CN101362917B - Organic/inorganic hybrid nanometer porous anti-reflection coating and its preparation method - Google Patents
Organic/inorganic hybrid nanometer porous anti-reflection coating and its preparation method Download PDFInfo
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- CN101362917B CN101362917B CN2008101616621A CN200810161662A CN101362917B CN 101362917 B CN101362917 B CN 101362917B CN 2008101616621 A CN2008101616621 A CN 2008101616621A CN 200810161662 A CN200810161662 A CN 200810161662A CN 101362917 B CN101362917 B CN 101362917B
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Abstract
The invention discloses an organic/inorganic hybrid nanometer porous anti-reflection coating layer; the organic/inorganic hybrid nanometer porous anti-reflection coating layer, with the thickness of 42.5-162.8nm, porosity of 23.2%-56.9% and aperture of 5-10nm, is gained through a sol-gel process by taking poly-(methyl methacrylate-b- methacryloxypropyltriethoxysilane) as precursor or through the sol-gel process by taking the mixture of the poly-(methyl methacrylate-b-methacryloxypropyltriethoxysilane) and tetraethyl orthosilicate; the invention takes the micro-phase morphology of the block copolymer after the micro-phase separation as a template so as to prepare the organic/inorganic hybrid nanometer porous anti-reflection coating layer; the aperture size is easy to be controlled; furthermore, the distribution of the aperture is uniform, and the basic framework of the anti-reflection layer has Si-O-Si structure; the organic/inorganic hybrid nanometer porous anti-reflection coating layer has excellent mechanical performance, creasing resistance and friction resistance, is rich in Si-OH functional group and can effectively solve the adhesion problem caused by anti-reflection coating layers and various substrates prepared by the prior art.
Description
Technical field
The present invention relates to a kind of organic-inorganic/hybrid nanoscale porous anti-reflection film and preparation method thereof.
Background technology
Anti-reflection coating can increase the transmittance of optics, reduces unnecessary reflection and dazzle, at solar battery panel, display device, prevents field important use such as light pollution.The main path of inhibitory reflex light has at present: 1) by the grinding process to substrate, make it form diffuse-reflectance to incident light, but such treatment process poor effect still has 2% reflectivity, reduce light transmission rate simultaneously significantly; 2) substrate surface is applied one deck anti-reflection coating (antireflection mechanism as shown in Figure 1).The ultimate principle of anti-reflection coating is to allow the reflected light of coating and air interface and the reflected light of coating and substrate interface produce interference, thereby has offset catoptrical energy, reaches the purpose of antireflection.The preparation of anti-reflection coating mainly concentrates in the preparation of porous membrane, and the pore size of porous-film and distribution and coat-thickness have all determined the effect of antireflection.As everyone knows, the microphase-separated of segmented copolymer can form nano ordered microfacies structure.Gather (methyl methacrylate-b-methacryloxypropyl triethyl silicane) binary segmented copolymer as reaction monomers by active free radical polymerization (as the RAFT polymerization) preparation with methyl methacrylate (MMA) and methacryloxypropyl triethyl silicane (MPES).Use the method for spin coating, block copolymer solution is coated in substrate surface, after complete microphase-separated takes place in segmented copolymer, sol-gel process by siloxanes in the polymkeric substance fixes the microfacies structure, can prepare nanometer porous film by the ultraviolet degradation polymethylmethacrylate, can form with segmented copolymer simultaneously, thickness and light application time are effectively regulated the film refractive index, realize different antireflection requirements.In addition, the skeleton of coating mainly is made up of the Si-O-Si structure, and contain Si-OH functional group, therefore this coating has higher intensity than single film, anti-fold rub resistance, with characteristics such as the binding property of substrate are good, can effectively overcome bad mechanical property and optical property problem of unstable that present all kinds of anti-reflection coating exists.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of organic/inorganic hybrid nanoscale porous anti-reflection coating is provided.
Hybrid nanoporous anti-reflection coating is: be presoma with poly-(methyl methacrylate-b-methacryloxypropyl triethyl silicane) obtains hybrid nanoporous anti-reflection coating or is that presoma obtains hybrid nanoporous anti-reflection coating by sol-gel process with the mixture of poly-(methyl methacrylate-b-methacryloxypropyl triethyl silicane) and tetraethoxy by sol-gel process, the thickness of hybrid nanoporous anti-reflection coating is 42.5～162.8nm, porosity is 23.2%～56.9%, and the aperture is 5～10nm.
Methyl methacrylate segmental number-average molecular weight in described poly-(methyl methacrylate-b-methacryloxypropyl triethyl silicane) is 7000～15000, and the methacryloxypropyl triethyl silicane segmental number-average molecular weight in poly-(methyl methacrylate-b-methacryloxypropyl triethyl silicane) is 6000～40000.
