CN101301805B - The manufacture method of laminate film - Google Patents
The manufacture method of laminate film Download PDFInfo
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- CN101301805B CN101301805B CN200810096707.1A CN200810096707A CN101301805B CN 101301805 B CN101301805 B CN 101301805B CN 200810096707 A CN200810096707 A CN 200810096707A CN 101301805 B CN101301805 B CN 101301805B
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- film
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- resin adhesive
- epoxide resin
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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
-
- 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 the manufacture method that a kind of light that need not irradiate very strong illumination or the use light-cured type epoxide resin adhesive heated after light irradiation carry out the laminate film of adhesive film, it is the manufacture method using light-cured type epoxide resin adhesive to carry out the laminate film of adhesive film, the method comprises: the light-cured type epoxide resin adhesive be present between film heated to the temperature of more than 40 DEG C, irradiates light make it solidify thus adhering film to it.
Description
Technical field
The present invention relates to a kind of manufacture method of the laminate film that can use in wide spectrum, use light-cured type epoxide resin adhesive thus the manufacture method of the laminate film of adhesive film in particular to a kind of.
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 electric electronic Instrument.While the variation of laminate film, High Level, about the manufacture method of laminate film, while also needing to maintain the quality of the laminate film manufactured, need the raising of productivity ratio, the raising of yield rate, the simplification, automation etc. of device.
Such as, the polarizer used in optical component or liquid crystal indicator is that the two sides adhesive bonds protective film of polariscope film or optical compensating film manufacture at polyvinyl alcohol (PVA) usually.As this bonding agent, use water system bonding agent or organic solvent system bonding agent, but replace in recent years and bring into use as the non-solvent system bonding agent of non-water system, non-organic solvent system, particularly light-cured type epoxide resin adhesive.
Past, in the manufacture using light-cured type epoxide resin adhesive as the laminate film of bonding agent, in order to solidify light-cured type epoxide resin adhesive fully, the light of strong illumination must be irradiated thus accelerate curing reaction by irradiation heat or reaction heat or after irradiation light, utilize the heating such as baking box thus curing reaction is terminated (Post RDBMS (After cure)).If the illuminated light of light-cured type epoxide resin adhesive, then the Photoepolymerizationinitiater initiater wherein included (catalyst) activates, and 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 being difficult to occur at normal temperatures, so must irradiate the light of strong illumination or utilize the heating such as baking box after irradiation light, thus accelerates or terminate the reaction of carbonium ion and epoxy radicals.
If irradiate the light of strong illumination; light changes because of heat; such as when for polariscope film; iodine discharge (ヨ ウ Su order け) is there is from the polyvinyl alcohol film dyeed by iodine etc. (deflecting mirror (deflection) film); or polariscope film or protective film or optical compensating film deform, thus degradation.
In addition, when after light irradiation with heating such as baking boxs, need the heaters such as heating oven, when especially on-line velocity (line speed) is fast, heating oven becomes very long, and running expense rises, and equipment investment expense increases.
Summary of the invention
A kind of use light-cured type epoxide resin adhesive of the ultraviolet or heating (Post RDBMS) after irradiating light that need not irradiate strong illumination in order to make light-cured type epoxide resin adhesive solidify fully is the object of the present invention is to provide to carry out the manufacture method of the laminate film of adhesive film.
The present inventor etc. concentrate on studies to solve described problem, found that by heating to specific temperature by light-cured type epoxide resin adhesive before irradiation light, can realize described problem, so that complete the present invention based on these opinions.
Utilize the present invention, the invention of following 1 ~ 4 is provided.
(1) a kind of manufacture method of laminate film, it is the manufacture method using light-cured type epoxide resin adhesive to carry out the laminate film of adhesive film, it is characterized in that, comprise: the light-cured type epoxide resin adhesive be present between film is heated to the temperature of more than 40 DEG C, and illumination is carried out to described binding agent penetrate and make it solidify thus adhering film.
