CN116715890A - Method for preparing antireflection film by adopting core-shell microstructure light-transmitting particles - Google Patents
Method for preparing antireflection film by adopting core-shell microstructure light-transmitting particles Download PDFInfo
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- 239000002245 particle Substances 0.000 title claims abstract description 45
- 239000011258 core-shell material Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 108
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 67
- 238000000576 coating method Methods 0.000 claims abstract description 55
- 239000011248 coating agent Substances 0.000 claims abstract description 47
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 45
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 38
- 229910052709 silver Inorganic materials 0.000 claims abstract description 36
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000004332 silver Substances 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 84
- 238000003756 stirring Methods 0.000 claims description 57
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 54
- 239000011259 mixed solution Substances 0.000 claims description 36
- 239000000243 solution Substances 0.000 claims description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- 238000006243 chemical reaction Methods 0.000 claims description 28
- 239000002244 precipitate Substances 0.000 claims description 26
- 239000008367 deionised water Substances 0.000 claims description 24
- 229910021641 deionized water Inorganic materials 0.000 claims description 24
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 22
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 15
- 239000007787 solid Substances 0.000 claims description 13
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 12
- 239000012956 1-hydroxycyclohexylphenyl-ketone Substances 0.000 claims description 12
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical compound CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 claims description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 12
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 12
- MQDJYUACMFCOFT-UHFFFAOYSA-N bis[2-(1-hydroxycyclohexyl)phenyl]methanone Chemical compound C=1C=CC=C(C(=O)C=2C(=CC=CC=2)C2(O)CCCCC2)C=1C1(O)CCCCC1 MQDJYUACMFCOFT-UHFFFAOYSA-N 0.000 claims description 12
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 12
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 12
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 12
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 12
- 239000004094 surface-active agent Substances 0.000 claims description 12
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 11
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 claims description 10
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 claims description 6
- 230000003213 activating effect Effects 0.000 claims description 6
- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical compound [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 claims description 6
- 229920002635 polyurethane Polymers 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 2
- 239000000047 product Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 4
- 230000000694 effects Effects 0.000 abstract description 3
- 239000010410 layer Substances 0.000 description 37
- 229910052681 coesite Inorganic materials 0.000 description 24
- 229910052906 cristobalite Inorganic materials 0.000 description 24
- 229910052682 stishovite Inorganic materials 0.000 description 24
- 229910052905 tridymite Inorganic materials 0.000 description 24
- 230000000052 comparative effect Effects 0.000 description 20
- 229920000139 polyethylene terephthalate Polymers 0.000 description 15
- 239000005020 polyethylene terephthalate Substances 0.000 description 15
- 239000003795 chemical substances by application Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 239000011247 coating layer Substances 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 238000002834 transmittance Methods 0.000 description 5
- 239000006117 anti-reflective coating Substances 0.000 description 4
- 239000003638 chemical reducing agent Substances 0.000 description 4
- 239000003973 paint Substances 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- 230000003667 anti-reflective effect Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 2
- -1 acrylic ester Chemical class 0.000 description 2
- 238000013507 mapping Methods 0.000 description 2
- 238000004528 spin coating Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000001579 optical reflectometry Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/042—Coating with two or more layers, where at least one layer of a composition contains a polymer binder
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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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/006—Anti-reflective coatings
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2475/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2475/04—Polyurethanes
- C08J2475/14—Polyurethanes having 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0806—Silver
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Abstract
The invention discloses a method for preparing an antireflection film by adopting core-shell microstructure light-transmitting particles, which specifically comprises the following steps: step 1, silicon dioxide coating silver material SiO 2 Ag; step 2, preparing silver coated silicon dioxide Ag@SiO 2 The method comprises the steps of carrying out a first treatment on the surface of the And 3, preparing a coating according to the products obtained in the step 1 and the step 2, and preparing the anti-reflection film with the core-shell microstructure. The anti-reflection film prepared by the invention reduces the cost and improves the anti-reflection effect of the film.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and relates to a method for preparing an antireflection film by adopting core-shell microstructure light-transmitting particles.
Background
In recent years, with the development of new display, face recognition, stereoscopic imaging and other scientific technologies, higher requirements are being placed on optical properties of materials and the like. For the new display OLED or LED, a glass or film substrate is added to the outer layer of the screen to improve the aesthetic appearance of the screen and protect the screen device, however, the added film of the outer layer of the screen causes light reflection (external light source mapping) to reduce the screen definition and visibility.
For this reason, antireflection films of a multilayer structure have been designed. For example, a plurality of materials with different refractive indexes are sequentially coated on a glass or film substrate, and the materials are absorbed by utilizing reflection and scattering among film layers with different refractive indexes, so that the mapping of an external light source is reduced. In general, glass and silica have refractive indexes of 1.5, and metal oxides such as aluminum oxide have refractive indexes of about 1.76, and if they are used to make a multilayer anti-reflection material, on the one hand, the cost is high, and on the other hand, the difference in refractive index between different layers is small, and the anti-reflection effect is poor.
Disclosure of Invention
The invention aims to provide a method for preparing an antireflection film by adopting core-shell microstructure light-transmitting particles, which can reduce cost and improve antireflection effect of the film.