The preparation method of hybrid nanoporous anti-reflection coating comprises the steps:
1) in weight percent concentration is poly-(methyl methacrylate-b-methacryloxypropyl triethyl silicane) solution of 2%～10%, the adding weight percent concentration is 0.5%～10% tetraethoxy, uniform mixing, obtain mixed solution, with sol evenning machine mixed solution being become thickness in the substrate surface spin coating is 80～160nm hybrid nano coating;
2) with in the saturated atmosphere of hybrid nano coating as for organic solvent, organic solvent annealing 1～7 day was annealed 1～5 day under in the vacuum drying oven 50～120 ℃ then, and annealing finishes, and cools off rapidly with ice cube; Then place the atmosphere 1～5 day of ammoniacal liquor, it is dry to put into vacuum drying oven; Place irradiation under the ultraviolet lamp again, prepare hybrid nanoporous anti-reflection coating.
Described organic solvent is: toluene, ethylbenzene, isopropyl benzene, p-Xylol, o-Xylol, methylene dichloride or dioxane six alkane.Ultraviolet lamp send wavelength less than 400nm.Substrate is slide glass or quartz glass plate.
The beneficial effect that the present invention compared with prior art has:
1) with the microfacies form after the segmented copolymer microphase-separated as the nanometer porous film of template for preparing, its pore size be easy to control and the pore size distribution homogeneous;
2) by the nano level film of spin-coating method preparation, film thickness is easy to regulation and control and thickness homogeneous;
3) mixture with siliceous binary segmented copolymer or it and tetraethoxy is the nano level film of precursor preparation, its basic boom is the Si-O-Si structure, the mechanical property excellence, anti-fold rub resistance, and be rich in Si-OH functional group, can effectively solve the problem of sticking by the film of present technical preparation and all kinds of substrates;
4) technology is simple.
Description of drawings
Fig. 1 is the mechanism figure of antireflective film of the present invention;
I: incident light; T: transmitted light; R1: the reflected light of film and air interface; R2: the reflected light of film and substrate interface; No: the refractive index of air; Nl: the refractive index of film; Ns: the refractive index of substrate; λ: lambda1-wavelength;
Fig. 2 is segmented copolymer body that the embodiment of the invention 1 the obtains TEM photo that is separated;
Fig. 3 is segmented copolymer film that the embodiment of the invention 1 the obtains AFM photo that is separated;
Fig. 4 is the AFM phase diagram photo of porous membrane behind the ultraviolet lighting that obtains of the embodiment of the invention 1;
Fig. 5 is the stereographic map photo of the AFM phase diagram of porous membrane behind the ultraviolet lighting that obtains of the embodiment of the invention 1;
Fig. 6 is the long light transmission graphic representation of visible light all-wave of the nanometer porous film that obtains of the embodiment of the invention 1.
Embodiment
Hybrid nanoporous anti-reflection coating is: be presoma with poly-(methyl methacrylate-b-methacryloxypropyl triethyl silicane) obtains hybrid nanoporous anti-reflection coating or is that presoma obtains hybrid nanoporous anti-reflection coating by sol-gel process with the mixture of poly-(methyl methacrylate-b-methacryloxypropyl triethyl silicane) and tetraethoxy by sol-gel process, the thickness of hybrid nanoporous anti-reflection coating is 42.5～162.8nm, porosity is 23.2%～56.9%, and the aperture is 5～10nm.
Methyl methacrylate segmental number-average molecular weight in described poly-(methyl methacrylate-b-methacryloxypropyl triethyl silicane) is 7000～15000, and the methacryloxypropyl triethyl silicane segmental number-average molecular weight in poly-(methyl methacrylate-b-methacryloxypropyl triethyl silicane) is 6000～40000.
Embodiment 1:
To gather (methyl methacrylate-b-methacryloxypropyl triethyl silicane) and be made into 5% tetrahydrofuran solution, add the 0.1g tetraethoxy, become the nano level film with the desk-top sol evenning machine of KW-4A type in the slide surface spin coating then, even glue fs rotating speed is controlled at 1000r/min, time 15s, even glue subordinate phase rotating speed is controlled at 3000r/min, time 60s.After smearing with in the saturated atmosphere of film as for tetrahydrofuran (THF), solvent annealing 4 days, then with film as for 90 ℃ of annealing in the vacuum drying oven 36 hours, annealing time finishes the back and cools off rapidly with ice cube at once.Be placed on after the cooling in the atmosphere of ammoniacal liquor 24 hours, seasoning subsequently put it in the vacuum drying oven 50 ℃ of dryings in 3 days 5 days again.Took out under the ultraviolet lamp be placed on UV-40w illumination subsequently 5 hours.Each nature parameters of the hybrid nanoporous anti-reflection coating that the embodiment of the invention 1 obtains sees Table 1.
