CN102565885A - Hardened optical thin film and preparation method thereof - Google Patents
Hardened optical thin film and preparation method thereof Download PDFInfo
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- CN102565885A CN102565885A CN2011104128458A CN201110412845A CN102565885A CN 102565885 A CN102565885 A CN 102565885A CN 2011104128458 A CN2011104128458 A CN 2011104128458A CN 201110412845 A CN201110412845 A CN 201110412845A CN 102565885 A CN102565885 A CN 102565885A
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Abstract
The invention discloses a hardened optical thin film. A hardened coating with good optical property is uniformly coated on a transparent thin film base material. The hardened coating consists of 10-90 parts of ultraviolet curable resin, 10-30 parts of ultraviolet solid activity diluted resin, 2-15 parts of light initiator, 0-3 parts of flatting agent, and 10-90 parts of solvent. The hardened optical thin film disclosed by the invention has the advantages as follows: 1, the polyester has higher heat resistance, higher melting point and controllable degradation speed; 2, titanium dioxide sediments cannot be formed in a production process since the use amount of catalyst is small, so that the maintenance and replacement period of production equipment can be prolonged; 3, the vertical and transverse tearing intensities of the polyester material are higher; and 4, the structure of the polyester is easy to control, gel is difficult to form in a reaction process, and the processed film material has no crystal points which are formed by the gel.
Description
Technical field
The present invention relates to a kind of preparation method of optical thin film, especially a kind of preparation method with optical thin film of higher hardness.
Background technology
In recent years, the fast development along with the liquid crystal display industry is widely used in daily life such as products such as smart mobile phone, touch-screens, therefore light and thin type optical clear plastic sheeting demand is also grown with each passing day.But present most of plastic sheetings surface causes outward appearance to wipe flower or cut through contacting with each other friction easily; For this reason in the plastic sheeting surface-coated or electroplate one deck hard conating and just receiving the favor in market, the optics of handling through surperficial stiffened gathers protection panel or the flexible ITO film that film can be widely used in touch screen and uses backing material.
At present; The method that the polyester film surface stiffened is handled mainly contains two kinds; A kind of main employing electroplating surface deposition one deck inorganic oxide film, for example silicon dioxide, antimony oxide etc., this coating hardness is high; But the filming equipment investment is big, and the relatively poor and flexible difference of inorganics sedimentary deposit adhesion chaps easily; A kind of in addition mainly is the high organic polymer resin of surface-coated one deck hardness, and this method coating is easily simple and pliability is better, is widely used in the volume to volume film.
Chinese patent 200910105659.2 discloses a kind of display touch screen structure and preparation method thereof; Its structure comprises basic unit's chemically reinforced glass, upper strata conductive layer and lower floor's conductive layer; And on the upper strata conductive layer PET film surface is provided with and adds hard formation, its advantage is, directly ito thin film is made in the chemically reinforced glass surface; Technology for manufacturing touch screen is simplified and the yield of product improves; The intensity that guarantees chemically reinforced glass does not simultaneously change, and its weak point is that transmittance damages to some extent and adhesion descends obviously.
Summary of the invention
The present invention aims to provide a kind of high transmission rate that has, the mylar that the stiffened of excellent weather resistance is handled, and another object of the present invention provides a kind of preparation method.
A kind of stiffened optical polyester film; The hard conating that adds that one deck excellent optical performance is arranged on the transparent membrane base material, the said component that adds hard conating is by consolidating active letdown resin, 2～15 parts of light triggers, 0～3 part of levelling agent, 10～90 parts of solvent compositions by 10～90 parts UV-cured resin, 10～30 parts ultraviolet light.
Above-mentioned film substrate can be transparent or opaque, preferably clear; Such as mylar, like polyethylene terephthalate, polyphenyl dioctyl phthalate fourth diester with gather dioctyl phthalate ethyl film, polyethylene film; Polypropylene film, viscose paper, diacetyl cellulose film, tri acetyl cellulose film; Butyric acid acetylcellulose film, polyvinyl chloride film, Vingon film, polyvinyl alcohol film; The ethylene-vinyl acetate copolymer film, polystyrene film, polycarbonate film, poly-methyl pentene film; Polysulphone film, Kapton, fluorine resin film, polyamide film and acryl resin film.
Above-mentioned film substrate, its thickness can be selected according to self-demand, and scope can be from 50um～300um, preferred 100um～250um.
Above-mentioned stiffened coating ingredients, its resin can be acrylic resin, urethane resin, vibrin, aldehyde ketone resin or its composition.
