WO2016010115A1 - 積層フィルム - Google Patents
積層フィルム Download PDFInfo
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- WO2016010115A1 WO2016010115A1 PCT/JP2015/070420 JP2015070420W WO2016010115A1 WO 2016010115 A1 WO2016010115 A1 WO 2016010115A1 JP 2015070420 W JP2015070420 W JP 2015070420W WO 2016010115 A1 WO2016010115 A1 WO 2016010115A1
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- film
- meth
- laminated film
- acrylate
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2433/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C08J2433/10—Homopolymers or copolymers of methacrylic acid esters
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F2201/00—Constructional arrangements not provided for in groups G02F1/00 - G02F7/00
- G02F2201/08—Constructional arrangements not provided for in groups G02F1/00 - G02F7/00 light absorbing layer
- G02F2201/086—UV absorbing
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F2201/00—Constructional arrangements not provided for in groups G02F1/00 - G02F7/00
- G02F2201/50—Protective arrangements
Definitions
- the present invention relates to a laminated film having a base film and a cured film provided on one or both sides of the base film.
- a film containing a cyclic olefin resin has high transparency and low water absorption, and for example, use of a conductive film constituting a touch panel or the like as a base film has been studied.
- Patent Document 1 Also known is a technique of forming a hard coat layer having excellent scratch resistance on both surfaces of a base film using a relatively low molecular weight acrylate (see, for example, Patent Document 1).
- a film containing a cyclic olefin resin has a low surface hardness, and the surface using the film may be scratched. It is possible to impart a certain degree of scratch resistance by forming a hard coat layer, but in that case, there is a problem that cracking tends to occur when the film is bent.
- a main object of the present invention is to provide a laminated film having excellent scratch resistance and flexibility while having a film containing a cyclic olefin resin as a base film.
- the present invention relates to a laminated film comprising a base film and a cured film that is a cured composition provided on one or both sides of the base film and cured.
- the base film is a film containing a cyclic olefin resin.
- the curable resin composition comprises (A) an acrylic resin having a polymerizable double bond, (B) three or more polymerizable double bonds, and a group containing the polymerizable double bond represented by the following general formula ( (2-1) or a polyfunctional polymerizable compound having one or more monovalent groups represented by (2-2), and (C) an alkylene oxide-modified bisphenol A di (C) represented by the following general formula (3): Contains (meth) acrylate.
- an arbitrary resin layer (film) can be provided on the surface of the base film on which the cured film is not provided as long as the effects of the present invention are not substantially impaired.
- Arbitrary resins such as cyclic olefin resin or an acrylic resin, can be used.
- R 1 represents a hydrogen atom or a methyl group
- d represents an integer of 2 to 4
- e represents an integer of 1 to 6.
- R 1 represents a hydrogen atom or a methyl group, m is 5, and n is an integer of 1 to 4.
- R 1 represents a hydrogen atom or a methyl group
- f represents an integer of 2 to 5
- g and h represent an integer of 1 or more
- g + h is 2 to 40.
- double bond equivalent molecular weight / number of polymerizable double bonds in the same molecule
- the double bond equivalent of the polyfunctional polymerizable compound is 130 or more and 500 or less. It may be.
- the polyfunctional polymerizable compound is a compound different from the acrylic resin.
- the double bond equivalent of the acrylic resin may be 220 or more and 2500 or less. Thereby, both scratch resistance and flexibility can be achieved at a higher level.
- the weight average molecular weight of the acrylic resin may be 5000 or more and 200,000 or less. Thereby, both scratch resistance and flexibility can be achieved at a higher level.
- the double bond equivalent of the polyfunctional polymerizable compound may be 130 or more and 300 or less. Thereby, the more excellent effect is acquired at the point of the abrasion resistance of a cured film.
- F in Formula (3) may be 2. Thereby, both scratch resistance and flexibility can be achieved at a higher level.
- the curable composition may further contain (D) a urethane (meth) acrylate having a urethane group and two or more (meth) acryloyl groups. Thereby, the more excellent effect is acquired at the point of the abrasion resistance of a cured film.
- the curable composition comprises 8 to 40 parts by mass of an acrylic resin, 40 to 80 parts by mass of a polyfunctional polymerizable compound, and 4 to 40 parts by mass of an alkylene oxide-modified bisphenol A di (meth) acrylate.
- Part or less, urethane (meth) acrylate may be included in a ratio of 0.5 parts by mass or more and 15 parts by mass or less.
- the curable composition may further contain (E) a photopolymerization initiator.
- the curable composition may contain fine particles (F) in order to adjust optical properties such as refractive index or to improve antiblocking properties.
- the base film may be a stretched film. Thereby, optical characteristics, such as retardation, can be expressed in the base film.
- the stretched film may be a diagonally stretched film.
- a base film that is an obliquely stretched film is suitable as a quarter-wave plate, for example.
- the quarter-wave plate generally needs to be bonded to the polarizer so that the slow axis and the transmission axis of the polarizer intersect at a predetermined angle that is neither parallel nor perpendicular.
- the obliquely stretched film can have a slow axis along a predetermined oblique direction that is neither parallel nor perpendicular to the width direction of the film, without requiring a cutting step before bonding, It can be efficiently bonded to a polarizer or the like by a to-roll method.
- the base film may be a multilayer film.
- the multilayer film can have, for example, an ultraviolet absorbing intermediate layer. Thereby, deterioration by the external light of a polarizer and a liquid crystal element can be prevented.
- the multilayer film further includes a surface layer that does not contain an ultraviolet absorber, thereby preventing contamination of the film transport roll and the film during the process.
- Another aspect of the present invention relates to a liquid crystal display device including a liquid crystal cell, a polarizer, and the laminated film.
- a polarizer and a laminated film are laminated in this order on the viewing side of the liquid crystal cell, and the laminated film is laminated in such a direction that the base film and the cured film are arranged in this order from the liquid crystal cell side.
- the liquid crystal cell may be an IPS liquid crystal cell.
- the laminated film of the present invention is excellent in both scratch resistance and flexibility.
- the laminated film of the present invention is less prone to burr on the end face when cut, and is excellent in workability.
- the curable composition of the present invention it is possible to obtain a sufficient function as a cured film by a single layer composed of an organic material without requiring other films such as a film of an inorganic material.
- the laminated film of the present invention is also excellent in terms of adhesion between the cyclic olefin resin film and the cured film.
- (meth) acryl means methacryl or acryl.
- (meth) acrylate means methacryl or acryl.
- the laminated film according to the present embodiment includes a base film and a cured film provided on one or both sides of the base film.
- the cured film is formed by curing a film of the curable composition.
- the base film may be a single-layer film consisting of only one layer or a multilayer film including two or more layers.
- FIG. 1 is a cross-sectional view showing an embodiment of a laminated film.
- a laminated film 1 shown in FIG. 1 is a multilayer film having a base film 10 and a cured film 3 provided on one side of the base film 10.
- the cured film may cover the entire surface of one side or both sides of the base film, or may cover a part thereof. Some layer (a primer layer, a barrier layer, etc.) may be provided between the cured film and the base film.
- a laminated film can be used to obtain a transparent conductive film having a transparent conductive layer or a barrier film.
- multilayer film, or between a cured film and a transparent conductive layer A configuration in which a refractive index adjusting layer is formed therebetween can be employed. That is, this laminated film used as a transparent conductive film further includes, for example, a barrier layer provided between the base film and the cured film, and a transparent conductive layer directly provided on the cured film. May be.
- the refractive index adjusting layer may be a single layer or a multilayer. By forming the refractive index adjusting layer, there is an advantage that the conductive layer pattern can be hardly seen.
- this laminated film used as a barrier film for example, a configuration in which a barrier layer is directly formed on a cured film constituting the laminated film, or a configuration in which an adhesion layer is formed between the cured film and the barrier layer. Can be adopted. That is, this laminated film used as a barrier film may further have, for example, a barrier layer provided between the base film and the cured film.
- Base film A base film is a film containing a cyclic olefin resin.
- the film containing a cyclic olefin resin is a molded product of a cyclic olefin resin composition containing a cyclic olefin resin and, if necessary, an additive.
- the base film 10 is provided on the intermediate layer 15, the first surface layer 11 laminated on one main surface side of the intermediate layer 15, and the other main surface side of the intermediate layer 15.
