CN101301805A - Manufacturing method of laminated film - Google Patents
Manufacturing method of laminated film Download PDFInfo
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- CN101301805A CN101301805A CNA2008100967071A CN200810096707A CN101301805A CN 101301805 A CN101301805 A CN 101301805A CN A2008100967071 A CNA2008100967071 A CN A2008100967071A CN 200810096707 A CN200810096707 A CN 200810096707A CN 101301805 A CN101301805 A CN 101301805A
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- film
- light
- resin adhesive
- epoxide resin
- cured type
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/40—Properties of the layers or laminate having particular optical properties
- B32B2307/42—Polarizing, birefringent, filtering
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- Adhesives Or Adhesive Processes (AREA)
- Polarising Elements (AREA)
- Laminated Bodies (AREA)
- Lining Or Joining Of Plastics Or The Like (AREA)
Abstract
The invention provides a method for producing lamination membrane formed by agglutinating membrane using photo-curing epoxide resin adhesive without irradiating strong light or heating after light irradiation, being a method for producing lamination membrane formed by agglutinating membrane using photo-curing epoxide resin adhesive. The method comprises: heating the photo-curing epoxide resin adhesive in the membranes above 40 degrees centigrade which is irradiated to be solidified thereby splicing membrane.
Description
Technical field
The present invention relates to a kind of manufacture method of the laminate film that can in wide spectrum, use, thereby in particular to a kind of manufacture method of using the laminate film that light-cured type epoxide resin adhesive adhesive film forms.
Background technology
Laminate film is used to comprise in the wide spectrum of automobile, aircraft, electric electronic Instrument.Particularly in recent years, the more and more various and High Level of the laminate film in the electric electronic Instrument.In the time of the variation of laminate film, High Level,, when also needing to keep the quality of laminate film of manufacturing, need simplification, automation of raising, the device of raising, the yield rate of productivity ratio etc. about the manufacture method of laminate film.
For example, the polarizer that uses in optical component or liquid crystal indicator is that make with adhesive bonds protective film or optical compensating film on the two sides of polariscope film at polyvinyl alcohol (PVA) usually.As this bonding agent, use be that water system bonding agent or organic solvent are bonding agent, to bring into use the non-solvent as non-water system, non-organic solvent system be bonding agent, particularly light-cured type epoxide resin adhesive but replace in recent years.
Past, in using of the manufacturing of light-cured type epoxide resin adhesive as the laminate film of bonding agent, in order to solidify the light-cured type epoxide resin adhesive fully, thereby thereby the light that must shine strong illumination quickens curing reaction with irradiation heat or reaction heat or utilize heating such as baking box to make curing reaction finish (back curing (After cure)) behind irradiates light.If the illuminated light of light-cured type epoxide resin adhesive, the Photoepolymerizationinitiater initiater that then wherein includes (catalyst) activation produces acid.The epoxy reaction of this acid and light-cured type epoxy resin, epoxy ring-opening produces carbonium ion.This carbonium ion constantly with the epoxy reaction of epoxy resin, epoxide resin adhesive is solidified.But, the reaction of carbonium ion and epoxy radicals is the reaction that is difficult to take place at normal temperatures, thus must shine the light of strong illumination or after irradiates light, utilize heating such as baking box, thus quicken or finish the reaction of carbonium ion and epoxy radicals.
If shine the light of strong illumination; light changes because of heat; for example under the situation that is the polariscope film; from by the polyvinyl alcohol film of dyeing such as iodine (deflecting mirror (deflection) film) iodine discharge (ヨ ウ Su order け) is taken place; perhaps polariscope film or protective film or optical compensating film deform, thereby degradation.
In addition, under the situation with heating such as baking box after illumination is penetrated, need heaters such as heating oven, especially under the fast situation of on-line velocity (line speed), it is very long that heating oven becomes, and running expense rises, and the equipment investment expense increases.
Summary of the invention
The object of the present invention is to provide the use light-cured type epoxide resin adhesive of a kind of ultraviolet ray that needn't shine strong illumination for the light-cured type epoxide resin adhesive is solidified fully or heating (back curing) irradiates light after to come the manufacture method of the laminate film that adhesive film forms.
The inventor etc. concentrate on studies in order to solve described problem, found that by before irradiates light the light-cured type epoxide resin adhesive being heated to specific temperature, can realize described problem, so that finish the present invention based on these opinions.
Utilize the present invention, following 1～4 invention is provided.