Above-mentioned stiffened coating ingredients, said solvent can be ethyl acetate, MEK, propylene glycol monomethyl ether, butyl acetate, toluene, normal hexane, isopropyl alcohol or its potpourri; In order to guarantee good appearance of film and to consider the dissolubility to other components of system, the butyl acetate that preferred surface tension force is lower, MEK, ethyl acetate, propylene glycol monomethyl ether or its potpourri.
In the above-mentioned stiffened coating formula, UV-cured resin A can comprise epoxy acrylate, polycarbamate acrylic ester, polyether acrylate and polyester acrylate, uv curable oligomer can use separately or two kinds be used in combination.
In the above-mentioned stiffened coating formula, ultraviolet light polymerization activated monomer resin B comprises simple function group and polyfunctional acrylic ester, like (methyl) methyl acrylate; IBOA, 1, the 4-butanediol ester; (methyl) acrylic acid 1,6-hexylene glycol ester, two (methyl) acrylic acid DOPCP; Two (methyl) polyalkylene glycol acrylate ester, ethane diacid (methyl) acrylic acid DOPCP, three (methyl) acrylic acid dipentaerythritol ester; Three (methyl) acrylic acid pentaerythritol ester, above-mentioned uv-curable monomer can use separately or two or more combinations are used, and the uV curable monomer can be used in combination with above-described uV curable prepolymer.
At stiffened coating ingredients of the present invention; Being fit to light trigger of the present invention can be 1-hydroxyl-cyclohexyl benzophenone (Irgacure184), styrax dimethyl ether, 2-hydroxyl-1-phenylacetone-1 (Irgacure1173), 2-methyl isophthalic acid-(4-methyl mercapto phenyl)-2-morpholine-1-acetone (Irgacure907), 2; 4; 6-trimethylbenzene formyl dimethyl oxidation phosphine (TPO), isopropyl thioxanthone, 4-methyldiphenyl ketone (4-BPZ), benzyl dimethyl amino ethyl ester, 4-dimethyl ethyl aminobenzoate, 2-originally increase the interest amino benzoic Acid potassium ester or their potpourri, preferred 1-hydroxyl-cyclohexyl benzophenone (Irgacure184), 2-hydroxy-2-methyl-1-phenylacetone-1 (Irgacure1173), 2-methyl isophthalic acid-(4-methyl mercapto phenyl)-2-morpholine-1-acetone (Irgacure907) or their potpourri.
Above-mentioned stiffened coating ingredients, levelling agent can be polyether-modified dimethyl silicone polymer, polyester modification dimethyl silicone polymer, alkyl (aralkyl) modified dimethyl polysiloxane; The preferred, polyethers modified dimethyl polysiloxane.
A kind of optics stiffened mylar of the present invention can prepare through following method:
Each component UV-cured resin, light trigger, levelling agent and the solvent of hardening liquid prescription be added in a mixing bowl after according to the accurate weighing of its corresponding ratio stir; Obtain the stiffened coating liquid; Then its vacuum defoamation is handled; With after the vacuum defoamation the stiffened coating liquid evenly be coated on the selected mylar base material and through the baking oven baking with solvent evaporates; The ultraviolet light polymerization of resin solidification institute energy requirement and form certain thick hard conating that adds of doing then, thus the mylar that the optical grade stiffened is handled obtained.
The baking oven roasting mode that the present invention adopts can be Steam Heating, heating wire heating, Infrared Heating, and preferred Infrared Heating is can be with solvent evaporates clean and help the coating levelling.
The coating method that the present invention uses can adopt that the extruding of bar seam is coated with, blade coating, showering, nick rubbing method, preferred nick rubbing method.
Optics stiffened mylar according to the invention, its advantage is:
1. on the transparent membrane base material, scribble the hard conating that adds of one deck excellent optical performance, can keep like this strengthening its substrate intensity under the transparent prerequisite of base material;
2. adopt multiple disposal route, can guarantee all even effect that applies;
3. the mylar after stiffened is handled has the high transmission rate low haze; And its performance can not change under high temperature, cold cycling and hot and humid condition; Can not produce yet, promptly have very much good weatherability such as phenomenons such as perk, whiting, xanthochromias; Especially as ITO film substrate, during the high temperature dehumidification treatments, this stiffened processing layer can prevent the problem that the surperficial external migration of oligomer causes mist degree sharply to raise in the mylar, and improves the adhesion of sputtering ITO to ground before sputtering ITO.
The instantiation mode
Below in conjunction with instance invention is further specified, but the scope that the present invention requires to protect is not limited to these embodiment.