Table 1
Embodiment 2:
To gather (methyl methacrylate-b-methacryloxypropyl triethyl silicane) and be made into 5% tetrahydrofuran solution, add the 0.05g tetraethoxy, become the nano level film with the desk-top sol evenning machine of KW-4A type in the slide surface spin coating then, even glue fs rotating speed is controlled at 1000r/min, time 15s, even glue subordinate phase rotating speed is controlled at 3000r/min, time 60s.After smearing with in the saturated atmosphere of film as for tetrahydrofuran (THF), solvent annealing 4 days, then with film as for 90 ℃ of annealing in the vacuum drying oven 36 hours, annealing time finishes the back and cools off rapidly with ice cube at once.Be placed on after the cooling in the atmosphere of ammoniacal liquor 24 hours, seasoning subsequently put it in the vacuum drying oven 50 ℃ of dryings in 3 days 5 days again.Took out under the ultraviolet lamp be placed on UV-40w illumination subsequently 5 hours.
Embodiment 3:
Methyl acrylate-b-methacryloxypropyl triethyl silicane) is made into 10% tetrahydrofuran solution, become the nano level film with the desk-top sol evenning machine of KW-4A type in the slide surface spin coating then, even glue fs rotating speed is controlled at 1000r/min, time 15s, even glue subordinate phase rotating speed is controlled at 3000r/min, time 60s.After smearing with in the saturated atmosphere of film as for tetrahydrofuran (THF), solvent annealing 4 days, then with film as for 90 ℃ of annealing in the vacuum drying oven 36 hours, annealing time finishes the back and cools off rapidly with ice cube at once.Be placed on after the cooling in the atmosphere of ammoniacal liquor 24 hours, seasoning subsequently put it in the vacuum drying oven 50 ℃ of dryings in 3 days 5 days again.Took out under the ultraviolet lamp be placed on UV-40w illumination subsequently 5 hours.
Embodiment 4:
To gather (methyl methacrylate-b-methacryloxypropyl triethyl silicane) and be made into 10% tetrahydrofuran solution, become the nano level film with the desk-top sol evenning machine of KW-4A type in quartz glass plate surface spin coating then, even glue fs rotating speed is controlled at 1000r/min, time 15s, even glue subordinate phase rotating speed is controlled at 3000r/min, time 60s.After smearing with in the saturated atmosphere of film as for tetrahydrofuran (THF), solvent annealing 4 days, then with film as for 90 ℃ of annealing in the vacuum drying oven 36 hours, annealing time finishes the back and cools off rapidly with ice cube at once.Be placed on after the cooling in the atmosphere of ammoniacal liquor 24 hours, seasoning subsequently put it in the vacuum drying oven 50 ℃ of dryings in 3 days 5 days again.Took out under the ultraviolet lamp be placed on UV-40w illumination subsequently 10 hours.
Embodiment 5:
To gather (methyl methacrylate-b-methacryloxypropyl triethyl silicane) and be made into 5% tetrahydrofuran solution, become the nano level film with the desk-top sol evenning machine of KW-4A type in quartz glass plate surface spin coating then, even glue fs rotating speed is controlled at 1000r/min, time 15s, even glue subordinate phase rotating speed is controlled at 3000r/min, time 60s.After smearing with in the saturated atmosphere of film as for tetrahydrofuran (THF), solvent annealing 4 days, then with film as for 90 ℃ of annealing in the vacuum drying oven 36 hours, annealing time finishes the back and cools off rapidly with ice cube at once.Be placed on after the cooling in the atmosphere of ammoniacal liquor 24 hours, seasoning subsequently put it in the vacuum drying oven 50 ℃ of dryings in 3 days 5 days again.Took out under the ultraviolet lamp be placed on UV-40w illumination subsequently 5 hours.
Embodiment 6:
To gather (methyl methacrylate-b-methacryloxypropyl triethyl silicane) and be made into 5% tetrahydrofuran solution, become the nano level film with the desk-top sol evenning machine of KW-4A type in quartz glass plate surface spin coating then, even glue fs rotating speed is controlled at 1000r/min, time 15s, even glue subordinate phase rotating speed is controlled at 3000r/min, time 60s.After smearing with in the saturated atmosphere of film as for tetrahydrofuran (THF), solvent annealing 4 days, then with film as for 90 ℃ of annealing in the vacuum drying oven 36 hours, annealing time finishes the back and cools off rapidly with ice cube at once.Be placed on after the cooling in the atmosphere of ammoniacal liquor 24 hours, seasoning subsequently put it in the vacuum drying oven 50 ℃ of dryings in 3 days 5 days again.Took out under the ultraviolet lamp be placed on UV-40w illumination subsequently 10 hours.