(1) a kind of manufacture method of laminate film, it is to use the light-cured type epoxide resin adhesive to come the manufacture method of the laminate film that adhesive film forms, it is characterized in that, comprise: the light-cured type epoxide resin adhesive that will be present between film is heated to the temperature more than 40 ℃, thereby and described binding agent is carried out illumination penetrate and make its curing adhering film.
(2) a kind of film adhering method; it is to use the light-cured type epoxide resin adhesive to come bonding polariscope film and protective film and/or optical compensating film and the adhering method of the film that forms; it is characterized in that; comprise: will be present in light-cured type epoxide resin adhesive between film and heat, thereby and described binding agent be carried out illumination penetrate and make its curing adhering film to more than 40 ℃ and the temperature below the heat resisting temperature of described film.
(3) according to the method for record in (1) or (2), wherein, the described temperature of heating is 40～120 ℃.
(4) according to the method for any record in (1)～(3), wherein, light is the ultraviolet ray that at least a portion in the light of wavelength below 400nm is cut off.
Utilize adhering device of the present invention, needn't shine the light of strong illumination for the light-cured type epoxide resin adhesive is solidified fully or heating (then solidify) after irradiates light, so laminate film that can polarizer easy and that workmanship is good effectively and so on.
The specific embodiment
Below describe the present invention in detail.
The light-cured type epoxide resin adhesive of Shi Yonging contains light-cured type photoreactive epoxy resin polymerization initiator in the present invention, also can contain habitual adding ingredient in addition.
Light-cured type epoxy resin for example comprises aromatic epoxy resin, aliphatic epoxy resin, alicyclic epoxy resin etc. so long as normally used light-cured type epoxy resin then is not particularly limited.
As aromatic epoxy resin, can enumerate bisphenol A type epoxy resin, bisphenol f type epoxy resin, bisphenol A type epoxy resin, naphthalene framework ring epoxy resins, phenol novolak type epoxy resin etc.
As aliphatic epoxy resin, can use the polyglycidyl ether of aliphatic polyol or its epoxides addition product.Example as aliphatic epoxy resin, can enumerate ethylene glycol diglycidylether, diethylene glycol (DEG) diglycidyl ether, propylene glycol diglycidylether, tripropyleneglycol diglycidyl ether, neopentylglycol diglycidyl ether, 1,4-butanediol diglycidyl ether, 1,6-hexanediol diglycidyl ether, trihydroxymethylpropanyltri diglycidyl ether, trimethylolpropane diglycidyl ether, polyethyleneglycol diglycidylether etc.In addition, can also use unrighted acid epoxies such as butadiene-based epoxy resin, isoprene epoxy resin.The viscosity of trihydroxymethylpropanyltri diglycidyl ether, trimethylolpropane diglycidyl ether is low, so preferred.The commercially available product of aliphatic epoxy resin for example comprises common prosperity society chemistry (strain) system エ Port ラ イ ト 100MF (trihydroxymethylpropanyltri diglycidyl ether), Na ガ セ ケ system テ Star Network ス (strain) system EX-321L (trimethylolpropane diglycidyl ether).
Alicyclic epoxy resin is to have the compound that is incorporated into the epoxy radicals of ester ring type ring more than 1 in molecule, as this example, can enumerate VCH monoxide, 1,2-epoxy radicals-4-vinyl cyclohexane, 1,2:8,9 bicyclic oxygen citrenes, 3,4-epoxy radicals cyclohexenyl group methyl-3 ', 4 '-epoxy radicals cyclohexene carboxylate ester etc.They are commercially available with CEL2000, CEL3000, CEL2021P by ダ イ セ Le chemical industry (strain).
As the light-cured type epoxy resin among the present invention, can use described epoxy resin separately, also can mix and use multiple epoxy resin with any cooperation ratio.
Photoepolymerizationinitiater initiater among the present invention is so long as utilize the irradiation of actinic energy rays such as luminous ray, ultraviolet ray, X ray, electron ray to produce cation or lewis acid, and the Photoepolymerizationinitiater initiater that causes the polymerization of epoxy radicals gets final product, and is not particularly limited.As the example of Photoepolymerizationinitiater initiater, can enumerate sulfonium salt, salt compounded of iodine, diazol.