- the second surface layer 12 is a multilayer film, and each of these layers may contain a cyclic olefin resin.
- Cyclic olefin resins are known to those skilled in the art, for example, as disclosed in JP-A-3-14882, JP-A-3-122137, JP-A-4-63807, or JP-A-2002-332102. Resin. Specifically, the cyclic olefin resin is, for example, a ring-opening polymer of norbornene or a derivative thereof, a hydrogenated product of the polymer, an addition polymer of norbornene or a derivative thereof, or an addition type of norbornene or a derivative thereof and an olefin.
- a norbornene derivative is a compound represented, for example by following formula (10).
- j is an integer of 0 or more
- R 2 , R 3 , R 4 , R 5 , R 6 , R 7 , R 8 , R 9 are each independently a hydrogen atom, a halogen atom, or R represents a hydrocarbon group which may be substituted with a halogen atom
- R 10 , R 11 , R 12 and R 13 are each independently a hydrogen atom, a halogen atom or a hydrocarbon group which may be substituted with a halogen atom, or , — (CH 2 ) k COOR 21 , — (CH 2 ) k OCOR 21 , — (CH 2 ) k OR 21 , — (CH 2 ) k CN, — (CH 2 ) k CONR 22 R 23 , — (CH 2 ) a group represented by COOZ, — (CH 2 ) OCOZ, — (CH 2 ) k OZ or — (CH 2 )
- R 10 , R 11 , R 12 and R 13 may be bonded to each other to form a monocyclic or polycyclic group, and the monocyclic or polycyclic group may contain a double bond.
- R 10 and R 11 , or R 12 and R 13 may form an alkylidene group.
- An acid anhydride group or an imide group may be formed by any one of R 10 and R 11 and any one of R 12 and R 13 .
- cyclic olefin resins examples include ZEONEX and ZEONOR (norbornene resin) manufactured by Nippon Zeon Co., Ltd., Sumilite FS-1700 manufactured by Sumitomo Bakelite Co., Ltd., Arton (modified norbornene system manufactured by JSR Corporation). Resin), Appell (cyclic olefin copolymer) manufactured by Mitsui Chemicals, Ltd., Topas (cyclic olefin copolymer) manufactured by Ticona, and Optretz OZ-1000 series (alicyclic) manufactured by Hitachi Chemical Co., Ltd. Formula acrylic resin).
- the number average molecular weight of the cyclic olefin resin is 10,000 to 200,000, 15,000 to 100,000, or 20, as a polyisoprene conversion value measured by a GPC (gel permeation chromatography) method using a cyclohexane solvent. It may be 000 to 50,000.
- the glass transition temperature (Tg) of the cyclic olefin resin may be 100 ° C. or higher, 120 ° C. or higher, or 130 ° C. or higher.
- Tg glass transition temperature
- the base film Deformation may occur.
- an annealing treatment is generally performed at a temperature of about 150 ° C. in order to lower the resistance value of the conductive layer, so that the glass transition temperature of the cyclic olefin resin is 150 ° C. or higher. It may be.
- the glass transition temperature of the cyclic olefin resin may be 180 ° C. or lower, 170 ° C. or lower, or 160 ° C. or lower. If the glass transition temperature of the cyclic olefin resin is excessively high, it may be difficult to form a film.
- the photoelastic coefficient C of the cyclic olefin resin may be 10 ⁇ 10 ⁇ 10 ⁇ Pa ⁇ 1 or less, 10 ⁇ 10 ⁇ 12 Pa ⁇ 1 or less, or 4 ⁇ 10 ⁇ 12 Pa ⁇ 1 or less.
- the photoelastic coefficient C of cyclic olefin resin is small, the change of the retardation of the base film resulting from the tensile stress which a laminated film receives in processes, such as bonding, can be suppressed.
- the base film is optionally made of an anti-aging agent such as phenol and phosphorus; an anti-aging agent such as phenol; an ultraviolet stabilizer such as benzophenone; an antistatic agent such as amine; an ester of an aliphatic alcohol; Various additives such as lubricants such as partial esters and partial ethers of polyhydric alcohols may be included.
- the base film can further contain a resin other than the cyclic olefin resin without departing from the gist of the present invention.
- the ratio of the cyclic olefin resin in the substrate film is usually 80% by mass or more based on the mass of the substrate film.
- the forming method of the base film is not particularly limited. Injection molding, melt extrusion, hot pressing, solvent casting, stretching, and the like can be used. Especially, since the volatile component in a base film can be reduced, the melt extrusion method is preferable.
- the thickness of the base film may be 10 ⁇ m or more, 20 ⁇ m or more, or 30 ⁇ m or more, or 250 ⁇ m or less or 200 ⁇ m or less.
- the thickness (total thickness) may be 10 ⁇ m or more, 20 ⁇ m or more, or 25 ⁇ m or more, or 250 ⁇ m or less, 150 ⁇ m or less, or 100 ⁇ m or less.
- the thickness of the base film can be measured by, for example, a contact-type film thickness meter (“Dial Gauge” manufactured by Mitutoyo Corporation).
- the base film (cyclic olefin resin film) may be a film having an in-plane and / or thickness direction retardation value of 10 nm or less.
- the base film may be a retardation film having an in-plane retardation value Re and a thickness direction retardation value Rth of arbitrary values.
- the retardation film may be a film having the characteristics of a quarter wavelength plate having an in-plane retardation value of 100 to 150 nm with respect to visible transmission light of 550 nm and a retardation value in the thickness direction of 60 to 225 nm. Good.
- nx represents a refractive index in a direction (in-plane direction) perpendicular to the thickness direction of the film and giving the maximum refractive index.
- ny represents a refractive index in the in-plane direction and in a direction orthogonal to the direction giving nx.
- nz represents the refractive index in the thickness direction.
- d represents the thickness of the film.
- the measurement wavelength is 550 nm unless otherwise specified.
- the retardation value can be measured using, for example, “AxoScan” (Axometrics) or “KOBRA-21ADH” (Oji Scientific).
- the variation of the in-plane retardation value Re of the base film may be within 10 nm, within 5 nm, or within 2 nm.
- the variation of the retardation value Rth in the thickness direction of the base film may be within 20 nm, within 15 nm, or within 10 nm. If the variations in retardation values Re and Rth are within these ranges, good display quality of the liquid crystal display device tends to be easily obtained.
- the retardation film can be obtained, for example, by stretching a film containing a cyclic olefin resin.
- the stretching may be, for example, longitudinal stretching, lateral stretching, sequential biaxial stretching, simultaneous biaxial stretching, or oblique stretching.
- the base film that can function as a quarter-wave plate is preferably an obliquely stretched film. Examples of the stretching method include a roll method, a float method, and a tenter method.
- Examples of the base film having the characteristics of a 1 ⁇ 4 wavelength plate include an unstretched film, a longitudinally stretched film, and an obliquely stretched film of ZEONOR film manufactured by Nippon Zeon.
- Sumitomo Bakelite's Sumilite FS-1700, JSR's Arton, Mitsui Chemicals' Appel, TICONA's TOPAS, Hitachi Chemical's Optretz OZ-1000 Series, etc. are subjected to film forming processing and stretched Film may be used.
- the intermediate layer may contain a cyclic olefin resin and an ultraviolet absorber.
- the first surface layer and the second surface layer include a cyclic olefin resin and may be substantially free of an ultraviolet absorber.
- the cyclic olefin resin contained in each of the first surface layer, the intermediate layer, and the second surface layer may be the same or different.
- the cyclic olefin resin of each layer is the same, formation of a layer is easy.
- a 1st surface layer and a 2nd surface layer can be formed with the same cyclic olefin resin as the cyclic olefin resin contained in an intermediate
- the glass transition temperature TgA of the cyclic olefin resin contained in the intermediate layer and the glass transition temperature TgB of the cyclic olefin resin contained in the first surface layer and the second surface layer satisfy the relationship of 0 ° C. ⁇ TgB ⁇ TgA ⁇ 15 ° C. It may be.
- UV absorber examples include organic UV absorbers such as triazine UV absorbers, benzophenone UV absorbers, benzotriazole UV absorbers, and acrylonitrile UV absorbers.
- organic UV absorbers such as triazine UV absorbers, benzophenone UV absorbers, benzotriazole UV absorbers, and acrylonitrile UV absorbers.