Embodiment 1
Place stirred tank fully to mix 15 parts of UV-cured resins, the active letdown resin of 30 parts of ultraviolet light polymerizations, 5 parts of Irgacure184,0.5 part of levelling agent and 25 parts of ethyl acetate, butyl acetate and 10 parts of propylene glycol monomethyl ethers of 15 parts, what obtain that stiffened handles adds the hard conating coating fluid.
Coating fluid evenly is coated on the surface of mylar base material with the nick rubbing method, the hard conating that the formation stiffened is handled through Infrared Heating is clean with solvent evaporates is through 1000mj/cm
2Energy ultraviolet ray irradiation is solidified, and obtains the mylar that stiffened is handled.Survey its performance (seeing table 1 for details)
Embodiment 2
Place stirred tank fully to mix 20 parts of UV-cured resins, the active letdown resin of 25 parts of ultraviolet light polymerizations, 5 parts of Irgacure184,0.5 part of levelling agent and 25 parts of ethyl acetate, butyl acetate and 10 parts of propylene glycol monomethyl ethers of 15 parts, what obtain that stiffened handles adds the hard conating coating fluid.
Method of application is with embodiment 1, and the result sees table 1 for details
Embodiment 3
Place stirred tank fully to mix 30 parts of UV-cured resins, the active letdown resin of 15 parts of ultraviolet light polymerizations, 5 parts of Irgacure184,0.5 part of levelling agent and 25 parts of ethyl acetate, butyl acetate and 10 parts of propylene glycol monomethyl ethers of 15 parts, what obtain that stiffened handles adds the hard conating coating fluid.
Method of application is with embodiment 1, and the result sees table 1 for details
Comparative Examples 1
Place stirred tank fully to mix in 15 parts of UV-cured resins, the active letdown resin of 30 parts of ultraviolet light polymerizations, 5 parts of Irgacure184 and 50 parts of ethyl acetate, what obtain that stiffened handles adds the hard conating coating fluid.
Method of application is with embodiment 1, and the result sees table 1 for details
Comparative Examples 2
Place stirred tank fully to mix 5 parts of UV-cured resins, the active letdown resin of 40 parts of ultraviolet light polymerizations, 5 parts of Irgacure184,0.5 part of levelling agent and 25 parts of ethyl acetate, butyl acetate and 10 parts of propylene glycol monomethyl ethers of 15 parts, what obtain that stiffened handles adds the hard conating coating fluid.
Method of application is with embodiment 1, and the result sees table 1 for details
The method of testing of each item performance:
(1) outward appearance coating
Observe the final outer light of coating,, be designated as paintability " * " if unit square rice has shrinkage cavity or brilliant point etc. more than 10; If unit square rice has shrinkage cavity or brilliant point etc. to surpass less than 10 but more than 3, be designated as paintability " △ "; If unit square rice has shrinkage cavity or brilliant point etc. to surpass less than 3, be designated as paintability " zero ".
(2) transmittance/mist degree
See through the WGT-S test perhaps with spectrophotometer (Tianjin, island makes UV3100, measures 550nm) test.
(3) pencil hardness
According to " GB/T6739-1996 film determination of pencil hardness method " testing coating hardness.
(4) adhesion
According to standard GB 1720-89 test, draw lattice 100 (1mm * 1mm), use the 3M600 adhesive tape test with sharp cutter.
(5) anti-scratch performance
At hard coating surface the steel wool of #0000 is set, and, is expressed as " zero " to the item of no marking through visual cut number of counting because the firmness testing machine increases the weight of 24.5kpa the hard coating surface after coming and going for 100 times.The item that is less than cut 10 is expressed as " △ ", is expressed as " * " to cut greater than 10 item.
(6) heat-shrinkable
According to GB/T 13519-1992, its heat-resisting shrinkability of tygon heat-shrinkable film standard testing: test condition: 150 ℃ * 30min; Available film thermal shrinkage appearance is measured.
(7) resistance to bend(ing)
According to JISK5400; With the hard coat film of 150mm*150mm at angular distortion around about 180 degree of axle with special diameter; Wherein the surface of hard conating outwards; Then, hard conating turns back to the cracking of original position hard conating and peels off and sees through visual judgement, produces the minimum diameter that ftractures and peel off and is expressed as resistance to bend(ing) (mm of unit)
(8) impressionability
According to an ASTMSTD D6182 standard dyne test surfaces tension force,, be designated as " zero " when surface tension has had good printing greater than 48 dyne/cm; When surface tension circle has had general printing in 42～48 dyne/cm, be designated as " △ "; Relatively poor when surface tension less than 42 dyne/cm printing, be designated as " * "
(9) migration of oligomer
Stiffened is handled optical polyester film as for 150 ℃ * 30min, take out then and observe outward appearance atomizing (this aerosol can be removed with organic solvent) situation, the surface is serious if atomizing seriously shows the film oligomer migration, is designated as " * "; If there is slight atomizing to show that the film oligomer has a small amount of migration surface, is designated as " △ "; If not having atomizing then showing does not have the oligomer migration surface, be designated as " zero ".