The technical scheme adopted by the invention is that the method for preparing the antireflection film by adopting the core-shell microstructure light-transmitting particles specifically comprises the following steps:
step 1, silicon dioxide coating silver material SiO 2 @Ag；
Step 2, preparing silver coated silicon dioxide Ag@SiO 2 ；
And 3, preparing a coating according to the products obtained in the step 1 and the step 2, and preparing the anti-reflection film with the core-shell microstructure.
The invention is also characterized in that:
the specific process of the step 1 is as follows:
1.1, dissolving 1.7g-3.4g of silver nitrate in 10mL of water, then adding 0.4g-0.6g of NaOH, stirring for 30min-60min to form a precipitate, adding 10wt% -20wt% of ammonia water to the precipitate until the precipitate is completely dissolved, then adding 1g-2g of polyvinylpyrrolidone, stirring uniformly, adding 2.5mL-5mL of 25wt% -30wt% of hydrazine hydrate solution, stirring for 12h-24h at room temperature, and centrifuging at a rotating speed of 7000r/min-10000r/min after the reaction is finished to obtain silver particles;
step 1.2, dispersing 1g-2g of silver particles into 150mL-300mL of glycerol, adding 0.1g-0.2g of surfactant sodium dodecyl sulfonate, then adding 2.5g-5g of tetraethyl orthosilicate and 0.8g-1.6g of NaOH, continuously stirring for 12h-24h, and adopting 7000r/min-1 after the reaction is finishedCentrifuging at 0000r/min, washing with 100-200mL ethanol and 100-200mL deionized water, and repeating for six times to obtain silicon dioxide coated silver material SiO 2 Material @ Ag.
The specific process of the step 2 is as follows:
step 2.1, preparing silicon dioxide particles;
2.2, dissolving 0.01g-0.05g of 3-mercaptopropyl trimethoxy silane into 100mL-200mL of ethanol solution, then adding 0.5g-1g of silica particles, stirring and reacting for 1h-2h, activating the surfaces of the silica particles, continuously adding 0.5g-1g of polyvinylpyrrolidone, and stirring uniformly to obtain a mixed solution C;
2.3, dissolving 0.5g-1g of silver nitrate in 10mL of water, then adding 0.1g-1g of NaOH, stirring for 30min-60min to form a precipitate, and then adding 10wt% -20wt% of ammonia water until the precipitate is completely dissolved to obtain a mixed solution D;
step 2.4, mixing and stirring the mixed solution C and the mixed solution D uniformly, then dropwise adding 20-30mL of 5-10wt% hydrazine hydrate, continuously stirring at room temperature for 12-24h after the dropwise adding is finished, centrifuging for 30-60min by 7000-10000r/min after the reaction is finished, collecting solids, washing the solids by 100-200mL of ethanol and 100-200mL of deionized water, and repeating for 6 times to obtain silver-coated silica Ag@SiO 2 。
The specific process of the step 2.1 is as follows:
step 2.1.1, adding 0.3g-0.5g of surfactant sodium dodecyl sulfonate into 250mL-500mL of deionized water with 0.5g-1g of tetraethyl orthosilicate, and uniformly stirring to obtain a mixed solution A;
2.1.2, dissolving 0.05g-0.1g of sodium ethoxide in 500mL-1000mL of ethanol to obtain a mixed solution B;
step 2.1.3, dropwise adding the solution A into the solution B, reacting for 12-24 hours at room temperature after the dropwise adding is finished, centrifuging for 30-60 minutes at 7000-10000r/min after the reaction is finished, collecting solid, washing with 100-200ml ethanol and 100-200ml deionized water, and repeating for 6 times to obtain the silicon dioxide particles.
The specific process of the step 3 is as follows:
step 3.1, 1g-2g urethane acrylate, 1g-2g of isooctyl acrylate, 1g to 2g of 1-hydroxycyclohexyl phenyl ketone, 0.5g to 1g of SiO 2 Mixing @ Ag and 5-10mL ethanol solution to obtain SiO 2 An @ Ag coating;
step 3.2, 1g-2g of polyurethane acrylate, 1g-2g of isooctyl acrylate, 1g-2g of 1-hydroxycyclohexyl phenyl ketone, 0.5g-1g of Ag@SiO 2 Mixing 5mL-10mL ethanol solution to obtain Ag@SiO 2 A coating;
step 3.3, using transparent PET as a carrier, and using the SiO prepared in the step 3.1 2 Ag@Ag coating and Ag@SiO prepared in step 3.2 2 The coating is sequentially and alternately dripped and coated on the surface of PET with the size of 5cmx5cm, spin-coated uniformly at the rotating speed of 1000r/min-3000r/min, and then is put into an ultraviolet curing machine to be cured into a film, so that the core-shell structure reflective film with the thickness of 0.4um-0.7um is obtained, and the curing conditions in the ultraviolet curing machine are as follows: flash irradiation for 1-2 min at 80-120deg.C, and ultraviolet power of 80-120W.
The invention has the beneficial effects that two core-shell structural materials are designed: core-shell material Ag@SiO with large refractive index and small refractive index 2 (Ag has a large refractive index and SiO2 has a small refractive index); the other is core-shell material SiO with small refractive index and large refractive index 2 Ag; the small-package large material and the large-package small material are respectively coated on PET, so that the anti-reflection performance of the film can be greatly improved, wherein each core-shell particle in the small-package large layer and the large-package small layer can be used as an optical microcavity to realize light reflection and absorption, and meanwhile, the reflection and absorption of light can be realized due to different refractive indexes between the small-package large layer and the large-package small layer.