(2) a kind of film bond method; it is the adhering method of the film using light-cured type epoxide resin adhesive to be formed to bond polariscope film and protective film and/or optical compensating film; it is characterized in that; comprise: the light-cured type epoxide resin adhesive be present between film is heated to more than 40 DEG C and temperature below the heat resisting temperature of described film, and illumination is carried out to described binding agent penetrate and make it solidify thus adhering film.
(3) according to the method recorded in (1) or (2), wherein, described warm temperature is 40 ~ 120 DEG C.
(4) according to the method that any one in (1) ~ (3) is recorded, wherein, light is the ultraviolet that be at least partially cut off of wavelength in the light of below 400nm.
Utilize adhering device of the present invention, light or the heating (Post RDBMS) after irradiation light of strong illumination need not be irradiated, so can the laminate film of easy and that workmanship is good effectively polarizer and so on to make light-cured type epoxide resin adhesive solidify fully.
Detailed description of the invention
Below describe the present invention in detail.
The light-cured type epoxide resin adhesive used in the present invention contains light-cured type photoreactive epoxy resin polymerization initiator, in addition also can containing usual adding ingredient.
As long as the normally used light-cured type epoxy resin of light-cured type epoxy resin is not particularly limited, such as, comprise aromatic epoxy resin, aliphatic epoxy resin, alicyclic epoxy resin etc.
As aromatic epoxy resin, bisphenol A type epoxy resin, bisphenol f type epoxy resin, bisphenol A type epoxy resin, naphthalene skeletal epoxy resin, phenol novolak type epoxy resin etc. can be enumerated.
As aliphatic epoxy resin, the polyglycidyl ether of aliphatic polyol or its epoxides addition product can be used.As the example of aliphatic epoxy resin, ethylene glycol diglycidylether, diethylene glycol (DEG) diglycidyl ether, propylene glycol diglycidylether, tripropyleneglycol diglycidyl ether, neopentylglycol diglycidyl ether, 1 can be enumerated, 4-butanediol diglycidyl ether, 1,6-hexanediol diglycidyl ether, trihydroxymethylpropanyltri diglycidyl ether, trimethylolpropane diglycidyl ether, polyethyleneglycol diglycidylether etc.In addition, the unrighted acid epoxy such as butadiene-based epoxy resin, isoprene epoxy resin can also be used.The viscosity of trihydroxymethylpropanyltri diglycidyl ether, trimethylolpropane diglycidyl ether is low, so preferably.The commercially available product of aliphatic epoxy resin such as comprises common prosperity society chemistry (strain) エ processed Port ラ イ ト 100MF (trihydroxymethylpropanyltri diglycidyl ether), Na ガ セ ケ system テ Star Network ス (strain) EX-321L processed (trimethylolpropane diglycidyl ether).
Alicyclic epoxy resin is in molecule, have the compound that more than 1 is incorporated into the epoxy radicals of ester ring type ring, as this example, vinylcyclohexene monoxide, 1 can be enumerated, 2-epoxy radicals-4-vinyl cyclohexane, 1,2:8,9 bicyclic oxygen citrenes, 3,4-epoxycyclohexyethylSiOi enylmethyl-3 ', 4 '-epoxycyclohexyethylSiOi olefinic carboxylic acid 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 in the present invention, can be used alone described epoxy resin, also can with any mixing ratio multiple epoxy resin used in combination.
As long as the Photoepolymerizationinitiater initiater in the present invention utilizes the irradiation of the actinic energy rays such as luminous ray, ultraviolet, X-ray, electron ray to produce cation or lewis acid, cause the Photoepolymerizationinitiater initiater of the polymerization of epoxy radicals, be not particularly limited.As the example of Photoepolymerizationinitiater initiater, sulfonium salt, salt compounded of iodine, diazol can be enumerated.