- Benzotriazole-based ultraviolet absorbers are particularly excellent in terms of ultraviolet absorption performance near a wavelength of 380 nm.
- the molecular weight of the ultraviolet absorber may be 400 or more, or 1500 or less.
- the triazine-based ultraviolet absorber may be, for example, a compound having a 1,3,5-triazine ring.
- Specific examples of the triazine-based ultraviolet absorber include 2- (4,6-diphenyl-1,3,5-triazin-2-yl) -5-[(hexyl) oxy] -phenol, and 2,4- Bis (2-hydroxy-4-butoxyphenyl) -6- (2,4-dibutoxyphenyl) -1,3,5-triazine.
- a commercial item of a triazine ultraviolet absorber for example, “Tinuvin 1577” (manufactured by Ciba Specialty Chemicals) can be mentioned.
- benzotriazole ultraviolet absorber examples include 2,2′-methylenebis [4- (1,1,3,3-tetramethylbutyl) -6- (2H-benzotriazol-2-yl) phenol], 2 -(3,5-di-tert-butyl-2-hydroxyphenyl) -5-chlorobenzotriazole, 2- (2H-benzotriazol-2-yl) -p-cresol, 2- (2H-benzotriazole-2 -Yl) -4,6-bis (1-methyl-1-phenylethyl) phenol, 2-benzotriazol-2-yl-4,6-di-tert-butylphenol, 2- [5-chloro (2H)- Benzotriazol-2-yl] -4-methyl-6- (tert-butyl) phenol, 2- (2H-benzotriazol-2-yl) -4,6-di- ert-Butylphenol, 2- (2H-benzotriazol-2-yl
- ultraviolet absorber one type may be used alone, or two or more types may be used in combination at any ratio.
- the amount of the ultraviolet absorber in the intermediate layer may be 1 part by mass or more, 3 parts by mass or more, or 10 parts by mass or less, or 8 parts by mass or less, with the mass of the intermediate layer being 100 parts by mass. Good.
- the amount of the ultraviolet absorber here means the total amount of the ultraviolet absorbers when two or more types of ultraviolet absorbers are used.
- the amount of the ultraviolet absorber is not less than the lower limit of the above range, the transmission of ultraviolet rays having a wavelength of 200 nm to 370 nm can be effectively suppressed. Since the yellowishness of a film is suppressed as the quantity of a ultraviolet absorber is below the upper limit of the said range, deterioration of a color can be suppressed. The fall of the heat resistance of cyclic olefin resin can be suppressed as the quantity of a ultraviolet absorber is in the said range. Moreover, it is easy to ensure good dispersibility of the ultraviolet absorber.
- the thickness of the intermediate layer may be 10 ⁇ m or more and 40 ⁇ m or less, and the total thickness of the first surface layer and the second surface layer may be 5 ⁇ m or more and 20 ⁇ m or less.
- the variation in the thickness of the intermediate layer is within ⁇ 2.0 ⁇ m in the entire intermediate layer, it is easy to obtain good image display properties of the liquid crystal display device.
- the multilayer film as the base film can be produced by, for example, a coextrusion method.
- a multilayer film including a first surface layer, an intermediate layer, and a second surface layer includes a cyclic olefin resin for forming the first surface layer, a cyclic olefin resin for forming the intermediate layer, and a second surface layer. It can manufacture by co-extruding the cyclic olefin resin for forming from a die
- the coextrusion methods the coextrusion T-die method is preferable. Examples of the co-extrusion T-die method include a feed block method and a multi-manifold method.
- the melting temperature of the cyclic olefin resin in the extruder having a T die used in the coextrusion T die method may be Tg + 80 ° C. or higher, or Tg + 100 ° C. or higher, or Tg + 180 ° C. or lower, or Tg + 150 ° C. or lower.
- Tg indicates the glass transition temperature of the cyclic olefin resin. This Tg is the glass transition temperature of the cyclic olefin resin contained in the first surface layer and the second surface layer when the substrate film includes the first surface layer, the intermediate layer, and the second surface layer.
- liquidity of cyclic olefin resin can fully be improved as the melting temperature in an extruder is more than the lower limit of the said range.
- the melting temperature in the extruder is not more than the upper limit of the above range, the deterioration of the cyclic olefin resin can be suppressed.
- the temperature of the cyclic olefin resin in the extruder may be Tg to (Tg + 100) ° C. at the resin inlet and (Tg + 50) to (Tg + 170) ° C. at the extruder outlet.
- the die temperature may be (Tg + 50) ° C. to (Tg + 170) ° C.
- the intermediate layer containing an ultraviolet absorber can be formed using a cyclic olefin resin composition containing a cyclic olefin resin and an ultraviolet absorber.
- This cyclic olefin resin composition is prepared by, for example, a method of blending a UV absorber with a cyclic olefin resin before production of a base film by a melt extrusion method; a method using a master batch containing a high concentration of a UV absorber; It can manufacture by the method of mix
- the light transmittance at a wavelength of 380 nm of the film may be 10% or less, 5% or less, or 1% or less.
- the light transmittance at a wavelength of 280 nm to 370 nm of the base film may be 1.5% or less, or 1% or less.
- the lower limit of the light transmittance at a wavelength of 380 nm and the light transmittance at a wavelength of 280 nm to 370 nm of the base film is 0%.
- the light transmittance of the base film When the light transmittance of the base film is small, damage to the polarizer and the liquid crystal cell due to ultraviolet rays can be suppressed in a liquid crystal display device including the base film. Therefore, it is possible to suppress a decrease in the degree of polarization of the polarizer and coloring. Furthermore, the liquid crystal driving of the liquid crystal cell can be stabilized.
- the light transmittance can be measured using a spectrophotometer according to JIS K0115.
- the amount of the volatile component of the base film may be 0.1% or less, 0.05% or less, or 0.02% or less based on the mass of the base film.
- the volatile component means a substance having a molecular weight of 200 or less. Examples of volatile components include residual monomers and solvents.
- the total amount of volatile components can be quantified by analysis using gas chromatography.
- the base film (cyclic olefin resin film) may be subjected to a surface treatment for the purpose of enhancing adhesion with a cured film (surface layer).
- the surface treatment include plasma treatment, corona treatment, alkali treatment, and coating treatment.
- corona treatment by using corona treatment, the adhesion between the base film and the cured film can be particularly strengthened.
- the dose of corona discharge electrons during the corona treatment is, for example, 1 to 1000 W / m 2 / min.
- the contact angle of the base film after corona treatment with respect to water may be 10 to 50 °.
- the curable composition may be applied, or may be applied after the base film is neutralized. From the point that the appearance of the surface layer becomes good, the curable composition can be applied after neutralizing the base film after the corona treatment.
- the cured film may exhibit a hardness of “B” or higher in the pencil hardness test specified by JISK5600-5-4 (1999).
- the thickness of the cured film may be 1.0 ⁇ m or more, or 2.0 ⁇ m or more. Further, the thickness of the cured film may be 10.0 ⁇ m or less. If the cured film is too thick, the visibility may be lowered. If the cured film is too thin, the scratch resistance and the like tend to be relatively lowered. When providing a cured film on both surfaces of a base film, although the thickness of two cured films may differ, those thickness may be the same in order to prevent the curling etc. of a laminated film. The thickness of the cured film can be measured by, for example, an interference film thickness meter ("F20 film thickness measurement system" manufactured by Filmetrics).
- Concave and convex portions may be formed on the surface of the cured film.
- the arithmetic average roughness (Ra) of the surface of the cured film may be 0.001 ⁇ m or more and 0.1 ⁇ m or less, or 0.01 ⁇ m or more and 0.1 ⁇ m or less.
- the ten-point average roughness (Rz) of the surface of the cured film may be from 0.01 ⁇ m to 1.0 ⁇ m, or from 0.1 ⁇ m to 1.0 ⁇ m.
- the arithmetic average roughness (Ra) and ten-point average roughness (Rz) of the cured film can be measured using a color 3D laser microscope (VK-9700 manufactured by Keyence Corporation) or an atomic force microscope (NanoScope IIIa manufactured by Digital Instruments). .
- the haze value of the cured film may be 1.0% or less, 0.5% or less, or 0.3% or less.
- the laminated film can be used, for example, in a display device having a touch panel.