Drawings
FIG. 1 is a diagram of a structural model and an optical motion model of a core-shell structured light-transmitting particle for an antireflection film;
FIG. 2 is Ag, siO2, siO 2 Ag and Ag@SiO 2 Is a hydraulic radius change value comparison chart;
FIG. 3 is a graph showing the transmittance of the anti-reflective coatings prepared in examples 1 and 2 and comparative examples 1 to 3, which are obtained by the method for preparing the anti-reflective coating using the core-shell microstructure light transmitting particles according to the present invention.
Detailed Description
The invention will be described in detail below with reference to the drawings and the detailed description.
The invention relates to a method for preparing an antireflection film by adopting core-shell microstructure light-transmitting particles, which specifically comprises the following steps:
step 1, silicon dioxide coated silver material (SiO 2 @ Ag) preparation:
1.1, dissolving 1.7-3.4g of silver nitrate in 10mL of water, then adding 0.4-0.6g of NaOH, stirring for 30-60min to form a precipitate, further adding 10-20wt% of ammonia water until the precipitate is completely dissolved, adding 1-2g of polyvinylpyrrolidone (template agent), stirring uniformly, adding 2.5-5mL of 25-30wt% of hydrazine hydrate (reducing agent) solution, stirring for 12-24h at room temperature, and centrifuging at a rotating speed of 7000-10000r/min after the reaction is finished to obtain silver particles.
Step 1.2, dispersing 1-2g of silver particles into 150-300mL of glycerol, adding 0.1-0.2g of surfactant sodium dodecyl sulfonate, then adding 2.5-5g of tetraethyl orthosilicate and 0.8-1.6g of NaOH, and stirring for 12-24 hours. After the reaction is finished, centrifuging at a rotating speed of 7000-10000r/min, washing with 100-200mL of ethanol and 100-200mL of deionized water, and repeating six times to obtain SiO 2 Material @ Ag.
Step 2, silver coated silica (Ag@SiO) 2 ) Is prepared from the following steps:
step 2.1, adding 0.3-0.5g of surfactant sodium dodecyl sulfonate into 250-500mL of deionized water with the weight of 0.5-1g of tetraethyl orthosilicate, and uniformly stirring to obtain a mixed solution A; then 0.05-0.1g of sodium ethoxide is dissolved in 500-1000mL of ethanol to obtain a mixed solution B. The solution A is dropwise added into the solution B (the dropping speed is 0.5 d/s), and after the addition is finished, the reaction is carried out for 12 to 24 hours at room temperature. Centrifuging for 30-60min at 7000-10000r/min after the reaction is finished, collecting solid, washing with 100-200ml ethanol and 100-200ml deionized water, and repeating for 6 times to obtain silica particles.
And 2.2, dissolving 0.01-0.05g of 3-mercaptopropyl trimethoxy silane into 100-200mL of ethanol solution, then adding 0.5-1g of silicon dioxide particles, stirring and reacting for 1-2h, activating the surfaces of the silicon dioxide particles, continuously adding 0.5-1g of polyvinylpyrrolidone (template agent), and stirring uniformly to obtain a mixed solution C. 0.5-1gSilver nitrate is dissolved in 10mL of water, then 0.1-1g of NaOH is added, the mixture is stirred for 30-60min to form a precipitate, and 10-20wt% of ammonia water is further added until the precipitate is completely dissolved to obtain a mixed solution D. And mixing and stirring the mixed solution C and the mixed solution D uniformly. Then dropwise adding 20-30mL of 5-10wt% hydrazine hydrate, and continuously stirring for 12-24h at room temperature after the dropwise adding is finished. Centrifuging at 7000-10000r/min for 30-60min after the reaction, collecting 100-200ml of solid, washing with ethanol and 100-200ml of deionized water, repeating for 6 times to obtain Ag@SiO 2 。
Step 3, preparation of an antireflection film with a core-shell microstructure:
SiO 2 preparing an Ag coating: urethane acrylate (1-2 g), isooctyl acrylate (1-2 g), 1-hydroxycyclohexyl phenyl ketone (1-2 g), siO 2 Ag (prepared in step 1) (0.5-1 g) and 5-10mL of ethanol solution.
Ag@SiO 2 Preparing a coating: polyurethane acrylic ester (1-2 g), isooctyl acrylate (1-2 g), 1-hydroxy cyclohexyl phenyl ketone (1-2 g), ag@SiO 2 (prepared in the step 2) (0.5-1 g) and 5-10mL of ethanol solution.
For SiO respectively 2 Ag coating and Ag@SiO 2 The paint is vacuumized to remove air. 1mL-2mLSiO was carried on transparent PET (polyethylene terephthalate) 2 Ag coating and 1mL-2mLAg@SiO 2 The coating is sequentially and alternately dripped and coated on the surface of PET with the size of 5cmx5cm, spin-coated uniformly at the rotating speed of 1000r/min-3000r/min, and then is put into an ultraviolet curing machine to be cured into a film, so that the core-shell structure reflective film with the thickness of 0.4um-0.7um is obtained, and the curing conditions in the ultraviolet curing machine are as follows: flash irradiation for 1-2 min at 80-120deg.C, and ultraviolet power of 80-120W.