As the example of sulfonium system, such as
Triphenylsulfonium hexafluorophosphate
Triphenylsulfonium hexafluoro antimonate
Triphenylsulfonium four (pentafluorophenyl group) borate
The two hexafluorophosphate of 4,4 '-bis-[diphenyl sulfonium base (ス Le ホ ニ オ)] diphenyl sulfide
The two hexafluoro antimonate of 4,4 '-bis-[two (beta-hydroxy ethyoxyl) phenyl sulfonium base] diphenyl sulfide
The two hexafluorophosphate of 4,4 '-bis-[two (beta-hydroxy ethyoxyl) phenyl sulfonium base] diphenyl sulfide
7-[two (toluoyl base) sulfonium base]-ITX hexafluoro antimonate
7-[two (toluoyl base) sulfonium base]-ITX four (pentafluorophenyl group) borate
4-phenylcarbonyl group-4 '-diphenyl sulfonium base-diphenyl sulfide hexafluorophosphate
4-(to tert-butyl-phenyl carbonyl)-4 '-diphenyl sulfonium base-diphenyl sulfide hexafluoro antimonate
4-(to tert-butyl-phenyl carbonyl)-4 '-two (toluoyl base) sulfonium base-diphenyl sulfide four (pentafluorophenyl group) borate
Deng.
As the example of salt compounded of iodine, such as, 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, such as, can enumerate
Benzene diazonium hexafluoro antimonate
Benzene diazonium hexafluorophosphate
Deng.
As the commercially available product of Photoepolymerizationinitiater initiater, the カ ヤ ラ Star De PCI-220 etc. of ア デ カ オ プ ト マ mono-SP-150 and SP-170 that rising sun electrochemical industry (strain) makes, PI2074 that ロ デ イ ア (strain) makes, Japanese chemical drug (strain) can be enumerated.
These Photoepolymerizationinitiater initiaters relative light-cured type epoxy resin 100 mass parts, uses 0.5 ~ 20 mass parts, preferably 1 ~ 10 mass parts.Photoepolymerizationinitiater initiater can individually use, and also can use two or more.
Light-cured type epoxide resin adhesive in the present invention can contain oxetane compound as required.Oxetane compound is the compound in molecule with 4 Yuans cyclic ethers and oxetanes ring.As the example of oxetane compound, 3-ethyl-3-hydroxymethyl oxetane can be enumerated, 1, two [{ (3-ethyl-3-oxetanyl) methoxyl group } methyl] benzene of 4-, 3-ethyl-3-(phenoxymethyl) oxetanes, two (3-ethyl-3-oxetanylmethyl) ether, 3-ethyl-3-(2-Ethylhexoxymethyl) oxetanes, 3-ethyl-[{ (3-triethoxysilylpropoxy) methyl } oxetanes], oxetanyl silsesquioxane (シ Le セ ス キ オ キ サ Application), phenol novolacs oxetanes etc.In these oxetane compounds, preferred 3-ethyl-3-hydroxymethyl oxetane, two (3-ethyl-3-oxetanylmethyl) ether, 3-ethyl-3-(2-Ethylhexoxymethyl) oxetanes.The commercially available product of oxetane compound such as comprises the commercially available trade name OXT-101 (3-ethyl-3-hydroxymethyl oxetane) in East Asia synthesis (strain), OXT-211 (3-ethyl-3-(phenoxymethyl) oxetanes), OXT-221 (two [1-ethyl (3-oxetanyl)] methyl ether), OXT-212 (3-ethyl-3-(2-Ethylhexoxymethyl) oxetanes).
In the present invention, oxetane compound relative light-cured type epoxy resin 100 mass parts, uses with the amount below 50 mass parts.Oxetane compound can individually use, and also can use two or more.
Light-cured type epoxide resin adhesive in the present invention can so that as required and use sensitising agent.By using sensitising agent, reactivity worth improves, and can improve mechanical strength or the adhesive strength of solidfied material.As sensitising agent, carbonyls, organosulfur compound, persulfide, redox based compound, azo and diazonium compound, halogen compounds, photo-reduction pigment etc. can be enumerated.As the example of sensitising agent, benzoin methyl ether, benzoin isopropyl ether, α can be enumerated, the benzoin derivative of alpha, alpha-dimethyl oxygen base-α-phenyl acetophenone and so on; Benzophenone, 2,4-dichloro-benzenes ketones, benzophenone methyl formate, 4, the methanone derivatives of 4 '-bis-(diethylin) Benzophenone and so on; The thioxanthone derivates of CTX, ITX, 2,4-diethyl thioxanthones 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; The anthracene derivant of 9,10-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 do not limited by these.In addition, these sensitising agents can be used alone, and also can use two or more.The commercially available product of sensitising agent such as can enumerate カ ヤ キ ユ ア DETX-S (Japanese chemical drug (strain) system) etc.Amount relative light-cured type epoxide resin adhesive 100 mass parts of sensitising agent is 0.01 ~ 20 mass parts, is preferably 0.1 ~ 5 mass parts.