- the haze value of the cured film can be measured using a haze meter (“Haze Guard II” manufactured by Toyo Seiki Co., Ltd.) in accordance with JIS K7136.
- the static friction coefficient and the dynamic friction coefficient between the cured film and the base film (cyclic olefin resin film) may be 0.9 or less, or 0.6 or less.
- the laminated film including the cured film according to the present embodiment has excellent scratch resistance.
- scratch resistance for example, when the steel wool is reciprocated while pressing # 0000 steel wool against the surface of the cured film (coat layer) with a predetermined load, the surface of the coat layer is visually checked. It can be evaluated by the method.
- the scratch resistance can be quantified based on the maximum value of the load in which no scratches are confirmed on the surface. This maximum value may be 150 gf or more, 200 gf or more, or 250 gf or more in order to prevent the film surface from being damaged in the manufacturing process of an image display device such as a touch panel.
- the upper limit of the scratch resistance value is not particularly limited, but is usually 500 gf or less or 2000 gf or less.
- the laminated film according to the present embodiment has excellent flexibility and is less likely to be cracked when folded.
- the bendability of the coat film is determined by wrapping the coat film around a mandrel or piano wire having a predetermined diameter with the coat layer facing outward, and visually confirming the presence or absence of cracks in the wound coat film (hereinafter, “ It may be referred to as “cylindrical mandrel method”), or a simple test (hereinafter also referred to as “mountain fold method”) in which the laminated film is folded in a mountain and completely folded.
- the mountain fold method is an operation where the laminated film is completely folded (folded 180 °) in any direction of the laminated film with the cured film facing outward, and the presence or absence of cracks in the cured film is visually confirmed. It is a method to do. According to the mountain fold method, a significant difference in flexibility can be detected as compared with the cylindrical mandrel method. When the diameter of the mandrel or piano wire is reduced stepwise, the flexibility can be quantified based on the minimum value of the diameter of the mandrel or piano wire in which no crack has occurred.
- the diameter of a mandrel or piano wire that cracks in a bendability test by the cylindrical mandrel method may be less than 1.5 mm, less than 1 mm, or less than 0.5 mm.
- this flexibility value is within these ranges, it is possible to effectively prevent cracks that occur during slit cutting or punching of the film. With such a laminated film having flexibility, it is possible to particularly effectively prevent the cured film from cracking or burr at the end of the cut in the manufacturing process of an image display device such as a touch panel.
- the lower limit of the flexibility value is not particularly limited, but may be, for example, 0 mm or more or 0.01 mm or more.
- the laminated film according to the present embodiment includes, for example, a step of forming a film of a curable composition on a base film and a step of forming a cured film by curing the film of the curable composition. It can obtain by the method containing these.
- the film of the curable composition can be formed by, for example, a method in which the curable composition is applied onto a base film and the solvent is removed from the applied curable composition as necessary.
- the temperature and pressure for removing the solvent can be appropriately set according to conditions such as the type of material of the curable composition, the type of solvent, and the coating thickness of the curable composition. Examples of the coating method include spin coating, bar coating, and dipping.
- the film can be cured by irradiating the film of the curable composition with ultraviolet rays. Irradiation with ultraviolet rays may be performed in, for example, an inert gas such as nitrogen and argon, or in the air.
- the curing temperature is not particularly limited as long as the curable composition can be cured, but is generally about 30 ° C to 180 ° C, or about 60 ° C to 150 ° C.
- the curing time can be set over a wide range depending on the curing temperature, for example, in the range of 30 seconds to 10 hours or more.
- the surface of the base film before applying the curable composition may be subjected to a surface treatment by corona treatment, saponification treatment, heat treatment, ultraviolet irradiation, electron beam irradiation or the like.
- the curable composition used for forming the cured film includes (A) an acrylic resin having a polymerizable double bond, (B) a polyfunctional polymerizable compound having a specific structure, and (C) an alkylene oxide-modified bisphenol.
- a di (meth) acrylate may be included.
- the curable composition may further contain other components such as (D) urethane (meth) acrylate and (E) photopolymerization initiator, if necessary.
- (A) Acrylic resin having a polymerizable double bond An acrylic resin having a polymerizable double bond is, for example, bonded to a main chain composed of a copolymer containing (meth) acrylic acid ester as a monomer unit, and the main chain. And a side chain containing a polymerizable double bond.
- the side chain containing a polymerizable double bond typically contains a (meth) acryloyl group, but is not limited thereto.
- acrylic resin having a polymerizable double bond examples include one or more (meth) acrylic acid esters (a1) and one or more polymerizable compounds (a2) having a reactive functional group.
- acrylic resin having a reactive functional group examples include one or more (meth) acrylic acid esters (a1) and one or more polymerizable compounds (a2) having a reactive functional group.
- a1 acrylic acid esters
- a2 polymerizable compounds
- an acrylic resin having a reactive functional group and one or more compounds having a functional group that reacts with the reactive functional group of the acrylic resin and a polymerizable double bond (b ) Is reacted with an acrylic resin to introduce a polymerizable double bond into the side chain of the acrylic resin.
- (Meth) acrylic acid ester (a1) is, for example, linear or branched alkyl (meth) acrylate, alicyclic (meth) acrylate, aromatic (meth) acrylate, alkoxyalkyl (meth) acrylate, alkoxy (poly) alkylene It may be at least one selected from the group consisting of glycol (meth) acrylate, alkoxyalkoxyalkyl (meth) acrylate, octafluoropentyl (meth) acrylate, and dialkylaminoalkyl (meth) acrylate.
- linear or branched alkyl (meth) acrylate examples include methyl (meth) acrylate, ethyl (meth) acrylate, n-propyl (meth) acrylate, n-butyl (meth) acrylate, isobutyl (meth) acrylate, t- Examples include butyl (meth) acrylate, ethylhexyl (meth) acrylate, stearyl (meth) acrylate, lauryl (meth) acrylate, and tridecyl (meth) acrylate.
- Examples of the alicyclic (meth) acrylate include cyclohexyl (meth) acrylate, isobornyl (meth) acrylate, and dicyclopentanyl (meth) acrylate.
- aromatic (meth) acrylate examples include phenoxyethyl (meth) acrylate.
- alkoxyalkyl (meth) acrylate examples include ethoxyethyl (meth) acrylate and butoxyethyl (meth) acrylate.
- alkoxy (poly) alkylene glycol (meth) acrylate examples include methoxydiethylene glycol (meth) acrylate, ethoxydiethylene glycol (meth) acrylate, methoxytriethylene glycol (meth) acrylate, butoxytriethylene glycol (meth) acrylate, and methoxydi Examples include propylene glycol (meth) acrylate.
- alkoxyalkoxyalkyl (meth) acrylate examples include 2-methoxyethoxyethyl (meth) acrylate and 2-ethoxyethoxyethyl (meth) acrylate.
- octafluoropentyl (meth) acrylate examples include 1H, 1H, 5H-octafluoropentyl (meth) acrylate.
- dialkylaminoalkyl (meth) acrylate examples include N, N-dimethylaminoethyl (meth) acrylate and N, N-diethylaminoethyl (meth) acrylate.
- the polymerizable compound (a2) may have one or more reactive functional groups selected from the group consisting of an epoxy group and a hydroxyl group.
- the epoxy group and the hydroxyl group have good reactivity with the compound (b) having a carboxyl group, an isocyanate group or the like.
- Examples of the polymerizable compound (a2) having an epoxy group as a reactive functional group include glycidyl (meth) acrylate and (meth) acrylate having an epoxy group such as 3,4-epoxycyclohexyl (meth) acrylate. .
- Examples of the polymerizable compound (a2) having a hydroxyl group as a reactive functional group include hydroxy such as 2-hydroxyethyl (meth) acrylate, 2-hydroxybutyl (meth) acrylate, and 2-hydroxypropyl (meth) acrylate.
- hydroxy such as 2-hydroxyethyl (meth) acrylate, 2-hydroxybutyl (meth) acrylate, and 2-hydroxypropyl (meth) acrylate.
- An alkyl (meth) acrylate is mentioned.
- the acrylic resin may contain other polymerizable compounds as monomer units in addition to the (meth) acrylic acid ester (a1) and the polymerizable compound (a2).
- examples of other polymerizable compounds include aromatic vinyl compounds such as styrene and vinyl toluene.