Example 1
Step 1, silicon dioxide coated silver material (SiO 2 @ Ag) was prepared
Step 1.1, dissolving 1.7g of silver nitrate in 10mL of water, then adding 0.4g of NaOH, stirring for 30min to form a precipitate, further adding 10wt% of ammonia water until the precipitate is completely dissolved, adding 1g of polyvinylpyrrolidone (template agent), stirring uniformly, adding 2.5mL of 25wt% of hydrazine hydrate (reducing agent) solution, stirring for 12h at room temperature, and centrifuging at a rotating speed of 7000r/min after the reaction is finished to obtain silver particles.
Step 1.2, 1g of silver particles was dispersed in 150mL of glycerol, 0.1g of sodium dodecyl sulfate as a surfactant was added, then 2.5g of tetraethyl orthosilicate and 0.8g of NaOH were added, and stirring was continued for 12 hours. After the reaction is finished, centrifuging at a rotating speed of 7000r/min, washing with 100mL of ethanol and 100 deionized water, and repeating six times to obtain SiO 2 Material @ Ag.
Step 2, silver coated silica (Ag@SiO) 2 ) Is prepared from
Step 2.1, adding 0.3g of surfactant sodium dodecyl sulfonate into 500mL of deionized water of 0.5g of tetraethyl orthosilicate, and uniformly stirring to obtain a mixed solution A; then, 0.05g of sodium ethoxide was dissolved in 1000mL of ethanol to obtain a mixed solution B. Solution A was added dropwise (drop rate: 0.5 d/s) to solution B, and after the addition was completed, the reaction was carried out at room temperature for 12 hours. After the reaction was completed, the mixture was centrifuged at 7000r/min for 30 minutes, and 100ml of ethanol and 100ml of deionized water were collected and washed, and repeated 6 times to obtain silica particles.
And 2.2, dissolving 0.01g of 3-mercaptopropyl trimethoxy silane into 100mL of ethanol solution, then adding 0.5g of silicon dioxide particles, stirring and reacting for 1h, activating the surfaces of the silicon dioxide particles, continuously adding 0.5g of polyvinylpyrrolidone (template agent), and stirring uniformly to obtain a mixed solution C. 0.5g of silver nitrate was dissolved in 10mL of water, then 0.1g of NaOH was added, and the mixture was stirred for 30 minutes to form a precipitate, and further 10wt% aqueous ammonia was added until the precipitate was completely dissolved to obtain a mixed solution D. And mixing and stirring the mixed solution C and the mixed solution D uniformly. Then 20mL of 5wt% hydrazine hydrate was added dropwise, and stirring was continued at room temperature for 12 hours after the addition was completed. Centrifuging at 7000r/min for 30min after the reaction is finished, collecting solid, washing with 100ml ethanol and 100ml deionized water, repeating for 6 times to obtain Ag@SiOj 2 。
Step 3, preparation of antireflection film of core-shell microstructure
Step 3.1, siO 2 Preparing an Ag coating: urethane acrylate (1 g), isooctyl acrylate (1 g), 1-hydroxycyclohexyl phenyl ketone (1 g), siO 2 Ag (0.5 g) and 5mL of ethanol solution were mixed together.
Step 3.2, ag@SiO 2 Preparing a coating: urethane acrylate (1 g), isooctyl acrylate (1 g), 1-hydroxycyclohexyl phenyl ketone (1 g), ag@SiO 2 (0.5 g) and 5mL of ethanol solution were mixed together.
Step 3.3, for SiO respectively 2 Ag coating and Ag@SiO 2 The paint is vacuumized to remove air. Transparent PET is taken as a carrier, and 1mLAg@SiO is sequentially and alternately dropwise coated on the surface of PET with the size of 5cm x5cm 2 Coating and 1mLSiO 2 After being uniformly spin-coated at 3000r/min, the @ Ag coating is put into an ultraviolet curing machine to be cured into a film, and then the core-shell structure reflective film (Ag@SiO2 and SiO2@Ag double-layer coated anti-reflective film, wherein SiO2@Ag is at the outermost layer) with the thickness of 0.4um is obtained, and the curing conditions in the ultraviolet curing machine are as follows: flash irradiation is carried out for 1 minute at 80 ℃, and the ultraviolet power is 80W.
