformly mixed and dispersed to obtain the super-hydrophilic silicon nano microstructure anti-reflection coating;
(3) spraying the super-hydrophilic silicon nano microstructure anti-reflection coating prepared in the step (2) on the surface of glass, and curing for 3 hours at the temperature of 150 ℃; and then cooling to room temperature, and finally sintering at the high temperature of 450 ℃ for 1h to obtain the super-hydrophilic silicon nano-microstructure anti-reflection coating.
Example 5
The preparation and application method of the super-hydrophilic silicon nano-microstructure antireflection coating provided by the embodiment comprises the following steps:
(1) weighing the following raw materials in parts by weight: 8 parts of polymethyl methacrylate microspheres, 10 parts of vinyl silicone oil modified polysilazane, BYK-3060.1 parts of a leveling agent, BYK-1300.3 parts of a dispersant and 82 parts of butyl acetate, wherein the average particle size of the polymethyl methacrylate microspheres is 0.1 mu m;
(2) adding polymethyl methacrylate microspheres into butyl acetate, then adding vinyl silicone oil modified polysilazane into the mixed solution, finally adding a leveling agent BYK-306 and a dispersing agent BYK-130, and stirring for 30min at a stirring speed of 1500rpm by using a high-speed stirrer until the polymethyl methacrylate microspheres are uniformly mixed and dispersed to obtain the super-hydrophilic silicon nano microstructure anti-reflection coating;
(3) spraying the super-hydrophilic silicon nano microstructure anti-reflection coating prepared in the step (2) on the surface of glass, and curing for 1h at 180 ℃; and then cooling to room temperature, and finally sintering at the high temperature of 500 ℃ for 1h to obtain the super-hydrophilic silicon nano-microstructure anti-reflection coating.
Example 6
The preparation and application method of the super-hydrophilic silicon nano-microstructure antireflection coating provided by the embodiment comprises the following steps:
(1) weighing the following raw materials in parts by weight: 8 parts of carbon black microspheres, 15 parts of dimethyl polysilazane, a flatting agent Tego-4500.2 parts, 0.25 part of dispersant BYK-P104S 0.25 and 77 parts of butyl acetate, wherein the average particle size of the carbon black microspheres is 0.2 mu m;
(2) adding carbon black microspheres into butyl acetate, then adding dimethyl polysilazane into the mixed solution, finally adding a leveling agent Tego-450 and a dispersant BYK-P104S, and stirring for 30min at a stirring speed of 2500rpm by using a high-speed stirrer until the carbon black microspheres are uniformly mixed and dispersed to obtain the super-hydrophilic silicon nano microstructure anti-reflection coating;
(3) spraying the super-hydrophilic silicon nano microstructure anti-reflection coating prepared in the step (2) on the surface of glass, and curing for 3 hours at the temperature of 150 ℃; and then cooling to room temperature, and finally sintering at the high temperature of 500 ℃ for 1h to obtain the super-hydrophilic silicon nano-microstructure anti-reflection coating.
Performance test 1
In order to further illustrate the beneficial effects of the present invention, the performance parameters of the super-hydrophilic silicon nano microstructure anti-reflection coating prepared in the above examples 1 to 6, such as adhesion, hardness, water contact angle, light transmittance, stain resistance, aging resistance test, acid and alkali resistance, and wear resistance (steel wool), are respectively detected, and the detection results are shown in table 1.
The performance parameters of the super-hydrophilic silicon nano-microstructure anti-reflection coating prepared in the embodiment 1-6 are measured according to the following method:
adhesion force: the assay was performed according to GB/T17748-1999.
Pencil hardness: the measurement was carried out according to ASTM D3363-00.
Water contact angle: the measurement was carried out by using a Memo contact Angle measuring apparatus JC2000D2 in Shanghai.
Light transmittance: the measurement was carried out according to the GB/T18915.1-2 transmission coefficient detection standard.
And (3) testing stain resistance and acid and alkali resistance: the assay was carried out according to GB/T9755-2001.
And (3) aging resistance test: the assay was performed according to GB/T1865-1997.
Abrasion resistance test (steel wool): the measurement was carried out according to GB/T1768-1979.
TABLE 1 Performance index of the coatings obtained in examples 1 to 6
From the above table 1, the super-hydrophilic silicon nano microstructure anti-reflection coating disclosed by the invention has the excellent performances of lower hydrophilic angle, better hardness, higher light transmittance, aging resistance, acid and alkali resistance, wear resistance and the like.
Example 7
Weighing the following raw materials in parts by weight: 1 part of polymethyl methacrylate microspheres, 10 parts of vinyl silicone oil modified polysilazane, BYK-3060.1 parts of leveling agent, BYK-1300.3 parts of dispersant and 89 parts of butyl acetate, wherein the average particle size of the polymethyl methacrylate microspheres is 0.1 mu m, then the coating is prepared according to the step (2) of the embodiment 5, and then the coating is prepared according to the step (3) of the embodiment 5.