As the example of sulfonium system, for example
The triphenylsulfonium hexafluorophosphate
The triphenylsulfonium hexafluoro antimonate
Triphenylsulfonium four (pentafluorophenyl group) borate
The two hexafluorophosphates of 4,4 '-two [diphenyl sulfonium base (ス Le ホ ニ オ)] diphenyl sulfide
The two hexafluoro antimonates of 4,4 '-two [two (beta-hydroxy ethyoxyl) phenyl sulfonium base] diphenyl sulfide
The two hexafluorophosphates of 4,4 '-two [two (beta-hydroxy ethyoxyl) phenyl sulfonium base] diphenyl sulfide
7-[two (toluoyl base) sulfonium base]-2-isopropyl thioxanthone hexafluoro antimonate
7-[two (toluoyl base) sulfonium base]-2-isopropyl thioxanthone four (pentafluorophenyl group) borate
4-phenylcarbonyl group-4 '-diphenyl sulfonium base-diphenyl sulfide hexafluorophosphate
4-(to the tert-butyl-phenyl carbonyl)-4 '-diphenyl sulfonium base-diphenyl sulfide hexafluoro antimonate
4-(to the tert-butyl-phenyl carbonyl)-4 '-two (toluoyl base) sulfonium base-diphenyl sulfide four (pentafluorophenyl group) borates
Deng.
As the example of salt compounded of iodine, for example can enumerate
Diphenyl iodine four (pentafluorophenyl group) borate
Diphenyl iodine hexafluorophosphate
Diphenyl iodine hexafluoro antimonate
Two (4-nonyl phenyl) iodine hexafluorophosphate
Deng.
As the example of diazol, for example can enumerate
Benzene diazonium hexafluoro antimonate
Benzene diazonium hexafluorophosphate
Deng.
As the commercially available product of Photoepolymerizationinitiater initiater, can enumerate ア デ カ オ プ ト マ one SP-150 of rising sun electrochemical industry (strain) system and PI2074, the カ ヤ ラ Star De PCI-220 of Japanese chemical drug (strain) etc. of SP-170, ロ デ イ ア (strain) system.
Relative light-cured type epoxy resin 100 mass parts of these Photoepolymerizationinitiater initiaters are used 0.5～20 mass parts, preferred 1～10 mass parts.Photoepolymerizationinitiater initiater can be distinguished use separately, also can use two or more.
Light-cured type epoxide resin adhesive among the present invention can contain oxetane compound as required.Oxetane compound is the compound that to have 4 Yuans cyclic ethers in molecule be the oxetanes ring.Example as oxetane compound, can enumerate 3-ethyl-3-hydroxymethyl oxetanes, 1, two [{ (3-ethyl-3-oxetanyl) methoxyl group } methyl] benzene of 4-, 3-ethyl-3-(phenoxymethyl) oxetanes, two (3-ethyl-3-oxetanes ylmethyl) ether, 3-ethyl-3-(2-ethyl hexyl oxy methyl) oxetanes, 3-ethyl-[{ (3-triethoxysilyl propoxyl group) methyl } oxetanes], oxetanyl silsesquioxane (シ Le セ ス キ オ キ サ Application), phenol novolaks oxetanes etc.In these oxetane compounds, preferred 3-ethyl-3-hydroxymethyl oxetanes, two (3-ethyl-3-oxetanes ylmethyl) ether, 3-ethyl-3-(2-ethyl hexyl oxy methyl) oxetanes.The commercially available product of oxetane compound for example comprises that East Asia synthesizes (strain) commercially available trade name OXT-101 (3-ethyl-3-hydroxymethyl oxetanes), OXT-211 (3-ethyl-3-(phenoxymethyl) oxetanes), OXT-221 (two [1-ethyl (3-oxetanyl)] methyl ether), OXT-212 (3-ethyl-3-(2-ethyl hexyl oxy methyl) oxetanes).
In the present invention, relative light-cured type epoxy resin 100 mass parts of oxetane compound are used with the amount below 50 mass parts.Oxetane compound can be distinguished use separately, also can use two or more.