Example 2
The difference from example 1 is that in step 3.3, the coating layers of ag@sio2 and sio2@ag coatings are different, and in example 2, four layers of ag@sio2 and sio2@ag coatings are alternately coated on the surface of PET, wherein sio2@ag is at the outermost layer;
comparative example 1
The difference from example 1 is that in step 3.3, the coating layers of the ag@sio2 and sio2@ag coatings are the same and the order is different, and in comparative example 1, the antireflection film is coated with two layers of ag@sio2 and sio2@ag, wherein ag@sio2 is the outermost layer;
comparative example 2
The difference from example 2 is that the coating layers of Ag@SiO2 and SiO2@Ag coatings are the same and different in sequence, and four layers of Ag@SiO2 and SiO2@Ag coatings are alternately coated on the surface of PET in comparative example 2, wherein Ag@SiO2 is the outermost layer;
comparative example 3
The difference from example 1 is that the number of coating layers of Ag@SiO2 and SiO2@Ag coatings is different; in comparative example 3, ag@SiO2 and SiO2@Ag coatings were applied alternately to the PET surface for a total of 3 layers, with Ag@SiO2 at the top layer
The coating structures of example 1, example 2 and comparative examples 1 to 3 are shown in table 1 below:
table 1 antireflection film laminate structure of core-shell microstructure
| First layer | Second layer | Third layer | Fourth layer | |
| Example 1 | Ag@SiO2 | SiO 2 @Ag | ||
| Example 2 | Ag@SiO 2 | SiO 2 @Ag | Ag@SiO 2 | SiO 2 @Ag |
| Comparative example 1 | SiO 2 @Ag | Ag@SiO 2 | ||
| Comparative example 2 | SiO 2 @Ag | Ag@SiO 2 | SiO 2 @Ag | Ag@SiO 2 |
| Comparative example 3 | Ag@SiO 2 | SiO 2 @Ag | Ag@SiO 2 |
In Table 1, the substrates of examples 1-2 were coated with 2 and 4 layers of coating, siO 2 Ag and Ag@SiO 2 Coating material alternate coating, structural feature SiO of examples 1-2 2 The @ Ag coatings are all at the outermost surface. Comparative examples 1-2 were coated with 2 and 4 layers of coating, ag@SiO 2 And SiO 2 Structural features of comparative examples 1-2 Ag@SiO 2 The coating is at the most surface. Comparative example 3 the substrate was coated with 3 layers of coating, ag@sioj 2 And SiO 2 Structural feature of comparative example 3 ag@sio 2 The coating is at the outermost surface.
Table 2 is an optical property test chart of the reflective films prepared in comparative examples 1 to 3 of example 1 and example 2.
Table 2 optical property characterization test of antireflection film
As can be seen from Table 2, the main expression is thatIn examples 1-2 SiO 2 The @ Ag is the outermost coating, and the outer layer Ag@SiO with low refractive index and high refractive index is formed 2 The forward scattering of light is favored, and the reflection of light is also very low, only 1.2 and 0.5, respectively. It was further found that an increase in the number of layers is advantageous for a reduction in light reflectance. The light reflectivity of comparative examples 1-3 was high, mainly because of the outermost layer Ag@SiO 2 The high Ag refractive index of (2) causes back scattering of light. The haze values of examples 1-2 were relatively low and the haze values of comparative examples 1-3 were high. In the same overlapping coating, the number of layers of the coating increases and the haze value increases.
The light-transmitting particles of core-shell structure shown in fig. 1 are used for a structural model and an optical motion model (a four-layer coating structure is taken as an example for illustration), the number of coating layers is sequentially up from a substrate, the light-transmitting particles in each layer are core-shell particles formed by Ag and SiO2, the refractive index of Ag is 1.76, and the refractive index of SiO2 is 1.45, so that the light-transmitting particles of the core-shell structure are all heterogeneous media, and light scattering can be formed.
FIG. 2 measurement of Ag, siO2 and SiO by laser dynamic scattering instrument 2 Ag and Ag@SiO 2 The hydraulic radii of the four materials were found to be 0.51 and 0.33um for the prepared Ag and SiO2 particles, respectively, whereas they increased to 0.71 and 0.60um, respectively, after coating (synthesis of the raw materials, indicating successful preparation of the core-shell structure).
FIG. 3 is a graph showing the transmittance ratio of the anti-reflective coatings prepared in examples 1 and 2 and comparative examples 1 to 3 according to the method for preparing an anti-reflective coating using core-shell microstructure light-transmitting particles of the present invention, and FIG. 3 shows that the transmittance ratio of examples 1 to 2 is high, mainly because of the use of SiO 2 The @ Ag is the outermost coating, and the outer layer Ag@SiO with low refractive index and high refractive index is formed 2 The forward scattering of light is facilitated, and the light transmittance is improved. The light transmittance of comparative examples 1-3 was low, mainly because of the outermost layer Ag@SiO 2 The high Ag refractive index of (2) causes back scattering of light.
Example 3
Step 1, silicon dioxide coated silver material (SiO 2 @ Ag) was prepared
Step 1.1, dissolving 3.4g of silver nitrate in 10mL of water, then adding 0.6g of NaOH, stirring for 60min to form a precipitate, further adding 20wt% of ammonia water until the precipitate is completely dissolved, adding 2g of polyvinylpyrrolidone (template agent), stirring uniformly, adding 5mL of 30wt% of hydrazine hydrate (reducing agent) solution, stirring for 24h at room temperature, and centrifuging at a rotating speed of 10000r/min after the reaction is finished to obtain silver particles.
Step 1.2, 2g of silver particles were dispersed in 300mL of glycerol, 0.2g of sodium dodecyl sulfonate as a surfactant was added, then 5g of tetraethyl orthosilicate and 1.6g of NaOH were added, and stirring was continued for 24 hours. After the reaction is finished, centrifuging at 10000r/min, washing with 200mL of ethanol and 200 deionized water, and repeating six times to obtain SiO 2 Material @ Ag.