As long as in the scope not destroying effect of the present invention, can so that light-cured type epoxide resin adhesive in the present invention in coordinate described beyond additive, such as filler, antioxidant, silane coupling agent.
As the example of filler, inorganic filler or the agent of the resin filling such as polypropylene, polyethylene such as talcum, silica, mica can be enumerated.
As antioxidant, such as, 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, vinyltrimethoxy silane can be enumerated, VTES, 2-(3, 4-ethoxycyclohexyl) ethyl trimethoxy silane, 3-glycidoxypropyltrime,hoxysilane, 3-glycidoxypropyl diethoxy silane, 3-glycidoxypropyl group triethoxysilane, to styryl trimethoxy silane, 3-methacryloyloxypropyl methyl dimethoxysilane, 3-methacryloxypropyl, 3-methacryloxypropyl trimethoxy silane, 3-triethoxysilyl-N-(1, 3-dimethyl-Ding pitches) propyl group amine etc.
The commercially available product of silane coupling agent such as can enumerate epoxy (such as KBM403, KBM303), ethene base system (KBM1003), acrylic silane coupling agent (KBM503), 3-ethyl (triethoxysilylpropoxy methyl) oxetanes (TESOX (East Asia synthesis (strain) system)) etc.
Light-cured type epoxide resin adhesive be in the present invention preferably viscosity 200mPas (25 DEG C) below so that be preferably 150mPas (25 DEG C) below.Viscosity is more low more easily to be applied, and in addition, the applied thickness of bond layer can be made thin, and such as, when for protective film or optical compensating film are attached at polarizer, the outward appearance of polarizer also becomes good.Also can use full-bodied bonding agent, but reduce coating amount in this case.
The film used in the present invention is necessary for the film of at least 1 film transmission light.As such photopermeability film, ployester series film, polycarbonate-based film, acrylic films, polyamide-based film, polyimides system film, amorphism polyolefin film, cyclic olefine film can be enumerated.PVA system film, cellulose-based film etc.
Amorphism polyolefin-based resins is generally ENB or has the resin of polymerized unit of cyclic polyolefin of many rings norborneol alkene monomer and so on, also can be the copolymer of cyclic olefin and chain cyclic olefin.As commercially available amorphism polyolefin-based resins, comprise the trade name ア mono-ト Application of JSR (strain), ZEONEX, the ZEONOR of Japanese ゼ オ Application (strain), APO, ア ペ Le etc. of Mitsui Chemicals (strain).
In the present invention, can with the film combinations not through light, the film not through light such as also can as the base film of laminate film.As so not through the film of light, such as can enumerate to include in order to painted or shading coloring pigment, illuminating colour, carbon black, inorganic particulate or high molecular particle and so on resin, there is no the Kapton etc. of photopermeability in the wavelength region of below 450nm.
The thickness of each film in the present invention is not particularly limited, the film of various thickness can be used as required.
When laminate film is polarizer, protective film or the optical compensating films such as cellulose-based film, cyclic olefine film such as PVA system polariscope film or triacetyl cellulose can be used.
In the present invention, the method of subtend base film coating light-cured type epoxide resin adhesive, be not particularly limited, such as, comprise the method using scraper, foundry pig, chill coating machine, health agate coating machine (カ Application マ コ mono-タ mono-), intaglio coating machine etc.In addition, the lamination of the film in the present invention can use metallic roll, rubber-surfaced roll etc. to carry out, and lamination pressure now can be 0 ~ 5Mpa.
Laminate film in the present invention can have the stepped construction be made up of 2 layers, 3 layers, 4 layers, 5 layers, 6 layers or its above film.
In the present invention, the adhesive surface that also can be used in film implements the film of sided corona treatment, plasma treatment, excimer process, UV process etc.