Light-cured type epoxide resin adhesive among the present invention can so that as required and use sensitising agent.By using sensitising agent, reactivity worth improves, and can improve the mechanical strength or the adhesive strength of solidfied material.As sensitising agent, can enumerate carbonyls, organosulfur compound, persulfide, redox based compound, azo and diazonium compound, halogen compounds, photo-reduction pigment etc.As the example of sensitising agent, can enumerate benzoin methyl ether, benzoin isopropyl ether, α, the benzoin derivative of alpha, alpha-dimethyl oxygen base-α-phenyl acetophenone and so on; Benzophenone, 2,4-dichloro-benzenes ketone, benzophenone methyl formate, 4, the methanone derivatives of 4 '-two (diethylin) Benzophenone and so on; 2-clopenthixal ketone, 2-isopropyl thioxanthone, 2, the thioxanthone derivates of 4-diethyl thioxanthone and so on; The anthraquinone derivative of 2-chloroanthraquinone, 2-methylanthraquinone and so on; The acridone derivatives of N-methylacridine ketone, N-butyl acridone and so on; 9, the anthracene derivant of 10-dibutoxy anthracene and so on; In addition, α, α-diethoxy acetophenone, benzil, Fluorenone, xanthone, lauryl (ラ ウ ニ Le) compound, halogen compounds, photo-reduction pigment etc., but not by these qualifications.In addition, these sensitising agents can use separately, also can use two or more.The commercially available product of sensitising agent for example can be enumerated カ ヤ キ ユ ア DETX-S (Japanese chemical drug (strain) system) etc.Relative light-cured type epoxide resin adhesive 100 mass parts of the amount of sensitising agent are 0.01～20 mass parts, are preferably 0.1～5 mass parts.
As long as in the scope of not destroying effect of the present invention, can so that light-cured type epoxide resin adhesive in the present invention in cooperate additive beyond described, for example filler, antioxidant, silane coupling agent.
As the example of filler, can enumerate inorganic filler or resin fillers such as polypropylene, polyethylene such as talcum, silica, mica.
As antioxidant, for example can enumerate dibutyl hydroxy toluene (BHT), イ Le ガ ノ Star Network ス 1010, イ Le ガ ノ Star Network ス 1035FF, イ Le ガ ノ Star Network ス 565 etc.
As silane coupling agent, can enumerate vinyltrimethoxy silane, VTES, 2-(3,4-ethyoxyl cyclohexyl) ethyl trimethoxy silane, the 3-glycidoxypropyltrime,hoxysilane, 3-glycidoxy propyl group methyldiethoxysilane, 3-glycidoxy propyl-triethoxysilicane, to the styryl trimethoxy silane, 3-methacryloxypropyl methyl dimethoxysilane, 3-methacryloxypropyl triethoxysilane, the 3-methacryloxypropyl trimethoxy silane, 3-triethoxysilyl-N-(1,3-dimethyl-Ding fork) propyl group amine etc.
The commercially available product of silane coupling agent for example can be enumerated epoxy system (for example KBM403, KBM303), ethene base system (KBM1003), acrylic acid series silane coupling agent (KBM503), 3-ethyl (triethoxysilyl propoxyl group methyl) oxetanes (TESOX (East Asia synthetic (strain) system)) etc.
Light-cured type epoxide resin adhesive in the present invention is preferably below the viscosity 200mPas (25 ℃) and then is preferably below the 150mPas (25 ℃).Low more easy more coating of viscosity in addition, can make the applied thickness of bond layer thin, for example is used for protective film or optical compensating film are attached under the situation of polarizer, and it is good that the outward appearance of polarizer also becomes.Also can use full-bodied bonding agent, but reduce coating amount in this case.
The film of Shi Yonging is necessary for the film that at least 1 film sees through light in the present invention.As such photopermeability film, can enumerate ployester series film, polycarbonate-based film, acrylic films, polyamide-based film, polyimides is film, amorphism polyolefin film, cyclic olefine film.PVA is film, cellulose-based film etc.
The amorphism polyolefin-based resins is generally ENB or has the resin of the polymerized unit of the cyclic polyolefin that encircles norborneol alkene monomers and so on more, also can be the copolymer of cyclic olefin and chain cyclic olefin.As commercially available amorphism polyolefin-based resins, comprise APO, ア ペ Le of ZEONEX, ZEONOR, the Mitsui Chemicals (strain) of trade name ア one ト Application, the Japanese ゼ オ Application (strain) of JSR (strain) etc.
In the present invention, can with the film combinations that does not see through light, the film that does not see through light for example also can be as the base film of laminate film.As such film that does not see through light, for example can enumerate and contain the Kapton etc. that the resin of coloring pigment, illuminating colour, carbon black, inorganic particulate or high molecular particle and so on, the wavelength region may below 450nm do not have photopermeability for painted or shading.
Thickness to each film among the present invention is not particularly limited, and can use the film of all thickness as required.