Step 2, silver coated silica (Ag@SiO) 2 ) Is prepared from
Step 2.1, adding 0.5g of surfactant sodium dodecyl sulfonate into 250mL of deionized water of 1g of tetraethyl orthosilicate, and uniformly stirring to obtain a mixed solution A; then, 0.1g of sodium ethoxide was dissolved in 500mL of ethanol to obtain a mixed solution B. Solution A was added dropwise (drop rate: 0.5 d/s) to solution B, and after the addition was completed, the reaction was carried out at room temperature for 24 hours. After the reaction, the mixture is centrifuged for 60 minutes at 10000r/min, and the solid is collected, washed with 200ml of ethanol and 200ml of deionized water, and repeated for 6 times to obtain silica particles.
And 2.2, dissolving 0.05g of 3-mercaptopropyl trimethoxy silane into 200mL of ethanol solution, adding 1g of silicon dioxide particles, stirring and reacting for 2h, activating the surfaces of the silicon dioxide particles, continuously adding 1g of polyvinylpyrrolidone (template agent), and stirring uniformly to obtain a mixed solution C. 1g of silver nitrate was dissolved in 10mL of water, then 1g of NaOH was added, and stirring was performed for 60min to form a precipitate, and 20wt% aqueous ammonia was further added until the precipitate was completely dissolved to obtain a mixed solution D. And mixing and stirring the mixed solution C and the mixed solution D uniformly. Then 30mL of 10wt% hydrazine hydrate was added dropwise, and stirring was continued at room temperature for 24 hours after the addition was completed. Centrifuging at 10000r/min for 60min after the reaction is finished, collecting solid, washing with 200ml ethanol and 200ml deionized water, repeating for 6 times to obtain Ag@SiO 2 。
Step 3, preparation of antireflection film of core-shell microstructure
Step 3.1, siO 2 Preparing an Ag coating: urethane acrylate (2 g), isooctyl acrylate (2 g), 1-hydroxycyclohexyl phenyl ketone (2 g), siO 2 Ag (1 g) and 10mL of ethanol solution were mixed together.
Step 3.2, ag@SiO 2 Preparing a coating: urethane acrylate (2 g), isooctyl acrylate (2 g), 1-hydroxycyclohexyl phenyl ketone (2 g), ag@SiO 2 (1g) 10mL of ethanol solution was mixed together.
Step 3.3, for SiO respectively 2 Ag coating and Ag@SiO 2 The paint is vacuumized to remove air. Transparent PET is taken as a carrier, and 2mLAg@SiO is sequentially and alternately dropwise added and coated on the surface of PET with the size of 5cm x and 5cm 2 Coating and 2mLSiO 2 After spin coating at 1000r/min, uniformly spin coating, putting into an ultraviolet curing machine for curing to form a film, thus obtaining a core-shell structure reflective film (Ag@SiO2 and SiO2@Ag double-layer coated anti-reflective film, wherein SiO2@Ag is at the outermost layer), and the curing conditions in the ultraviolet curing machine are as follows: flash irradiation is carried out for 2 minutes at 120 ℃, and the ultraviolet power is 120W.
Example 4
Step 1, silicon dioxide coated silver material (SiO 2 @ Ag) was prepared
Step 1.1, dissolving 2g of silver nitrate in 10mL of water, then adding 0.5g of NaOH, stirring for 50min to form a precipitate, further adding 15wt% of ammonia water until the precipitate is completely dissolved, adding 1.5g of polyvinylpyrrolidone (template agent), stirring uniformly, adding 3mL of 28wt% of hydrazine hydrate (reducing agent) solution, stirring for 18h at room temperature, and centrifuging at a rotating speed of 8000r/min after the reaction is finished to obtain silver particles.
Step 1.2, 1.5g of silver particles were dispersed in 200mL of glycerol, 0.15g of sodium dodecyl sulfate as a surfactant was added, and then 4g of tetraethyl orthosilicate and 1.2g of NaOH were added, followed by stirring for 20 hours. After the reaction is finished, centrifuging at 8000r/min, washing with 150mL of ethanol and 150 deionized water, and repeating six times to obtain SiO 2 Material @ Ag.
Step 2, silver coated silica (Ag@SiO) 2 ) Is prepared from
Step 2.1, adding 0.4g of surfactant sodium dodecyl sulfonate into 400mL of deionized water of 0.8g of tetraethyl orthosilicate, and uniformly stirring to obtain a mixed solution A; then, 0.08g of sodium ethoxide was dissolved in 800mL of ethanol to obtain a mixed solution B. Solution A was added dropwise (drop rate: 0.5 d/s) to solution B, and after the addition was completed, the reaction was carried out at room temperature for 20 hours. After the reaction, the mixture is centrifuged for 50 minutes at 8000r/min, and the solid is collected, washed with 150ml of ethanol and 150ml of deionized water, and repeated 6 times to obtain silica particles.