Example 8
Weighing the following raw materials in parts by weight: 8 parts of polymethyl methacrylate microspheres, 30 parts of vinyl silicone oil modified polysilazane, BYK-3060.1 parts of a leveling agent, BYK-1300.3 parts of a dispersant and 69 parts of butyl acetate, wherein the average particle size of the polymethyl methacrylate microspheres is 0.1 mu m, then the coating is prepared according to the step (2) of the embodiment 5, and then the coating is prepared according to the step (3) of the embodiment 5.
To further illustrate the beneficial effects of the present invention, the present invention tests the performance of the coating obtained in this example according to the method of performance test 1, and the test results are shown in table 2.
TABLE 2 Performance index of the coatings obtained in examples 7 to 8
Example 9
In this example 9, polystyrene microspheres with average particle diameters of 0.01 μm, 0.05 μm, 0.5 μm, 1 μm and 5 μm are sequentially used to replace the polystyrene microspheres with average particle diameters of 0.1 μm in example 1, and a coating are prepared according to the method in example 1, in order to further illustrate the beneficial effects of the present invention, this example also tests the performance of the coating obtained in this example according to the method in performance test 1, and the test results are shown in table 3.
TABLE 3 Performance index of the coating obtained in example 9
Example 10
In order to further illustrate the beneficial effects of the present invention, the modified polysilazane in examples 1 to 6 is respectively replaced with the iron-modified polysilazane, the steps of examples 1 to 6 are repeated to prepare the coating, the performance of the obtained coating is tested according to the method of performance test 1, and the test results show as follows:
(1) adhesion force: level 0;
(2) hardness: 6H;
(3) water contact angle: 4-12 degrees;
(4) light transmittance: not less than 90%;
(5) stain resistance: level 0;
(6) aging resistance test of a xenon lamp for 2000 h: the appearance is not changed;
(7) acid resistance (5 parts sulfuric acid immersion 48 h): no change in surface;
(8) alkali resistance (48 h soaking in saturated solution): no change in surface;
(9) wear resistance: not less than 5000 times.
It is understood that the modified polysilazanes in the above examples are all prepared by the prior art.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.
Claims (10)
1. The super-hydrophilic silicon nano-microstructure anti-reflection coating is characterized by comprising the following raw materials in parts by weight: 1-20 parts of polymer microspheres, 5-30 parts of polysilazane and 50-94 parts of organic solvent.
2. The super-hydrophilic silicon nano-microstructure anti-reflection coating as claimed in claim 1, wherein the polymer microspheres are selected from one or more of polystyrene microspheres, polymethyl methacrylate microspheres and carbon black microspheres.
3. The super-hydrophilic silicon nano-microstructure antireflection coating according to claim 1, wherein the average particle size of the polymer microspheres is 0.01 to 5.0 μm.
4. The superhydrophilic siliceous nano-microstructured antireflective coating of claim 1, wherein the polysilazane is selected from one or more of an inorganic polysilazane, an organic polysilazane, and a modified polysilazane.
5. The super-hydrophilic silicon nano-microstructure anti-reflection coating according to claim 4, wherein the inorganic polysilazane is perhydropolysilazane; the organic polysilazane is selected from one or more of methyl polysilazane, dimethyl polysilazane and methyl vinyl polysilazane; the modified polysilazane is selected from one or more of vinyl silicone oil modified polysilazane, fluorine-containing modified polysilazane, boron modified polysilazane and transition metal element modified polysilazane.
6. The super-hydrophilic siliceous nano-microstructured antireflection coating according to claim 1, wherein the organic solvent is selected from one or more of ethyl acetate, toluene, xylene, D40 mineral spirit, butyl acetate, n-octane, cyclohexane, methylcyclohexane, n-butyl ether and tetrahydrofuran.
7. The super-hydrophilic silicon nano-microstructure anti-reflection coating according to claim 1, further comprising an organic auxiliary agent, wherein the organic auxiliary agent is one or two of a leveling agent and a dispersing agent.
8. The super-hydrophilic silicon nano-microstructure anti-reflection coating as claimed in claim 1, wherein the leveling agent is one or more selected from a leveling agent BYK-333, a leveling agent BYK-306 and a leveling agent Tego-450, and the dispersing agent is one or more selected from a dispersing agent BYK-130, a dispersing agent BYK-170, a dispersing agent BYK-P104S and a dispersing agent BYK-2009.
9. A preparation method of the super-hydrophilic silicon nano-microstructure antireflection coating as described in any one of claims 1 to 8, characterized by comprising the following steps:
and mixing and dispersing the polymer microspheres, the polysilazane, the organic solvent and the organic auxiliary agent uniformly to obtain the polymer microsphere.
10. The use method of the super-hydrophilic silicon nano-microstructure anti-reflection coating as claimed in any one of claims 1 to 8, is characterized by comprising the following steps:
coating the super-hydrophilic silicon nano-microstructure anti-reflection coating on the surface of a substrate, baking and curing at 120-200 ℃, and finally removing the polymer microspheres through high-temperature sintering to obtain the super-hydrophilic silicon nano-microstructure anti-reflection coating.
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