- the compound (b) having a polymerizable double bond is at least one selected from the group consisting of a carboxyl group and an isocyanate group that reacts with a reactive functional group (epoxy group, hydroxyl group, etc.) of the polymerizable compound (a2). Has various functional groups.
- the compound (b) having a carboxyl group examples include (meth) acrylic acid, a dimer of (meth) acrylic acid (for example, Aronix M5600 manufactured by Toa Gosei Co., Ltd.), caprolactone-modified (meth) acrylic acid (for example, , ⁇ -carboxy-polycaprolactone monoacrylate, Aronix M5300 manufactured by Toagosei Co., Ltd., a compound obtained by ring-opening reaction of (meth) acrylate having a hydroxyl group and carboxylic anhydride (for example, monohydroxyethyl acrylate phthalate, Toago Aronix M5400 manufactured by Synthetic Co., Ltd.) and ⁇ -acryloyloxyethyl hydrogen succinate (for example, NK Ester A-SA manufactured by Shin-Nakamura Chemical Co., Ltd.).
- a dimer of (meth) acrylic acid for example, Aronix M5600 manufactured by Toa Gosei Co
- compound (b) having an isocyanate group examples include methacryloyloxyethyl isocyanate (for example, Karenz MOI manufactured by Showa Denko KK).
- the double bond equivalent of the acrylic resin having a polymerizable double bond may be 220 or more and 2500 or less. There exists a tendency for the flexibility of a coat film to fall that the double bond equivalent of an acrylic resin is less than 220. When the double bond equivalent of the acrylic resin is larger than 2500, the scratch resistance tends to decrease. For the same reason, the double bond equivalent of the acrylic resin may be 230 or more and 1000 or less, or 240 or more and 500 or less.
- double bond equivalent molecular weight / number of double bonds in the same molecule.
- the value of the double bond equivalent defined by the above formula is, for example, the amount of double bond in the sample quantified based on the iodine value measured by the method of JIS K0070 (established in 1992) and the mass of the sample. Alternatively, it can be estimated from the molecular weight.
- the double bond equivalent may be determined by fractionating each component as necessary and measuring the iodine value of the fractionated component.
- the weight average molecular weight of the acrylic resin having a polymerizable double bond may be 5000 or more and 200,000 or less. When the weight average molecular weight of the acrylic resin is 5000 or more, more excellent scratch properties are obtained, and when the weight average molecular weight of the acrylic resin is 200,000 or less, more excellent flexibility is obtained.
- the weight average molecular weight of the acrylic resin may be 10,000 or more and 100,000 or less, or 10,000 or more and 60000 or less, in that an excellent coating film appearance is obtained when the curable composition is applied to a transparent plastic film.
- the weight average molecular weight means a standard polystyrene equivalent value measured by gel permeation chromatography.
- the polyfunctional polymerizable compound used as the component (B) has three or more polymerizable double bonds.
- the group containing a polymerizable double bond is typically a (meth) acryloyl group, but is not limited thereto.
- the polyfunctional polymerizable compound has one, two, or three or more monovalent groups represented by the following general formula (2-1) or (2-2) as a group containing a polymerizable double bond. You may do it.
- the group of formula (2-1) or (2-2) as a group containing a polymerizable double bond, the stress when the cured film is deformed while maintaining high strength of the formed cured film Can be relaxed. As a result, excellent flexibility of the cured film can be obtained.
- the scratch resistance of the cured film is improved.
- the number of polymerizable double bonds in the polyfunctional polymerizable compound may be 6 or more and 9 or less. All of the polymerizable double bonds in the polyfunctional polymerizable compound may be contained in the group of the formula (2-1) or (2-2), or the polyfunctional polymerizable compound is represented by the formula (2-1). ) Or a group containing a polymerizable double bond in addition to the group (2-2).
- R 1 represents a hydrogen atom or a methyl group
- d represents an integer of 2 to 4
- e represents an integer of 1 to 6.
- R 1 represents a hydrogen atom or a methyl group
- m is 5, and n is an integer of 1 to 4.
- the double bond equivalent of the polyfunctional polymerizable compound may be 130 to 500, 130 to 300, or 130 to 250. Thereby, a more excellent effect can be obtained in terms of the scratch resistance of the protective film.
- alkylene oxide modification means a compound having an oxyethylene group or a polyoxyethylene group formed by adding an alkylene oxide such as ethylene oxide to a hydroxyl group of an alcohol compound.
- Ethylene oxide modification may be abbreviated as “EO modification”
- propylene oxide modification may be abbreviated as “PO modification”.
- the polyfunctional polymerizable compound derived from the alkylene oxide-modified polyhydric alcohol has a monovalent group of the formula (2-1).
- caprolactone modification means a compound having a divalent group formed by reacting a hydroxyl group of an alcohol compound with caprolactone (eg, ⁇ -caprolactone).
- the polyfunctional polymerizable compound derived from caprolactone-modified polyhydric alcohol has a monovalent group represented by the formula (2-2).
- the (meth) acrylic acid ester of alkylene oxide-modified or caprolactone-modified polyhydric alcohol is represented, for example, by the following general formula (20).
- R 10 represents a polyhydric alcohol residue (a portion excluding the hydroxyl group) having 3 or more hydroxyl groups
- Z is represented by the formula (2-1) or (2-2).
- a monovalent group having a polymerizable double bond other than these x represents an integer of 3 or more, y represents an integer of 0 or more, and x + y represents a valence of R 10 equal.
- Plural Zs in one molecule may be the same or different, and one or more of the plural Zs are monovalent groups represented by the formula (2-1) or (2-2).
- x + y total number of hydroxyl groups of the polyhydric alcohol
- x may be 3 to 9.
- the polyhydric alcohol corresponding to R 10 can be, for example, at least one selected from the group consisting of polyglycerin, dipentaerythritol, pentaerythritol, and trimethylolpropane.
- polyfunctional polymerizable compound examples include alkylene oxide modified or caprolactone modified dipentaerythritol hexa (meth) acrylate, alkylene oxide modified or caprolactone modified dipentaerythritol penta (meth) acrylate, alkylene oxide modified or caprolactone modified dipentaerythritol.
- an alkylene oxide-modified or caprolactone-modified dipentaerythritol hexa (meth) acrylate may be used in combination with an alkylene oxide-modified or caprolactone-modified polyglycerol polyacrylate.
- alkylene oxide modified bisphenol A di (meth) acrylate has a structure containing an oxyalkylene group represented by the following general formula (3).
- R 1 represents a hydrogen atom or a methyl group
- f represents an integer of 2 to 5
- g and h represent an integer of 1 or more
- g + h is 2 to 40.
- f may be 2 or 3. That is, the alkylene oxide modified bisphenol A di (meth) acrylate may be ethylene oxide modified (EO modified) or propylene oxide modified (PO modified) bisphenol A di (meth) acrylate.
- g + h may be 10 or more and 40 or less, or 25 or more and 35 or less. When g + h is within these ranges, a cured film having particularly excellent flexibility with improved stress relaxation can be obtained.
- the curable composition may contain one or more compounds represented by the formula (3).
- the curable composition comprises (A) an acrylic resin having a polymerizable double bond in an amount of 8 to 40 parts by mass, 10 to 25 parts by mass, or It may be included at a ratio of 12 parts by mass or more and 20 parts by mass or less.
- an acrylic resin having a polymerizable double bond in an amount of 8 to 40 parts by mass, 10 to 25 parts by mass, or It may be included at a ratio of 12 parts by mass or more and 20 parts by mass or less.
- the amount of the acrylic resin is within this range, both scratching and flexibility can be achieved at a higher level. If the amount of the acrylic resin is less than 8 parts by mass, the flexibility tends to be relatively lowered. When the amount of the acrylic resin is more than 40 parts by mass, the scratch resistance tends to be relatively lowered.
- the curable composition may contain (B) the polyfunctional polymerizable compound in a ratio of 40 parts by mass to 80 parts by mass, 45 parts by mass to 73 parts by mass, or 58 parts by mass to 69 parts by mass. Good.
- the amount of the polyfunctional polymerizable compound is within the range, both scratch resistance and flexibility can be achieved at a higher level.
- the amount of the polyfunctional polymerizable compound is less than 40 parts by mass, the scratch resistance tends to be relatively lowered.