And 2.2, dissolving 0.03g of 3-mercaptopropyl trimethoxy silane into 150mL of ethanol solution, adding 0.8g of silicon dioxide particles, stirring and reacting for 1.5h, activating the surfaces of the silicon dioxide particles, continuously adding 0.8g of polyvinylpyrrolidone (template agent), and stirring uniformly to obtain a mixed solution C. 0.8g of silver nitrate was dissolved in 10mL of water, then 0.8g of NaOH was added, and the mixture was stirred for 50 minutes to form a precipitate, and 15wt% aqueous ammonia was further added until the precipitate was completely dissolved to obtain a mixed solution D. And mixing and stirring the mixed solution C and the mixed solution D uniformly. Then 25mL of 8wt% hydrazine hydrate was added dropwise, and stirring was continued at room temperature for 20h after the addition was completed. Centrifuging at 7000r/min for 50min after the reaction is finished, collecting solid, washing with 150ml ethanol and 150ml deionized water, repeating for 6 times to obtain Ag@SiOj 2 。
Step 3, preparation of antireflection film of core-shell microstructure
Step 3.1, siO 2 Preparing an Ag coating: urethane acrylate (1.5 g), isooctyl acrylate (1.5 g), 1-hydroxycyclohexyl phenyl ketone (1.5 g), siO 2 Ag (0.8 g) and 8mL of ethanol solution were mixed together.
Step 3.2, ag@SiO 2 Preparing a coating: urethane acrylate (1.5 g), isooctyl acrylate (1.5 g), 1-hydroxycyclohexyl phenyl ketone (1.5 g), ag@SiO 2 (0.8 g) and 8mL of ethanol solution were mixed together.
Step 3.3, for SiO respectively 2 Ag coating and Ag@SiO 2 The paint is vacuumized to remove air. Transparent PET is taken as a carrier, and 1.5 mM LAg@SiO is sequentially and alternately dripped and coated on the surface of PET with the size of 5cm x and 5cm 2 Coating and 1.5mLSiO 2 The @ Ag coating is uniformly spin-coated at the rotating speed of 2000r/min and then is put into an ultraviolet curing machine to be cured into a film,the core-shell structure reflective film (Ag@SiO2 and SiO2@Ag double-layer coated anti-reflective film, wherein SiO2@Ag is at the outermost layer) with the thickness of 0.5um is obtained, and the curing conditions in an ultraviolet light photo-generator are as follows: flash irradiation is carried out for 1.5 minutes at the temperature of 100 ℃, and the ultraviolet power is 100W.
Claims (5)
1. The method for preparing the antireflection film by adopting the core-shell microstructure light-transmitting particles is characterized by comprising the following steps of: the method specifically comprises the following steps:
step 1, silicon dioxide coating silver material SiO 2 @Ag；
Step 2, preparing silver coated silicon dioxide Ag@SiO 2 ；
And 3, preparing a coating according to the products obtained in the step 1 and the step 2, and preparing the anti-reflection film with the core-shell microstructure.
2. The method for producing an antireflection film using core-shell microstructured light-transmitting particles according to claim 1, characterized in that: the specific process of the step 1 is as follows:
1.1, dissolving 1.7g-3.4g of silver nitrate in 10mL of water, then adding 0.4g-0.6g of NaOH, stirring for 30min-60min to form a precipitate, adding 10wt% -20wt% of ammonia water to the precipitate until the precipitate is completely dissolved, then adding 1g-2g of polyvinylpyrrolidone, stirring uniformly, adding 2.5mL-5mL of 25wt% -30wt% of hydrazine hydrate solution, stirring for 12h-24h at room temperature, and centrifuging at a rotating speed of 7000r/min-10000r/min after the reaction is finished to obtain silver particles;
step 1.2, dispersing 1g-2g of silver particles into 150mL-300mL of glycerol, adding 0.1g-0.2g of surfactant sodium dodecyl sulfonate, then adding 2.5g-5g of tetraethyl orthosilicate and 0.8g-1.6g of NaOH, continuing stirring for 12h-24h, centrifuging at a rotating speed of 7000r/min-10000r/min after the reaction is finished, washing with 100mL-200mL of ethanol and 100mL-200mL of deionized water, and repeating six times to obtain the silicon dioxide coated silver material SiO 2 Material @ Ag.
3. The method for producing an antireflection film using core-shell microstructured light-transmitting particles according to claim 1, characterized in that: the specific process of the step 2 is as follows:
step 2.1, preparing silicon dioxide particles;
2.2, dissolving 0.01g-0.05g of 3-mercaptopropyl trimethoxy silane into 100mL-200mL of ethanol solution, then adding 0.5g-1g of silica particles, stirring and reacting for 1h-2h, activating the surfaces of the silica particles, continuously adding 0.5g-1g of polyvinylpyrrolidone, and stirring uniformly to obtain a mixed solution C;
2.3, dissolving 0.5g-1g of silver nitrate in 10mL of water, then adding 0.1g-1g of NaOH, stirring for 30min-60min to form a precipitate, and then adding 10wt% -20wt% of ammonia water until the precipitate is completely dissolved to obtain a mixed solution D;
step 2.4, mixing and stirring the mixed solution C and the mixed solution D uniformly, then dropwise adding 20-30mL of 5-10wt% hydrazine hydrate, continuously stirring at room temperature for 12-24h after the dropwise adding is finished, centrifuging for 30-60min by 7000-10000r/min after the reaction is finished, collecting solids, washing the solids by 100-200mL of ethanol and 100-200mL of deionized water, and repeating for 6 times to obtain silver-coated silica Ag@SiO 2 。
4. The method for producing an antireflection film using core-shell microstructured light-transmitting particles according to claim 3, wherein: the specific process of the step 2.1 is as follows:
step 2.1.1, adding 0.3g-0.5g of surfactant sodium dodecyl sulfonate into 250mL-500mL of deionized water with 0.5g-1g of tetraethyl orthosilicate, and uniformly stirring to obtain a mixed solution A;
2.1.2, dissolving 0.05g-0.1g of sodium ethoxide in 500mL-1000mL of ethanol to obtain a mixed solution B;
step 2.1.3, dropwise adding the solution A into the solution B, reacting for 12-24 hours at room temperature after the dropwise adding is finished, centrifuging for 30-60 minutes at 7000-10000r/min after the reaction is finished, collecting solid, washing with 100-200ml ethanol and 100-200ml deionized water, and repeating for 6 times to obtain the silicon dioxide particles.