The warm temperature of the light-cured type epoxide resin adhesive in the present invention is necessary for more than 40 DEG C.The upper limit of warm temperature is the heat resisting temperature of bur film, depends on the heat resistance of bur film, so can not limit without exception, such as, is 120 DEG C.At this, when the heat resisting temperature of film refers to and film is positioned over lower 60 seconds of certain temperature, compared with before heating, do not occur that temperature the highest in the temperature of deterioration does not occur for the distortion (warpage, distortion) of film and the optical characteristics (transmitance, degree of polarization) of film actually.When the warm temperature of bonding agent is below 40 DEG C, utilizes the solidification of light-struck light-cured type epoxy resin insufficient, effect of the present invention can not be reached.The warm temperature of bonding agent is preferably 50 ~ 100 DEG C, is more preferably 60 ~ 80 DEG C.
Heating of light-cured type epoxide resin adhesive in the present invention such as can enumerate near infrared ray Halogen lamp LED, far infra-red heater, hot blast, heating plate, warm-up mill etc., but is not limited to these.
Only refer to the actinic energy rays such as luminous ray, ultraviolet, X-ray, electron ray in the present invention, be preferably ultraviolet.Illumination is penetrated and metal halide lamp, high-pressure sodium lamp, xenon lamp, Halogen lamp LED etc. can be used to carry out.Under using ultraviolet situation, in order to make the deterioration of film minimum, preferably containing wavelength below 400nm, preferably below 390nm light at least partially, in addition more preferably containing the whole ultraviolet of wavelength at below 400nm, the preferably light of below 390nm.Such ultraviolet such as can obtain at the optical filter of light of 310 or below 390nm by using near infrared ray to end (cut) wave filter or cutoff wavelength between ultraviolet lamp and bur film.As this optical filter, quartz glass, hot line cut-off filter (IRCF), below 310nm cut-off filter, 320nm cut-off filter, 340nm cut-off filter, 390nm cut-off filter, soda lime glass, 400 ~ 450nm bandpass filter etc. can be enumerated.
The irradiation of the light in the present invention is carried out when the temperature of light-cured type epoxide resin adhesive has more than 40 DEG C.The exposure intensity of the light in the present invention is different according to object bonding agent or resin film, does not limit, is preferably 10 ~ 500mW/cm to the exposure intensity of the effective wavelength region of the activation of Photoepolymerizationinitiater initiater
2.The irradiation time of light is different according to the kind of photo-curable epoxy resin used or the material of film, not restriction, 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 to these examples.
The preparation of Production Example A ~ F light-cured type epoxide resin adhesive
Measure in polyethylene container and add following raw material, with mixer mixing, stirring, obtain homogeneous light-cured type epoxide resin adhesive (viscosity: 150mPa/s (25 DEG C)).
[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, large Japanese ink (イ Application キ) chemistry (strain)
エ ピ Network ロ Application N740: phenol novolak-type epoxy oligomer, large 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-epoxycyclohexyethylSiOi enylmethyl-3 ', 4 '-epoxycyclohexyethylSiOi olefinic carboxylic acid ester, ダ イ セ Le chemical industry (strain)
CPI-101A: photopolymerization catalyst サ Application ア プ ロ (strain)
SP-172: photopolymerization catalyst, (strain) ADEKA
KBM403:3-glycidoxypropyltrime,hoxysilane, SHIN-ETSU HANTOTAI's chemical industry (strain)
DBA:9,10-dibutoxy anthracene, Kawasaki changes into industry (strain)
The manufacture of embodiment 1 ~ 6 and comparative example 1 ~ 3 laminate film (polarizer)
By the photo-curable epoxide resin adhesive prepared in Production Example (symbol: A), carrying out simple tension and bonding triacetylcellulose film with the one side of the polyvinyl alcohol polarization mirror film of iodine staining, at another side bonding amorphism film of polyolefin resin (the ゼ オ ノ ア film that Japanese ゼ オ Application (strain) is made), obtain the film of 3-tier architecture.Use infrared lamp, the 3-tier architecture film obtained is heated to room temperature (25 DEG C), 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 100 DEG C, 120 DEG C and 140 DEG C, then metal halide lamp (ア イ グ ラ Off イ ツク ス Inc.) is used immediately, with exposure intensity 200mW/cm
2(405nm), accumulative light quantity 1000mJ/cm
2(405nm), carry out illumination and penetrate, obtain laminate film.Bond layer between laminate film is the thickness of about 1 ~ 3 μm, for homogeneous.Electron microscope is utilized to confirm these results.