- the amount of the polyfunctional polymerizable compound is more than 80 parts by mass, the flexibility tends to be relatively lowered.
- the curable composition comprises (C) alkylene oxide-modified bisphenol A di (meth) acrylate in a ratio of 4 parts by mass to 40 parts by mass, 5 parts by mass to 30 parts by mass, or 10 parts by mass to 20 parts by mass. May be included.
- the amount of the alkylene oxide-modified bisphenol A di (meth) acrylate is within this range, both scratch resistance and flexibility can be achieved at a higher level. If the amount of the alkylene oxide-modified bisphenol A di (meth) acrylate is less than 4 parts by mass, the flexibility tends to be relatively lowered. When the amount of the alkylene oxide-modified bisphenol A di (meth) acrylate is more than 40 parts by mass, the scratch resistance tends to be relatively lowered.
- ratios can be adjusted with the total mass of the curable composition, or, when the curable composition contains a solvent, the total mass of the components excluding the solvent from the curable composition as 100 parts by mass. The same applies to the ratio of other components.
- the curable composition may contain a urethane (meth) acrylate having one or more urethane groups and two or more (meth) acryloyl groups. Urethane (meth) acrylate can contribute to further improvement of the scratch resistance of the cured film.
- the double bond equivalent of urethane (meth) acrylate When the double bond equivalent of urethane (meth) acrylate is small, the scratch resistance tends to be further improved. Specifically, the double bond equivalent of urethane (meth) acrylate may be less than 130 or 80 or more.
- Urethane (meth) acrylate can be obtained, for example, by a reaction between a polyisocyanate compound having two or more isocyanate groups and a hydroxyl group-containing (meth) acrylate having a hydroxyl group and a (meth) acryloyl group.
- polyisocyanate compounds used to form urethane (meth) acrylates include tolylene diisocyanate, xylylene diisocyanate, diphenylmethane diisocyanate, hexamethylene diisocyanate, trimethylhexamethylene diisocyanate, tetramethylxylylene diisocyanate, isophorone diisocyanate ( IPDI), hydrogenated tolylene diisocyanate, hydrogenated xylylene diisocyanate, hydrogenated diphenylmethane diisocyanate, m-phenylene diisocyanate, biphenylene diisocyanate, tetramethylene diisocyanate, hexamethylene diisocyanate, and their dimers or 3 A monomer is mentioned.
- IPDI isophorone diisocyanate
- dimer examples include dihexamethylene diisocyanate addition condensate (hexamethylene diisocyanate dimer) and trimethylhexamethylene diisocyanate addition condensate (trimethylhexamethylene diisocyanate dimer or trimer).
- polyisocyanate compound IPDI and / or dihexamethylene diisocyanate addition condensate can be selected.
- hydroxyl group-containing (meth) acrylate used to form urethane (meth) acrylate include 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, and 4-hydroxybutyl (meth).
- Hydroxyalkyl (meth) acrylates such as acrylate, pentaerythritol tri (meth) acrylate, trimethylolpropane di (meth) acrylate, and dipentaerythritol penta (meth) acrylate; isocyanuric acid di (meth) acrylic acid esters and their ethylene oxides And caprolactone-modified products.
- a polyisocyanate compound pentaerythritol tri (meth) acrylate, dipentaerythritol penta (meth) acrylate, and trimethylolpropane di (meth) acrylate because it provides excellent cured film properties.
- Urethane (meth) acrylate obtained by reaction with one kind of hydroxyl group-containing (meth) acrylate can be used.
- Isophorone diisocyanate can also be selected as the polyisocyanate compound.
- the curable composition may contain urethane (meth) acrylate in a ratio of 0.5 parts by mass or more and 15 parts by mass or less, 1 part by mass or more and 10 parts by mass or less, or 1 part by mass or more and 5 parts by mass or less. .
- the amount of urethane (meth) acrylate is within this range, the scratch resistance can be further improved while maintaining excellent flexibility.
- the amount of urethane (meth) acrylate is more than 15 parts by mass, the flexibility tends to be relatively lowered.
- the curable composition may contain a photopolymerization initiator for the purpose of curing the coating film.
- the photopolymerization initiator is not particularly limited as long as it is a compound that can be decomposed by light irradiation to generate radicals to initiate polymerization.
- Specific examples of the photopolymerization initiator include acetophenone, acetophenone benzyl ketal, 1-hydroxycyclohexyl phenyl ketone, 2,2-dimethoxy-1,2-diphenylethane-1-one, xanthone, fluorenone, benzaldehyde, fluorene, anthraquinone, Triphenylamine, carbazole, 3-methylacetophenone, 4-chlorobenzophenone, 4,4'-dimethoxybenzophenone, 4,4'-diaminobenzophenone, benzoin propyl ether, benzoin ethyl ether, benzyldimethyl ketal, 1- (4-isopropyl Phenyl) -2-hydroxy-2-methylpropan-1-one, 2-
- the curable composition may contain a photopolymerization initiator in a ratio of 0.01 parts by mass or more and 10 parts by mass or less, 0.1 part by mass or more and 6 parts by mass or less, or 1 part by mass or more and 5 parts by mass or less. Good. Particularly good photopolymerizability can be obtained when the amount of the photopolymerizable compound is within this range.
- the curable composition may contain fine particles for the purpose of adjusting optical properties such as refractive index or increasing anti-blocking properties.
- the average particle diameter of the fine particles may be 1 to 1000 nm, or 5 to 200 nm. When the average particle diameter of the fine particles is within this range, light scattering can be prevented, and good transparency and antiblocking properties can be obtained.
- the average particle diameter can be measured by a laser diffraction / scattering method.
- the refractive index of the fine particles is not particularly limited, but may be 1.40 to 1.70, 1.40 to 1.60, or 1.40 to 1.50.
- the difference in refractive index between the fine particles and a portion (matrix resin) other than the fine particles in the cured film may be 0.05 or less, 0.02 or less, or 0.01 or less.
- the fine particles are not particularly limited, but silicon dioxide particles, tin oxide particles, calcium carbonate particles, zirconium oxide particles, talc, kaolin, barium sulfate particles, titanium dioxide particles, aluminum oxide particles, zinc oxide particles, pentoxide.
- Inorganic fine particles such as antimony particles, indium oxide / tin oxide particles, antimony oxide / tin oxide particles, indium oxide particles, antimony oxide particles, magnesium fluoride particles, zeolite particles, synthetic mica particles, smectite particles and calcium sulfate particles. It is done.
- the fine particles include organic polymer particles such as (meth) acrylic particles, styrene-acrylic copolymer particles, polystyrene particles, polyester particles, urethane particles, and silicone particles, and organic-inorganic hybrid particles.
- the fine particles may be surface-treated. Since the surface hardness of the cured film can be increased, the strength can be particularly increased, and a desired refractive index can be obtained, the fine particles may be inorganic fine particles, particularly silicon dioxide particles. There may be only one kind of fine particles, or two or more kinds.
- the amount of fine particles in the curable composition (the total amount when two or more types of fine particles are included) is 0.1 parts by mass or more and 60 parts by mass or less, with the mass of the curable composition being 100 parts by mass, or 1 mass part or more and 50 mass parts or less may be sufficient. When the amount of fine particles is within these ranges, good transparency and antiblocking properties can be obtained.
- the curable composition may further contain a solvent that dissolves or disperses each component for the purpose of adjusting viscosity, coating property, and thickness of the coating film.
- the solvent include ketones such as acetone, methyl ethyl ketone, methyl isobutyl ketone, cyclopentanone and cyclohexanone; esters such as ethyl acetate and butyl acetate; alcohols such as isopropyl alcohol and ethyl alcohol; benzene, toluene and xylene , Aromatic hydrocarbons such as methoxybenzene and 1,2-dimethoxybenzene; phenols such as phenol and parachlorophenol; halogenated hydrocarbons such as chloroform, dichloromethane, dichloroethane, tetrachloroethane, trichloroethylene, tetrachloroethylene and chlorobenzene Is mentioned. These solvents may be used alone or in combination of two or more.
- the curable composition may contain other components without departing from the spirit of the present invention.
- the curable composition may contain an antifouling agent, a flame retardant, an antioxidant, a dispersant, an ultraviolet absorber, a pigment, a plasticizer, a surfactant, a thixotropic agent, and the like. These additives may be used alone or in combination of two or more.