5. The method for producing an antireflection film using core-shell microstructured light-transmitting particles according to claim 1, characterized in that: the specific process of the step 3 is as follows:
step 3.1, 1g to 2g of urethane acrylate, 1g to 2g of isooctyl acrylate, 1g to 2g of 1-hydroxycyclohexyl phenyl ketone, 0.5g to 1g of SiO 2 Mixing @ Ag and 5-10mL ethanol solution to obtain SiO 2 An @ Ag coating;
step 3.2, 1g-2g of polyurethane acrylate, 1g-2g of isooctyl acrylate, 1g-2g of 1-hydroxycyclohexyl phenyl ketone, 0.5g-1g of Ag@SiO 2 Mixing 5mL-10mL ethanol solution to obtain Ag@SiO 2 A coating;
step 3.3, using transparent PET as a carrier, and using the SiO prepared in the step 3.1 2 Ag@Ag coating and Ag@SiO prepared in step 3.2 2 The coating is sequentially and alternately dripped and coated on the surface of PET with the size of 5cmx5cm, spin-coated uniformly at the rotating speed of 1000r/min-3000r/min, and then is put into an ultraviolet curing machine to be cured into a film, so that the core-shell structure reflective film with the thickness of 0.4um-0.7um is obtained, and the curing conditions in the ultraviolet curing machine are as follows: flash irradiation for 1-2 min at 80-120deg.C, and ultraviolet power of 80-120W.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100806915B1 (en) * | 2006-10-10 | 2008-02-22 | 요업기술원 | Silver coated silica, method of making the same, and products using the same |
| KR20120138195A (en) * | 2011-06-14 | 2012-12-24 | 한국과학기술원 | Hollow silica particles, method of preparing the same and low-reflection coatings using the same |
| KR101410239B1 (en) * | 2013-05-07 | 2014-06-24 | 국립대학법인 울산과학기술대학교 산학협력단 | Polymer solar cell comprising silica-coated silver nanoparticles |
| CN108085987A (en) * | 2017-12-15 | 2018-05-29 | 上海工程技术大学 | A kind of aqueous sterilization finishing agent based on modified Nano silver, preparation method and application |
| CN108250873A (en) * | 2018-03-22 | 2018-07-06 | 深圳瑞凌新能源科技有限公司 | The round-the-clock sun light reflection of outdoor use and infra-red radiation refrigeration coating |
| CN109280389A (en) * | 2018-08-06 | 2019-01-29 | 青岛科技大学 | A kind of preparation method of Nano silver grain Composite silicone resin |
| CN209071007U (en) * | 2018-10-23 | 2019-07-05 | 惠州市天誉科技有限公司 | A kind of ITO conductive film structure of low-resistance high transmittance |
-
2023
- 2023-07-31 CN CN202310945275.1A patent/CN116715890B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100806915B1 (en) * | 2006-10-10 | 2008-02-22 | 요업기술원 | Silver coated silica, method of making the same, and products using the same |
| KR20120138195A (en) * | 2011-06-14 | 2012-12-24 | 한국과학기술원 | Hollow silica particles, method of preparing the same and low-reflection coatings using the same |
| KR101410239B1 (en) * | 2013-05-07 | 2014-06-24 | 국립대학법인 울산과학기술대학교 산학협력단 | Polymer solar cell comprising silica-coated silver nanoparticles |
| CN108085987A (en) * | 2017-12-15 | 2018-05-29 | 上海工程技术大学 | A kind of aqueous sterilization finishing agent based on modified Nano silver, preparation method and application |
| CN108250873A (en) * | 2018-03-22 | 2018-07-06 | 深圳瑞凌新能源科技有限公司 | The round-the-clock sun light reflection of outdoor use and infra-red radiation refrigeration coating |
| CN109280389A (en) * | 2018-08-06 | 2019-01-29 | 青岛科技大学 | A kind of preparation method of Nano silver grain Composite silicone resin |
| CN209071007U (en) * | 2018-10-23 | 2019-07-05 | 惠州市天誉科技有限公司 | A kind of ITO conductive film structure of low-resistance high transmittance |
Non-Patent Citations (1)
| Title |
|---|
| 陈名等: "纳米球和核壳纳米球对有机太阳能电池光吸收增强效果的研究", 《人工晶体学报》, vol. 46, no. 3, 31 March 2017 (2017-03-31), pages 501 - 506 * |
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