The performance measurement result of table 1 embodiment and Comparative Examples
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative Examples 1 | Comparative Examples 2 |
| The outward appearance coating | ○ | ○ | ○ | × | ○ |
| The all fronts transmittance | 91.5% | 91.6% | 91.4% | 91.3% | 91.5% |
| Mist degree | 0.21% | 0.35% | 0.26% | 0.23% | 0.18% |
| b * | 1.03 | 1.04 | 1.02 | 1.01 | 1.05 |
| Pencil hardness | 3H | 2H | H | 3H | 4H |
| Adhesion | 100/100 | 100/100 | 100/100 | 100/100 | 100/100 |
| The anti-scratch performance | ○ | △ | × | ○ | ○ |
| Thermal contraction performance | 0.3% | 0.2% | 0.1% | 0.3% | 0.5% |
| The resistance to bend(ing) ability | φ15mm | φ15mm | φ10mm | φ15mm | φ20mm |
| Impressionability | ○ | ○ | △ | △ | ○ |
| The migration of oligomer | ○ | △ | × | ○ | ○ |
Can find out from table 1; Its optical property of mylar and the coating machine performance of passing through surperficial hardening liquid processing in the instance are all good; Effectively customer service problems such as organic oxygen compound coating embrittlement, can be extensively because the flexible panel that shows be protected and the substrate of flexible ITO film.
The present invention has carried out detailed description with reference to concrete embodiment; Above embodiment; Be not that the content of composition of the present invention is done any restriction; Every according to technical spirit of the present invention or composition components or content to any trickle modification, equivalent variations and modification that above embodiment did, all belong in the scope of technical scheme of the present invention.
Claims (9)
1. a stiffened optical thin film is characterized in that: the hard conating that adds that one deck excellent optical performance is arranged on the transparent membrane base material; The said hard conating that adds, by 10～90 parts UV-cured resin, 10～30 parts ultraviolet light is active letdown resin admittedly, 2～15 parts of light triggers, 0～3 part of levelling agent, 10～90 parts of solvent compositions by weight.
2. according to the said stiffened optical thin film of claim 1; It is characterized in that: said transparent membrane base material is polyethylene film, polypropylene screen, ethylene-propylene copolymer film, polyester film, polyethylene terephthalate film, polychloroethylene film or polyvinyl acetate (PVA) film, and its thickness is 50～300um.
3. according to the said stiffened optical thin film of claim 1, it is characterized in that said UV-cured resin can be one or more the potpourri in esters of acrylic acid prepolymer, epoxies prepolymer, polyurethane prepolymers, the silicone based prepolymer.
4. according to the said stiffened mylar of claim 1; It is characterized in that; The active letdown resin of said ultraviolet light polymerization can be simple function group or multi-functional acrylate's class monomer or resin, comprises methyl methacrylate, IBOA, 1,6 hexanediol diacrylate; Propylene glycol diacrylate, a kind of or its potpourri in tripropylene glycol diacrylate, the trimethylolpropane triacrylate.
5. according to the said stiffened optical thin film of claim 1, it is characterized in that said light trigger can be styrax dimethyl ether, 2-hydroxyl-1-phenylacetone-1,1-hydroxyl-cyclohexylbenzene ketone compounds or its potpourri.
6. according to the said stiffened optical thin film of claim 1, it is characterized in that said levelling agent can be polyether-modified dimethyl silicone polymer, polyester modification dimethyl silicone polymer, alkyl (aralkyl) modified dimethyl polysiloxane.
7. according to the said stiffened optical thin film of claim 1, it is characterized in that said solvent can be ethyl acetate, butyl acetate, MEK, toluene, propylene glycol monomethyl ether or its potpourri.
8. the method for preparing the said stiffened optical thin film of claim 1-6; Its step is following: each component UV-cured resin, light trigger, levelling agent and the solvent of hardening liquid prescription is added in a mixing bowl after according to the accurate weighing of its corresponding ratio stirs; Obtain the stiffened coating liquid; Then its vacuum defoamation is handled; With after the vacuum defoamation the stiffened coating liquid evenly be coated on the selected mylar base material and through the baking oven baking with solvent evaporates, the ultraviolet light polymerization of resin solidification institute energy requirement and form certain thick hard conating that adds of doing then, thus obtain the mylar that the optical grade stiffened is handled.