Laminate film is under the situation of polarizer, and can use PVA is protective film or optical compensating films such as cellulose-based film such as polariscope film or triacetyl cellulose, cyclic olefine film.
In the present invention, the method of subtend base film coating light-cured type epoxide resin adhesive, be not particularly limited, for example comprise the method for using scraper, foundry pig, chill coating machine, health agate coating machine (カ Application マ コ one one), intaglio coating machine etc.In addition, the lamination of the film among the present invention can use metallic roll, rubber-surfaced roll etc. to carry out, and the lamination pressure of this moment can be 0～5Mpa.
Laminate film among the present invention can have the stepped construction that is made of 2 layers, 3 layers, 4 layers, 5 layers, 6 layers or film more than it.
In the present invention, also can use the film of implementing sided corona treatment, plasma treatment, excimer processing, UV processing etc. at the adhesive surface of film.
The temperature of heating of the light-cured type epoxide resin adhesive among the present invention is necessary for more than 40 ℃.The upper limit of the temperature of heating is the heat resisting temperature of bur film, depends on the hear resistance of bur film, so can not limit without exception, for example is 120 ℃.At this, the heat resisting temperature of film is meant film is positioned over certain temperature in the time of following 60 seconds, with compare before the heating, the highest temperature in the temperature of deterioration does not take place in the optical characteristics (transmitance, degree of polarization) that does not occur the distortion (warpage, distortion) of film and film actually.The temperature of heating of bonding agent is below 40 ℃ the time, utilizes the curing of light-struck light-cured type epoxy resin insufficient, can not reach effect of the present invention.The temperature of heating of bonding agent is preferably 50～100 ℃, more preferably 60～80 ℃.
Heating of light-cured type epoxide resin adhesive among the present invention for example can be enumerated near infrared ray Halogen lamp LED, far infra-red heater, hot blast, heating plate, warm-up mill etc., but do not limited by these.
Only refer to actinic energy rays such as luminous ray, ultraviolet ray, X ray, electron ray among the present invention, be preferably ultraviolet ray.Illumination is penetrated and can be used metal halide lamp, high-pressure sodium lamp, xenon lamp, Halogen lamp LED etc. to carry out.Use under the ultraviolet situation, for the deterioration that makes film minimum, preferred at least a portion that does not contain wavelength at the light below the 400nm, below the preferred 390nm does not more preferably contain the whole ultraviolet ray of wavelength at the light below the 400nm, below the preferred 390nm in addition.Such ultraviolet ray for example can by between ultraviolet lamp and bur film, use near infrared ray by (cut) wave filter or cutoff wavelength 310 or the optical filter of light below the 390nm obtain.As this optical filter, can enumerate quartz glass, hot line cut-off filter (IRCF), the following cut-off filter of 310nm, 320nm cut-off filter, 340nm cut-off filter, 390nm cut-off filter, soda lime glass, 400～450nm bandpass filter etc.
When having more than 40 ℃, the temperature that is radiated at the light-cured type epoxide resin adhesive of the light among the present invention carries out.The exposure intensity of the light among the present invention is according to purpose bonding agent or resin film and difference is unqualified, and the exposure intensity of the effective wavelength region may of activation of Photoepolymerizationinitiater initiater is preferably 10～500mW/cm
2The irradiation time of light is according to the material of the kind of the photo-curable epoxy resin that uses or film and difference is unqualified, and is 100～3000mJ/cm as the accumulation light quantity of the product representation of exposure intensity and irradiation time
2(wavelength 405nm) is preferably 700～2000mJ/cm
2(wavelength 405nm).
[embodiment]
Below utilize embodiment to show the present invention, but the present invention is not limited by these embodiment.
The preparation of Production Example A～F light-cured type epoxide resin adhesive
Metering and the following raw material of adding mix, stir with mixer in the polyethylene container made, obtain the light-cured type epoxide resin adhesive (viscosity: 150mPa/s (25 ℃)) of homogeneous.