Table 2 represents the optical characteristics after the distortion of the state of the postradiation bonding agent of material temperature, UV, the postradiation laminate film of UV, the wear properties of laminate film, humidity test.
[table 2]
| Embodiment or comparative example | Material temperature (DEG C) | The state of the postradiation bonding agent of UV | The distortion of the postradiation film of UV | Wear properties after humidity test | Optical characteristics after humidity test |
| Comparative example 1 | 25 | For liquid state, solidify insufficient | Nothing | × | - |
| Comparative example 2 | 30 | For liquid state, solidify insufficient | Nothing | × | - |
| Embodiment 1 | 40 | △ | Nothing | × | - |
| Embodiment 2 | 50 | ○ | Nothing | × | - |
| Embodiment 3 | 60 | ◎ | Nothing | △ | Some is deteriorated |
| Embodiment 4 | 70 | ◎ | Nothing | △ | Not change |
| Embodiment 5 | 80 | ○ | Warpage slightly | △ | Not change |
| Embodiment 6 | 100 | ○ | Greatly warpage | × | - |
| Comparative example 3 | 140 | Strip off | Greatly be out of shape | × | - |
The temperature (warm temperature) of the bonding agent before material temperature: UV irradiates
The state of the postradiation bonding agent of UV:
Evaluate according to following standard.
For liquid state, solidify insufficient: be liquid condition, solidify insufficient, not bonding
Strip off: film is stripped off
△: bonding, but intensity a bit weak (~ 100g/25mm)
Zero: bonding, intensity is middle degree (100 ~ 200g/25mm)
◎: bonding, intensity fully (200g/25mm ~)
The distortion of the postradiation film of UV: detect by an unaided eye.
Wear properties after humidity test:
According to following standard, evaluate the outward appearance (discharge or film sex change) after 500 hours in the humidity test groove of condition laminate film being positioned over 60 DEG C-90%.
×: seriously strip off or be out of shape, the discharge of polariscope part.
△: strip off or be out of shape, the discharge of polariscope part.
Zero: the discharge that polariscope part seldom occurs, but do not strip off or be out of shape.
◎: do not strip off or be out of shape, the discharge of polariscope part.
Optical characteristics after humidity test:
To before humidity test and after laminate film, measure degree of polarization and transmitance, evaluate with their deterioration (reduction from the value of the laminate film before humidity test).
*for the sex change (distortion, wear properties, optical characteristics) of sticker material, not only, also there is deterioration in heat under ultraviolet light.
As known from Table 2, if after heating to 40 ~ 70 DEG C, carry out illumination and penetrate, solidification, then 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, when warm temperature is 25 DEG C, 30 DEG C, although do not have the distortion of film, the solidification of light-cured type epoxide resin adhesive is insufficient or uncured, and cementability is very bad.In addition, when material temperature is more than 80 ~ 100 DEG C, light-cured type epoxide resin adhesive is solidified fully, demonstrates good cementability, but film slightly warpage.In addition, when more than 100 DEG C, light-cured type epoxide resin adhesive is solidified fully, demonstrates good cementability, but film greatly sex change.
Identical research is carried out to light-cured resin B ~ F, although cementability more or less there are differences, all can obtain same result.
In addition, when replacing infrared lamp and heat with heating plate or when carrying out with hot blast, the laminate film with described same performance can be obtained.