- FIG. 2 is a cross-sectional view showing an embodiment of a liquid crystal display device.
- the liquid crystal display device 20 shown in FIG. 2 includes a liquid crystal cell 5, a polarizer 7 provided on the viewing side of the liquid crystal cell 5, and a laminated film 1 provided on the viewing side of the polarizer 7.
- the laminated film 1 the laminated film according to the above-described embodiment can be used.
- An arbitrary polarizing plate protective film may be provided between the polarizer 7 and the laminated film 1.
- the polarizer is not particularly limited, and may be, for example, a film obtained by stretching a polyvinyl alcohol film doped with iodine.
- a polarizing plate protective film an optically isotropic isotropic film may be used, or a retardation film having a desired retardation may be used.
- the liquid crystal display device of this embodiment is better than a conventional liquid crystal display device including a polarizing plate protective film made of a material such as triacetyl cellulose. It can have heat resistance and moisture resistance.
- the laminated film 1 can be bonded without using an aqueous adhesive at the time of bonding. By not using a water-based adhesive, it is possible to suppress deterioration in quality in a durability test under high temperature and high humidity.
- the base film 10 includes an ultraviolet absorber
- components such as a liquid crystal cell and a polarizer are obtained from ultraviolet rays that are exposed when a liquid crystal display device is manufactured and ultraviolet rays that are exposed when the liquid crystal display device is used. Can be protected.
- the liquid crystal cell may be a cell of an arbitrary system such as a TN system, a VA system, and an IPS system.
- the display color of the liquid crystal display hardly changes when the viewing angle changes.
- an in-cell type liquid crystal cell may be used to reduce the thickness of the entire liquid crystal display device.
- the laminated film is usually provided in such a direction that the cured film and the base film are arranged in this order from the liquid crystal cell side. You may provide glass further through the adhesive agent etc. on the opposite side to the base film of a cured film.
- the laminated film is arranged so that the slow axis of the base film of the laminated film forms a predetermined angle ⁇ with respect to the transmission axis of the polarizer. Is preferred. Specifically, the angle ⁇ may be 40 ° or more, or 43 ° or more, and may be 50 ° or less, or 48 ° or less. The angle ⁇ may be within a range of 45 ° ⁇ 1 °.
- the polarized light passing through the liquid crystal cell and the polarizer and traveling through the laminated film is circularly polarized or Can be converted to elliptically polarized light.
- the display content of a liquid crystal display device can also be visually recognized through polarized sunglasses.
- the sliding test was performed using a sliding test apparatus manufactured by HEIDON. Two laminated films were attached to the sample attachment portion of the sliding portion of the sliding test apparatus so that the cured films overlapped with each other. While applying a vertical load of 50 gf or 200 gf to the attached laminated film, it was confirmed whether or not one laminated film slipped when the sliding portion was moved in the horizontal direction. When the laminated film slipped at a load of 200 gf, the laminated film was considered to have slipperiness with respect to a load of 200 gf or more. When the laminated film did not slip at a load of 50 gf, it was considered that the load having the slipperiness of the laminated film was less than 50 gf.
- the laminated film had slipperiness with respect to a load of 200 gf or more, the slipperiness was considered sufficient.
- the score for comprehensive evaluation was set as follows. 2 points: The laminated film slides at a load of 200 gf. 1 point: The laminated film does not slip at a load of 50 gf.
- Pencil hardness of cured film The pencil hardness of the cured film was measured in accordance with the scratch hardness (pencil method) of JIS K5600-5-4.
- the weight average molecular weight of the polymer acrylate is a value obtained by conversion using a standard polystyrene calibration curve measured by a gel permeation chromatography (GPC) method.
- the measurement conditions of the GPC method are as follows. The weight average molecular weight of the polymer acrylate in the following synthesis examples was measured under the same conditions.
- silica particle sol fine particles 1 (as the amount of silica particles), 0.5 parts by mass of a leveling agent (UV-3500 manufactured by BYK), and photopolymerization start 4 parts by mass of an agent (Irgacure 184, manufactured by BASF) was stirred and mixed in MIBK using a stirrer to prepare a curable composition for coating.
- silica particle sol methyl ethyl ketone silica sol (MEK-ST-L manufactured by Nissan Chemical Industries, Ltd., number average particle size 0.056 ⁇ m, silica particle concentration 30 mass%, spherical) was used.
- This curable composition was used for the production of a laminated film.
- Example 4 Production and evaluation of laminated film (Example 1) A cyclic olefin resin film (manufactured by Nippon Zeon Co., Ltd., trade name ZeonorFilm ZF16, glass transition temperature: 163 ° C.) was prepared as a base film. On one side of this base film, the curable composition was applied with a thickness of 2.5 ⁇ m using a bar coater. The coating was dried by heating in a dryer for 1 minute. The dried coating film was irradiated with ultraviolet rays having a light amount of 400 mJ / cm 2 using a conveyor type high-pressure mercury lamp. A cured film of the curable composition was formed by ultraviolet irradiation to obtain a laminated film. During the ultraviolet irradiation, nitrogen was introduced to reduce the oxygen concentration to 10 ppm or less.
- Example 2 A cyclic olefin resin film having a thickness of 100 ⁇ m (manufactured by Nippon Zeon Co., Ltd., trade name ZeonorFilm ZF14, glass transition temperature: 136 ° C.) was prepared as a base film. A laminated film having a cured film was produced by the same procedure as in Example 1 except that this base film was used.
- Example 3 A pellet of cyclic olefin resin A1 (manufactured by Nippon Zeon Co., Ltd., “ZEONOR1600”, glass transition temperature: 163 ° C.) was dried at 100 ° C. for 4 hours using a hot air dryer in which air was circulated. The dried pellets were fed into an extruder and melted in the extruder. The molten resin was passed through a polymer pipe and a polymer filter, extruded from a T-die onto a casting drum in a sheet form, and cooled to obtain a base film having a thickness of 35 ⁇ m. A laminated film having a cured film was produced by the same procedure as in Example 1 except that this base film was used.
- Example 4 Norbornene and ethylene copolymer, cyclic olefin resin A2 having a copolymerization ratio of norbornene and ethylene of 82:18 (glass transition temperature: 170 ° C., melt volume rate (MVR): 1.5, trade name) “TOPAS” and TOPAS Advanced Polymers) were prepared. This resin was molded by a melt extrusion method at a resin temperature of 300 ° C. and a take-up roll temperature of 130 ° C. to obtain a cyclic olefin resin film having a thickness of 100 ⁇ m. A laminated film having a cured film was produced by the same procedure as in Example 1 except that this cyclic olefin resin film was used as a base film.
- Example 5 A cyclic olefin resin film (manufactured by Nippon Zeon Co., Ltd., trade name ZeonorFilm ZF16, glass transition temperature: 163 ° C.) was prepared as a base film. Using this base film, a laminated film having a cured film was produced by the same procedure as in Example 1 except that the thickness of the film of the curable composition after coating was 1.5 ⁇ m.
- Example 6 30 parts by mass of zirconium sol particles (fine particles 2) (manufactured by Nissan Chemical Industries, Ltd., OZ-S30K, average particle diameter 10 nm) with respect to 100 parts by mass of the curable composition prepared in “3. Preparation of curable composition” was further added.
- a laminated film having a cured film was produced by the same procedure as in Example 1 except that the curable composition after addition was used.
- Example 7 A laminated film having a cured film was produced by the same procedure as in Example 6 except that the amount of the zirconium sol particles (fine particles 2) was changed to 25 parts by mass.
- Example 8 The pellets of cyclic olefin resin A3 (manufactured by Nippon Zeon Co., Ltd., “ZEONOR”, glass transition temperature: 126 ° C.) were dried at 100 ° C. for 4 hours using a hot air dryer in which air was circulated. The dried pellets were fed into an extruder and melted in the extruder. The molten resin was passed through a polymer pipe and a polymer filter, extruded from a T-die onto a casting drum in a sheet form, and cooled to obtain a film (A) before stretching having a thickness of 70 ⁇ m.
- the obtained film before stretching (A) was supplied to a tenter stretching machine, and the film before stretching (A) was obliquely stretched by a tenter stretching machine to obtain a quarter wavelength plate.