[table 1]
100MF: trihydroxymethylpropanyltri diglycidyl ether, common prosperity company chemistry (strain)
エ ピ Network ロ Application EXA-850S:4,4 '-2-glycidyl oxygen base-2,2 '-diphenyl propane, big Japanese ink (イ Application キ) chemistry (strain)
エ ピ Network ロ Application N740: phenol phenolic varnish type epoxy oligomer, big Japanese ink chemistry (strain)
CEL2000:1,2-epoxy radicals-4-vinyl cyclohexane, ダ イ セ Le chemical industry (strain)
CEL3000:1,2:8,9 bicyclic oxygen citrenes, ダ イ セ Le chemical industry (strain)
CEL2021P:3,4-epoxy radicals cyclohexenyl group methyl-3 ', 4 '-epoxy radicals cyclohexene carboxylate ester, ダ イ セ Le chemical industry (strain)
CPI-101A: photopolymerization catalyst サ Application ア プ ロ (strain)
SP-172: photopolymerization catalyst, (strain) ADEKA
The KBM403:3-glycidoxypropyltrime,hoxysilane, SHIN-ETSU HANTOTAI's chemical industry (strain)
DBA:9,10-dibutoxy anthracene, Kawasaki change into industry (strain)
The manufacturing of embodiment 1～6 and comparative example 1～3 laminate film (polarizer)
By the photo-curable epoxide resin adhesive (symbol of in Production Example, preparing: A), the bonding triacetylcellulose film of single face at the polyvinyl alcohol polariscope film that carries out simple tension and usefulness iodine staining, at the bonding amorphism film of polyolefin resin of another side (the ゼ オ ノ ア film of Japanese ゼ オ Application (strain) system), obtain the film of 3-tier architecture.Use infrared lamp, the 3-tier architecture film that obtains is heated to room temperature (25 ℃), 30 ℃, 40 ℃, 50 ℃, 60 ℃, 70 ℃, 80 ℃, 100 ℃, 120 ℃ and 140 ℃, use metal halide lamp (ア イ グ ラ Off イ Star Network ス corporate system) then immediately, with exposure intensity 200mW/cm
2(405nm), accumulative total light quantity 1000mJ/cm
2(405nm), carry out illumination and penetrate, obtain laminate film.Bond layer between the laminate film is the thickness about 1～3 μ m, is homogeneous.Utilize electron microscope to confirm these results.
Table 2 expression material temperature, the state of the postradiation bonding agent of UV, the distortion of the postradiation laminate film of UV, the wear properties of laminate film, the optical characteristics after the humidity test.
[table 2]
| Embodiment or comparative example | Material temperature (℃) | The state of the postradiation bonding agent of UV | The distortion of the postradiation film of UV | Wear properties after the humidity test | Optical characteristics after the humidity test |
| Comparative example 1 | 25 | Be liquid state, solidify insufficient | Do not have | × | - |
| Comparative example 2 | 30 | Be liquid state, solidify insufficient | Do not have | × | - |
| Embodiment 1 | 40 | △ | Do not have | × | - |
| Embodiment 2 | 50 | ○ | Do not have | × | - |
| Embodiment 3 | 60 | ◎ | Do not have | △ | Some variation |
| Embodiment 4 | 70 | ◎ | Do not have | △ | Do not change |
| Embodiment 5 | 80 | ○ | Warpage slightly | △ | Do not change |
| Embodiment 6 | 100 | ○ | Warpage greatly | × | - |
| Comparative example 3 | 140 | Strip off | Greatly distortion | × | - |
The temperature (temperature of heating) of the bonding agent before material temperature: the UV irradiation
The state of the postradiation bonding agent of UV:
Estimate according to following standard.
Be liquid state, solidify insufficient: be liquid condition, solidify insufficiently, do not have bonding
Strip off: film is stripped off
△: bonding, but intensity some is weak (～100g/25mm)
Zero: bonding, intensity is middle degree (100～200g/25mm)
◎: bonding, intensity is (200g/25mm～) fully
The distortion of the postradiation film of UV: detect by an unaided eye.
Wear properties after the humidity test:
According to following standard, estimate laminate film is positioned over the outward appearance (discharge or film sex change) after 500 hours in 60 ℃-90% the humidity test groove of condition.
*: seriously strip off or the discharge of distortion, polariscope part.
△: strip off or the discharge of distortion, polariscope part.
Zero: the discharge of polariscope part seldom takes place, but do not strip off or be out of shape.
◎: do not strip off or the discharge of distortion, polariscope part.
Optical characteristics after the humidity test:
To before the humidity test and after laminate film, measure degree of polarization and transmitance, estimate with their deterioration (reduction of the value of the laminate film before the humidity test).
*For the sex change (distortion, wear properties, optical characteristics) of sticker material, not only deterioration also takes place in heat under ultraviolet ray.