The manufacture of embodiment 7 ~ 13 and comparative example 4 ~ 6 laminate film
In the manufacture of the laminate film of embodiment 1 ~ 6 and comparative example 1 ~ 3, between metal halide lamp and bur film, configuration cutoff wavelength, at the optical filter (ア イ グ ラ Off イ ツク ス Inc.) of the light of below 390nm, irradiates light.Carry out in the same manner as 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 (DEG C) | The state of the postradiation bonding agent of UV | The distortion of the postradiation film of UV | Wear properties after humidity test | Optical characteristics after humidity test |
| Comparative example 4 | 25 | For liquid state, solidify insufficient | Nothing | × | - |
| Comparative example 5 | 30 | For liquid state, solidify insufficient | Nothing | × | - |
| Embodiment 7 | 40 | △ | Nothing | △ | Some is deteriorated |
| Embodiment 8 | 50 | ○ | Nothing | ○ | Slightly be deteriorated |
| Embodiment 9 | 60 | ◎ | Nothing | ◎ | Unchanged |
| Embodiment 10 | 70 | ◎ | Nothing | ◎ | Unchanged |
| Embodiment 11 | 80 | ◎ | Nothing | ◎ | Unchanged |
| Embodiment 12 | 100 | ◎ | Nothing | △ | Some is deteriorated |
| Embodiment 13 | 120 | ○ | Warpage slightly | △ | Some is deteriorated |
| Comparative example 6 | 140 | ○ | Distortion | × | - |
As known from Table 3, if configure the optical filter of cutoff wavelength at the light of below 390nm between metal halide lamp and bur, then compared with situation about not configuring, the sex change of polariscope and film is few, can obtain having good cementability and the laminate film of wear properties.Even if replace cutoff wavelength at the wave filter of below 390nm, and use cutoff wavelength in the wave filter of below 320nm, cutoff wavelength at the wave filter of below 340nm or the cutoff wavelength wave filter at below 370nm, also can obtain same result, and cutoff wavelength is minimum on the impact forming film in the use of the wave filter of below 390nm.By using optical filter, the distortion of heating to film when 120 DEG C can be suppressed, and the distortion of heating to film when 140 DEG C can not be suppressed.
The manufacture of comparative example 7 ~ 12 laminate film
Carry out similarly to Example 1, obtain the film of 3-tier architecture.Not heat the film of the 3-tier architecture obtained, and use metal halide lamp (ア イ グ ラ Off イ ツク ス Inc.), 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 accumulative light quantity
2(405nm), when, use and be configured at the optical filter (ア イ グ ラ Off イ ツク ス Inc.) of the cutoff wavelength between metal halide lamp and bur film at the light of below 390nm, carry out illumination and penetrate, obtain laminate film.
[table 4]
| Embodiment or comparative example | Optical filter | Accumulative 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 | Nothing | 500 | For liquid state, solidify insufficient | Nothing |
| Comparative example 8 | Nothing | 1000 | For liquid state, solidify insufficient | Nothing |
| Comparative example 9 | Nothing | 2000 | ○ | Distortion |
| Comparative example 10 | Have | 2000 | ○ | Distortion |
| Comparative example 11 | Nothing | 3000 | ◎ | Distortion |
| Comparative example 12 | Have | 3000 | ◎ | Distortion |
As known from Table 4, when not heating before illumination is penetrated, even if the irradiation light quantity of increase and decrease light, cementability can not be obtained outstanding and there is no the laminate film of distortion of film.
Utilizability in industry
The present invention may be used in the manufacture comprising the laminate film used in the industry-wide field of automobile, aircraft, electric electronic Instrument.In addition, due to the process for having rapidly-curable rapid link, so greatly contribute to the raising of manufacturing speed or the reduction of heating process.
Claims (7)
1. a manufacture method for laminate film, it uses light-cured type epoxide resin adhesive to bond the manufacture method of the laminate film of polariscope film and protective film and/or optical compensating film, it is characterized in that, comprising:
In the single or double coating light-cured type epoxide resin adhesive of described polariscope film; after described polariscope film bonds described protective film and/or optical compensating film; the light-cured type epoxide resin adhesive be present between described film is heated to the temperature of more than 40 DEG C; and illumination is carried out to described binding agent penetrate and make it solidify thus bonding described film
The viscosity of described light-cured type epoxide resin adhesive 25 DEG C time is below 200mPas,
The thickness be present in after the solidification of the described light-cured type epoxide resin adhesive between described film is 1 ~ 3 μm, and
Described laminate film is polarizer.