Embodiment 7:
1) in weight percent concentration is poly-(methyl methacrylate-b-methacryloxypropyl triethyl silicane) solution of 2%, the adding weight percent concentration is 0.5% tetraethoxy, uniform mixing, obtain mixed solution, with sol evenning machine mixed solution being become thickness in the slide surface spin coating is 80nm hybrid nano coating;
2) with in the saturated atmosphere of hybrid nano coating as for toluene, ethylbenzene annealing 1 day was annealed 1 day under in the vacuum drying oven 50 ℃ then, and annealing finishes, and cools off rapidly with ice cube; Then place the atmosphere 1 day of ammoniacal liquor, it is dry to put into vacuum drying oven; Place irradiation under the ultraviolet lamp again, prepare hybrid nanoporous anti-reflection coating.
Embodiment 8:
1) in weight percent concentration is poly-(methyl methacrylate-b-methacryloxypropyl triethyl silicane) solution of 10%, the adding weight percent concentration is 10% tetraethoxy, uniform mixing, obtain mixed solution, with sol evenning machine mixed solution being become thickness in quartz glass plate surface spin coating is 160nm hybrid nano coating;
2) with in the saturated atmosphere of hybrid nano coating as for dioxane six alkane, dioxane six alkane annealing 7 days was annealed 5 days under in the vacuum drying oven 120 ℃ then, and annealing finishes, and cools off rapidly with ice cube; Then place the atmosphere 5 days of ammoniacal liquor, it is dry to put into vacuum drying oven; Place irradiation under the ultraviolet lamp again, prepare hybrid nanoporous anti-reflection coating.
Claims (4)
1. hybrid nanoporous anti-reflection coating, it is characterized in that: be presoma with poly-(methyl methacrylate-b-methacryloxypropyl triethyl silicane) obtains hybrid nanoporous anti-reflection coating or is that presoma obtains hybrid nanoporous anti-reflection coating by sol-gel process with the mixture of poly-(methyl methacrylate-b-methacryloxypropyl triethyl silicane) and tetraethoxy by sol-gel process, the thickness of hybrid nanoporous anti-reflection coating is 42.5～162.8nm, porosity is 23.2%～56.9%, and the aperture is 5～10nm; Methyl methacrylate segmental number-average molecular weight in described poly-(methyl methacrylate-b-methacryloxypropyl triethyl silicane) is 7000～15000, and the methacryloxypropyl triethyl silicane segmental number-average molecular weight in poly-(methyl methacrylate-b-methacryloxypropyl triethyl silicane) is 6000～40000; Concrete preparation method comprises the steps:
1) in weight percent concentration is poly-(methyl methacrylate-b-methacryloxypropyl triethyl silicane) solution of 2%～10%, the adding weight percent concentration is 0.5%～10% tetraethoxy, uniform mixing, obtain mixed solution, with sol evenning machine mixed solution being become thickness in the substrate surface spin coating is 80～160nm hybrid nano coating;
2) the hybrid nano coating is placed the saturated atmosphere of organic solvent, organic solvent annealing 1～7 day places the annealing 1～5 day down of 50～120 ℃ of vacuum drying ovens then, and annealing finishes, and cools off rapidly with ice cube; Then place the atmosphere 1～5 day of ammoniacal liquor, it is dry to put into vacuum drying oven; Place irradiation under the ultraviolet lamp again, prepare hybrid nanoporous anti-reflection coating.
2. the preparation method according to the described hybrid nanoporous of claim 1 anti-reflection coating is characterized in that comprising the steps:
1) in weight percent concentration is poly-(methyl methacrylate-b-methacryloxypropyl triethyl silicane) solution of 2%～10%, the adding weight percent concentration is 0.5%～10% tetraethoxy, uniform mixing, obtain mixed solution, with sol evenning machine mixed solution being become thickness in the substrate surface spin coating is 80～160nm hybrid nano coating;
2) the hybrid nano coating is placed the saturated atmosphere of organic solvent, organic solvent annealing 1～7 day places the annealing 1～5 day down of 50～120 ℃ of vacuum drying ovens then, and annealing finishes, and cools off rapidly with ice cube; Then place the atmosphere 1～5 day of ammoniacal liquor, it is dry to put into vacuum drying oven; Place irradiation under the ultraviolet lamp again, prepare hybrid nanoporous anti-reflection coating.
3. the preparation method of a kind of hybrid nanoporous anti-reflection coating according to claim 2 is characterized in that: described organic solvent is: tetrahydrofuran (THF), toluene, ethylbenzene, isopropyl benzene, p-Xylol, o-Xylol, methylene dichloride or dioxane.
4. the preparation method of a kind of hybrid nanoporous anti-reflection coating according to claim 2 is characterized in that: described ultraviolet lamp send wavelength less than 400nm.
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| CN104789076A (en) * | 2015-04-15 | 2015-07-22 | 苏州创佳电子材料有限公司 | Multifunctional anti-glaring transparent coating material as well as preparation method and application thereof |
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