As known from Table 2, if heating after 40～70 ℃, carry out illumination and penetrate, solidify, then the light-cured type epoxide resin adhesive is solidified fully, demonstrates good cementability, does not also almost have the distortion of film simultaneously.On the other hand, be that although there is not the distortion of film, the light-cured type epoxide resin adhesive is solidified insufficient or uncured under 25 ℃, 30 ℃ the situation in the temperature of heating, cementability is very bad.In addition, material temperature is that the light-cured type epoxide resin adhesive is solidified fully, demonstrates good cementability under the situation more than 80～100 ℃, but film warpage slightly.In addition, surpass under 100 ℃ the situation, the light-cured type epoxide resin adhesive is solidified fully, demonstrates good cementability, but greatly sex change of film.
Light-cured resin B～F is carried out identical research,, all can obtain same result although cementability more or less there are differences.
In addition, replace infrared lamp and under the situation of carrying out when heating or with hot blast, can obtain laminate film with described same performance with heating plate.
The manufacturing of embodiment 7～13 and comparative example 4～6 laminate films
In the manufacturing of the laminate film of embodiment 1～6 and comparative example 1～3, between metal halide lamp and bur film, the optical filter (ア イ グ ラ Off イ Star Network ス corporate system) of the light of configuration cutoff wavelength below 390nm, irradiates light.Similarly carry out with embodiment 1～6 and comparative example 1～3, obtain the laminate film of embodiment 7～13 and comparative example 4～6 respectively.
[table 3]
| Embodiment or comparative example | Material temperature (℃) | The state of the postradiation bonding agent of UV | The distortion of the postradiation film of UV | Wear properties after the humidity test | Optical characteristics after the humidity test |
| Comparative example 4 | 25 | Be liquid state, solidify insufficient | Do not have | × | - |
| Comparative example 5 | 30 | Be liquid state, solidify insufficient | Do not have | × | - |
| Embodiment 7 | 40 | △ | Do not have | △ | Some variation |
| Embodiment 8 | 50 | ○ | Do not have | ○ | Variation slightly |
| Embodiment 9 | 60 | ◎ | Do not have | ◎ | No change |
| Embodiment 10 | 70 | ◎ | Do not have | ◎ | No change |
| Embodiment 11 | 80 | ◎ | Do not have | ◎ | No change |
| Embodiment 12 | 100 | ◎ | Do not have | △ | Some variation |
| Embodiment 13 | 120 | ○ | Warpage slightly | △ | Some variation |
| Comparative example 6 | 140 | ○ | Distortion | × | - |
As known from Table 3, if the optical filter of the light of configuration cutoff wavelength below 390nm between metal halide lamp and bur, then compare with situation about not disposing, the sex change of polariscope and film is few, can obtain having the good cementability and the laminate film of wear properties.Even replace the wave filter of cutoff wavelength below 390nm, and use cutoff wavelength the wave filter below the 320nm, cutoff wavelength at wave filter below the 340nm or cutoff wavelength the wave filter below 370nm, also can obtain same result, and the use of the wave filter of cutoff wavelength below 390nm is minimum to the influence that constitutes film.By using optical filter, the distortion of the film in the time of can suppressing to heat to 120 ℃, and the distortion of the film can not suppress to heat to 140 ℃ the time.
The manufacturing of comparative example 7～12 laminate films
Carry out similarly to Example 1, obtain the film of 3-tier architecture.The film of the 3-tier architecture that obtains of not heating, and use metal halide lamp (ア イ グ ラ Off イ Star Network ス corporate system), with exposure intensity 500mW/cm
2(405nm), integration light quantity 500,1000,2000 and 3000mJ/cm
2(405nm), carry out illumination and penetrate, obtain laminate film.And then, be 2000 and 3000mJ/cm in the accumulative total light quantity
2Under the situation (405nm), use the optical filter (ア イ グ ラ Off イ Star Network ス corporate system) that is disposed at the light of cutoff wavelength below 390nm between metal halide lamp and the bur film, carry out illumination and penetrate, obtain laminate film.
[table 4]
| Embodiment or comparative example | Optical filter | Accumulative total light quantity (the mJ/cm of UV 2(405nm)) | The state of the postradiation bonding agent of UV | The distortion of the postradiation film of UV |
| Comparative example 7 | Do not have | 500 | Be liquid state, solidify insufficient | Do not have |
| Comparative example 8 | Do not have | 1000 | Be liquid state, solidify insufficient | Do not have |
| Comparative example 9 | Do not have | 2000 | ○ | Distortion |
| Comparative example 10 | Have | 2000 | ○ | Distortion |
| Comparative example 11 | Do not have | 3000 | ◎ | Distortion |
| Comparative example 12 | Have | 3000 | ◎ | Distortion |
As known from Table 4, under the situation of not heating before illumination is penetrated, even the irradiation light quantity of increase and decrease light, it is outstanding and do not have a laminate film of the distortion of film to obtain cementability.