2. the manufacture method of laminate film according to claim 1, wherein,
Described warm temperature is 40 ~ 120 DEG C.
3. the manufacture method of laminate film according to claim 1, wherein,
Described light is the ultraviolet that be at least partially cut off of wavelength in the light of below 390nm.
4. the manufacture method of laminate film according to claim 1, wherein,
One of described film is polariscope film,
Described polariscope film is polyethenol series polariscope film.
5. a film bond method, it is the adhering method of the film using light-cured type epoxide resin adhesive to be formed to bond polariscope film and protective film and/or optical compensating film, it is characterized in that, comprising:
In the single or double coating light-cured type epoxide resin adhesive of described polariscope film; after described polariscope film bonds described protective film and/or optical compensating film; the light-cured type epoxide resin adhesive be present between described film is heated to more than 40 DEG C and temperature below the heat resisting temperature of described film; and illumination is carried out to described binding agent penetrate and make it solidify thus bonding described film
The viscosity of described light-cured type epoxide resin adhesive 25 DEG C time is below 200mPas,
The thickness be present in after the solidification of the described light-cured type epoxide resin adhesive between described film is 1 ~ 3 μm.
6. film bond method according to claim 5, wherein,
Described warm temperature is 40 ~ 120 DEG C.
7. film bond method according to claim 5, wherein,
Described light is the ultraviolet that be at least partially cut off of wavelength in the light of below 390nm.
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| JP5586174B2 (en) * | 2009-06-15 | 2014-09-10 | 住友化学株式会社 | Optical laminate and method for producing the same |
| CN101983866A (en) * | 2010-08-16 | 2011-03-09 | 郑健生 | Film compounding process |
| JP6298248B2 (en) * | 2010-12-24 | 2018-03-20 | 日東電工株式会社 | Active energy ray-curable adhesive composition, polarizing plate, optical film, and image display device |
| JP5677883B2 (en) * | 2011-03-29 | 2015-02-25 | 住友化学株式会社 | Photo-curable adhesive, polarizing plate and laminated optical member |
| JP2012208187A (en) * | 2011-03-29 | 2012-10-25 | Sumitomo Chemical Co Ltd | Method for manufacturing polarizing plate |
| JP5827483B2 (en) * | 2011-03-29 | 2015-12-02 | 住友化学株式会社 | Polarizing plate and laminated optical member using photocurable adhesive |
| JP6308721B2 (en) * | 2012-03-30 | 2018-04-11 | 日東電工株式会社 | Polarizing film, optical film, and image display device |
| KR20130134236A (en) * | 2012-05-30 | 2013-12-10 | 삼성디스플레이 주식회사 | Display device |
| JP6296701B2 (en) * | 2012-10-15 | 2018-03-20 | 住友化学株式会社 | Manufacturing method of electronic device |
| JP6265697B2 (en) | 2013-11-18 | 2018-01-24 | サムスン エスディアイ カンパニー，リミテッドＳａｍｓｕｎｇ Ｓｄｉ Ｃｏ．，Ｌｔｄ． | Adhesive composition for polarizing plate |
| WO2015072800A1 (en) * | 2013-11-18 | 2015-05-21 | 삼성에스디아이 주식회사 | Adhesive composition for polarizing plate |
| CN106569296B (en) * | 2015-10-07 | 2020-08-14 | 住友化学株式会社 | Polarizing plate |
| JP6335360B2 (en) * | 2017-04-27 | 2018-05-30 | 日東電工株式会社 | Polarizing plate, method for producing the polarizing plate, optical film, and image display device |
| KR102649217B1 (en) * | 2021-11-03 | 2024-03-20 | 정낙군 | Method for fabricating x-ray grids and x-ray grids |
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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 |
| JP3428176B2 (en) * | 1994-09-22 | 2003-07-22 | ジェイエスアール株式会社 | Polarizing film |
| 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 |
| JP4276407B2 (en) * | 2002-05-08 | 2009-06-10 | ヘンケル コーポレイション | Photocationically curable epoxy resin composition |
| 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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