9. according to claims 7 said methods that prepare the stiffened optical thin film, it is characterized in that coating can adopt nick roller coating, spraying, showering, blade coating, the extruding of bar seam to be coated with.
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| CN102766428A (en) * | 2012-08-08 | 2012-11-07 | 番禺南沙殷田化工有限公司 | Ultraviolet curable resin composition and application thereof |
| CN102786875A (en) * | 2012-08-27 | 2012-11-21 | 杭州惠之星科技有限公司 | Anti-static hardened film |
| CN103194233A (en) * | 2013-03-29 | 2013-07-10 | 上海师范大学 | Preparation method of blue/purple long-distance triggered LED (Light Emitting Diode) white-light emitting illumination material |
| CN106147636A (en) * | 2015-04-01 | 2016-11-23 | 上海精涂新材料技术有限公司 | A kind of hardening protecting film and production method thereof |
| CN106279737A (en) * | 2016-08-12 | 2017-01-04 | 苏州柯创电子材料有限公司 | A kind of PET protection film with excellent anti-scratch performance |
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| CN115464955A (en) * | 2020-12-09 | 2022-12-13 | 黎银茵 | PVC composite membrane with high visible light catalytic activity |
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| CN102766428A (en) * | 2012-08-08 | 2012-11-07 | 番禺南沙殷田化工有限公司 | Ultraviolet curable resin composition and application thereof |
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| CN102786875A (en) * | 2012-08-27 | 2012-11-21 | 杭州惠之星科技有限公司 | Anti-static hardened film |
| CN102786875B (en) * | 2012-08-27 | 2015-06-24 | 宁波惠之星新材料科技有限公司 | Anti-static hardened film |
| CN103194233A (en) * | 2013-03-29 | 2013-07-10 | 上海师范大学 | Preparation method of blue/purple long-distance triggered LED (Light Emitting Diode) white-light emitting illumination material |
| CN106147636A (en) * | 2015-04-01 | 2016-11-23 | 上海精涂新材料技术有限公司 | A kind of hardening protecting film and production method thereof |
| CN106279737A (en) * | 2016-08-12 | 2017-01-04 | 苏州柯创电子材料有限公司 | A kind of PET protection film with excellent anti-scratch performance |
| CN107976830B (en) * | 2016-10-21 | 2022-05-24 | 三星电子株式会社 | Plastic substrate and display device including the same |
| CN107976830A (en) * | 2016-10-21 | 2018-05-01 | 三星电子株式会社 | Plastic base and the display device for including it |
| CN106634462A (en) * | 2016-12-23 | 2017-05-10 | 合肥乐凯科技产业有限公司 | Hard coating film with high dyne value |
| CN106634462B (en) * | 2016-12-23 | 2018-12-14 | 合肥乐凯科技产业有限公司 | One kind is up to because being worth cured film |
| CN108928073A (en) * | 2018-05-30 | 2018-12-04 | Oppo（重庆）智能科技有限公司 | Composite board and preparation method thereof, shell and electronic equipment |
| CN111333893A (en) * | 2018-12-17 | 2020-06-26 | 浙江欣麟新材料技术有限公司 | Hardened film and preparation method thereof |
| CN111524823A (en) * | 2020-04-10 | 2020-08-11 | 上海华虹宏力半导体制造有限公司 | Equipment detection method and test wafer |
| CN115464955A (en) * | 2020-12-09 | 2022-12-13 | 黎银茵 | PVC composite membrane with high visible light catalytic activity |
| CN115464955B (en) * | 2020-12-09 | 2024-05-24 | 广东世骅新材料科技有限公司 | PVC composite film with high visible light catalytic activity |
| CN114163858A (en) * | 2021-11-15 | 2022-03-11 | 广州有趣生物科技有限公司 | Photocuring PET coating and preparation method thereof, and preparation method and application of PET substrate |
| CN114230725A (en) * | 2021-12-20 | 2022-03-25 | 江西昊泽光学膜科技有限公司 | Modified polyester film based on ultraviolet light hardening and preparation method thereof |
| CN114230725B (en) * | 2021-12-20 | 2023-08-15 | 江西昊泽光学膜科技有限公司 | Modified polyester film based on ultraviolet light hardening and preparation method thereof |
| CN115340817A (en) * | 2022-09-15 | 2022-11-15 | 中国科学技术大学 | Hardening coating with wide temperature range and high damping performance and preparation method thereof |
| CN115340817B (en) * | 2022-09-15 | 2023-10-20 | 中国科学技术大学 | Hardening coating with wide temperature range and high damping performance and preparation method thereof |
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Application publication date: 20120711 |