Utilizability on the industry
The present invention can be for the manufacturing of the laminate film that uses in the industry-wide field that comprises automobile, aircraft, electric electronic Instrument. In addition, because for to have the process of the quick cementability of rapidly-curable, so greatly help the raising of manufacturing speed or the reduction of heating process.
Claims (4)
1. the manufacture method of a laminate film, it is to use the light-cured type epoxide resin adhesive to come the manufacture method of the laminate film that adhesive film forms, and it is characterized in that, comprising:
The light-cured type epoxide resin adhesive that will be present between film is heated to the temperature more than 40 ℃, thereby and described binding agent is carried out illumination penetrate and make its curing adhering film.
2. film adhering method, it is to use the light-cured type epoxide resin adhesive to come bonding polariscope film and protective film and/or optical compensating film and the adhering method of the film that forms, it is characterized in that, comprising:
To be present in light-cured type epoxide resin adhesive between film and heat, thereby and described binding agent be carried out illumination penetrate and make its curing adhering film to more than 40 ℃ and the temperature below the heat resisting temperature of described film.
3. method according to claim 1 and 2, wherein,
The described temperature of heating is 40～120 ℃.
4. according to any described method in the claim 1～3, wherein,
Light is the ultraviolet ray that at least a portion in the light of wavelength below 400nm is cut off.
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| JP (1) | JP5221893B2 (en) |
| KR (1) | KR101486082B1 (en) |
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| CN101923183A (en) * | 2009-06-15 | 2010-12-22 | 住友化学株式会社 | Optical laminate and manufacture method thereof |
| CN101983866A (en) * | 2010-08-16 | 2011-03-09 | 郑健生 | Film compounding process |
| CN103443236A (en) * | 2011-03-29 | 2013-12-11 | 住友化学株式会社 | Photocurable adhesive, polarizing plate, and laminate optical member |
| CN103597383A (en) * | 2011-03-29 | 2014-02-19 | 住友化学株式会社 | Polarizing plate using photocurable adhesive and laminate optical member |
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| JP3544003B2 (en) * | 1994-08-22 | 2004-07-21 | 大日本インキ化学工業株式会社 | Epoxy resin composition |
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| JP2000109780A (en) * | 1998-10-07 | 2000-04-18 | Dainippon Ink & Chem Inc | Ultraviolet-hardening type adhesive composition for optical member |
| JP2001247834A (en) * | 2000-03-02 | 2001-09-14 | Sekisui Chem Co Ltd | Curable pressure-sensitive adhesive composition, curable pressure-sensitive adhesive sheet, and bonding method of optical or electronic substrate |
| US6949297B2 (en) * | 2001-11-02 | 2005-09-27 | 3M Innovative Properties Company | Hybrid adhesives, articles, and methods |
| JP2003246970A (en) * | 2001-12-21 | 2003-09-05 | Sekisui Chem Co Ltd | Apparatus and method for producing structure adhered by photoreactive adhesive |
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| CN1556163A (en) * | 2003-12-31 | 2004-12-22 | 广州市光聚化学材料有限公司 | Light solidifying resin suitable for thick coating layer and its use method |
| JP4620967B2 (en) * | 2004-04-26 | 2011-01-26 | 太陽ホールディングス株式会社 | Thermosetting resin composition for permanent hole filling |
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2007
- 2007-05-07 JP JP2007122698A patent/JP5221893B2/en active Active
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- 2008-04-21 TW TW097114451A patent/TWI432326B/en active
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Also Published As
| Publication number | Publication date |
|---|---|
| JP2008273148A (en) | 2008-11-13 |
| CN101301805B (en) | 2015-10-21 |
| KR20080099154A (en) | 2008-11-12 |
| TW200904634A (en) | 2009-02-01 |
| JP5221893B2 (en) | 2013-06-26 |
| CN102774121A (en) | 2012-11-14 |
| CN102774121B (en) | 2015-10-14 |
| KR101486082B1 (en) | 2015-01-23 |
| TWI432326B (en) | 2014-04-01 |
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