- the stretching conditions for the oblique stretching were a stretching ratio of 2.36 times and a stretching temperature of 144 ° C.
- the in-plane retardation value Re of the obtained quarter-wave plate was 130 nm, the thickness was 47 ⁇ m, and the direction of the slow axis was 45 ° with respect to the width direction.
- a laminated film having a cured film was produced by the same procedure as in Example 1 except that this quarter-wave plate was used as the base film.
- Example 9 100 parts by mass of cyclic olefin resin A3 (manufactured by Nippon Zeon Co., Ltd., “ZEONOR”, glass transition temperature: 126 ° C.) and 5.5 parts by mass of benzotriazole-based ultraviolet absorber (ADEKA “LA-31”) And mixed by a twin screw extruder. Next, the mixture was put into a hopper connected to an extruder, supplied to a single screw extruder, melt extruded, and a cyclic olefin resin composition J1 containing an ultraviolet absorber was obtained. The amount of the ultraviolet absorber in the cyclic olefin resin composition J1 was 5.2 parts by mass, and the glass transition temperature was 118 ° C.
- the cyclic olefin resin composition J1 was charged into a hopper charged in the single screw extruder.
- the cyclic olefin resin composition J1 was melted, and the molten cyclic olefin resin composition J1 was supplied to the multi-manifold die at an exit temperature of the extruder of 280 ° C. and a rotation speed of the extruder gear pump of 10 rpm.
- the arithmetic surface roughness Ra of the die slip of this multi-manifold die was 0.1 ⁇ m.
- the cyclic olefin resin A3 used for the production of the cyclic olefin resin composition J1 was charged into a hopper charged in the single screw extruder.
- the cyclic olefin resin A3 was melted, and the molten cyclic olefin resin A3 was supplied to the multi-manifold die at an exit temperature of the extruder of 285 ° C. and a rotation speed of the extruder gear pump of 4 rpm.
- a molten cyclic olefin resin A3, a molten cyclic olefin resin composition J1 containing an ultraviolet absorber, and a molten cyclic olefin resin A3 are each discharged from a multi-manifold die at 280 ° C., and the temperature is adjusted to 150 ° C.
- the film was cast on a cooled roll to obtain a film (B) before stretching.
- the air gap amount was set to 50 mm.
- Edge pinning was adopted as a method of casting the discharged resin onto a cooling roll.
- the film before stretching (B) is a 15 ⁇ m thick resin layer made of cyclic olefin resin A3, a 40 ⁇ m thick resin layer made of cyclic olefin resin composition J1 containing an ultraviolet absorber, and a 15 ⁇ m thick cyclic olefin resin A3. It was a multilayer film having a three-layer structure provided with resin layers in this order. The total thickness of the unstretched film (B) was 70 ⁇ m.
- the unstretched film (B) was supplied to a tenter stretching machine, and the unstretched film (B) was obliquely stretched at a stretching ratio of 1.5 times and a stretching temperature of 140 ° C. with a tenter stretching machine to obtain a stretched film.
- the obtained stretched film has a first surface layer of 8 ⁇ m thickness made of cyclic olefin resin A3, an intermediate layer of 31 ⁇ m thickness made of cyclic olefin resin composition J1 containing an ultraviolet absorber, and a thickness of 8 ⁇ m made of cyclic olefin resin A3.
- a multilayer film having a total thickness of 47 ⁇ m and having a second surface layer in this order.
- the in-plane retardation value Re of the multilayer film was 100 nm, and the light transmittance of the multilayer film at a measurement wavelength of 380 nm was 0.02%.
- a laminated film having a cured film was produced by the same procedure as in Example 1 except that the obtained multilayer film was used as a base film.
- Example 10 A polarizer (“HLC2-5618S” manufactured by Sanlitz) was prepared. One side of this polarizer and the surface on the base film side of the laminated film prepared in Example 8 were bonded together via an ultraviolet curable acrylic adhesive to produce a polarizing plate. The laminated film was bonded to the polarizer so that the slow axis of the base film was at an angle of 45 ° with respect to the transmission axis of the polarizer.
- a commercially available mobile phone (NTT Docomo F-09A) equipped with an IPS liquid crystal panel was disassembled, and the polarizing plate on the viewing side was removed. Instead of the removed polarizing plate on the viewing side, the produced polarizing plate was arranged so that the cured film of the laminated film was on the viewing side, and a liquid crystal display device was assembled.
- the image display surface of the obtained liquid crystal display device is displayed in white and the white display is observed through polarized sunglasses, even if the viewing direction is tilted from about 45 to 90 °, the visibility of the image changes. There was no. Even when the outermost cured film was scratched with a pencil having a hardness of HB, no visual scratch was observed.
- ZNR means a polymer film of a norbornene derivative
- TOPAS means a film of a copolymer of norbornene and ethylene.
- cyclic olefin resin film used in Example 4 is shown.
- the laminated film of the present invention has excellent scratch resistance and flexibility while having a cyclic olefin resin film as a base film, and the base film and the cured film are It was confirmed that the adhesion was also good.
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Abstract
Description
基材フィルムは、環状オレフィン樹脂を含むフィルムである。具体的には、環状オレフィン樹脂を含むフィルムは、環状オレフィン樹脂と、必要により含まれる添加剤等とを含む環状オレフィン樹脂組成物の成形体である。図1に示されるように、基材フィルム10が、中間層15と、中間層15の一方の主面側に積層された第一表面層11と、中間層15の他方の主面側に設けられた第二表面層12とを有する多層フィルムであり、これら各層がそれぞれ環状オレフィン樹脂を含んでいてもよい。
硬化膜は、JISK5600-5-4(1999)で規定される鉛筆硬度試験において「B」以上の硬度を示すものであり得る。
本実施形態に係る積層フィルムは、例えば、基材フィルム上に硬化性組成物の膜を形成させる工程と、硬化性組成物の膜を硬化することにより硬化膜を形成させる工程とを含む方法により、得ることができる。
重合性二重結合を有するアクリル樹脂は、例えば、(メタ)アクリル酸エステルをモノマー単位として含む共重合体からなる主鎖と、主鎖に結合し、重合性二重結合を含む側鎖とを有していてもよい。重合性二重結合を含む側鎖は、典型的には(メタ)アクリロイル基を含むが、これに限られない。
(B)成分として用いられる多官能重合性化合物は、3個以上の重合性二重結合を有する。重合性二重結合を含む基は、典型的には(メタ)アクリロイル基であるが、これに限られない。多官能重合性化合物は、重合性二重結合を含む基として、下記一般式(2-1)又は(2-2)で表される一価の基を1個、2個又は3個以上有していてもよい。重合性二重結合を含む基として式(2-1)又は(2-2)の基を導入したことにより、形成される硬化膜の高い強度を維持しつつ、硬化膜が変形したときの応力を緩和することができる。その結果、硬化膜の優れた屈曲性が得られる。多官能重合性化合物が3個以上の重合性二重結合を有していることにより、硬化膜の耐擦傷性が向上する。多官能重合性化合物中の重合性二重結合の数は、6個以上9個以下であってもよい。多官能重合性化合物中の重合性二重結合の全てが式(2-1)又は(2-2)の基中に含まれていてもよいし、多官能重合性化合物が式(2-1)又は(2-2)の基以外に、重合性二重結合を含む基を有していてもよい。
アルキレンオキシド変性ビスフェノールAジ(メタ)アクリレートは、下記一般式(3)で表される、オキシアルキレン基を含む構造を有する。
硬化性組成物は、(A)重合性二重結合を有するアクリル樹脂を、8質量部以上40質量部以下、10質量部以上25質量部以下、又は12質量部以上20質量部以下の比率で含んでいてもよい。アクリル樹脂の量がこの範囲であると擦傷性と屈曲性が更に高いレベルで両立できる。アクリル樹脂の量が8質量部未満の場合であると屈曲性が相対的に低下する傾向がある。アクリル樹脂の量が40質量部より多いと耐擦傷性が相対的に低下する傾向がある。
硬化性組成物は、1個又は2個以上のウレタン基と、2個以上の(メタ)アクリロイル基とを有するウレタン(メタ)アクリレートを含んでいてもよい。ウレタン(メタ)アクリレートは、硬化膜の耐擦傷性のより一層の向上に寄与することができる。
硬化性組成物は、塗膜を硬化させるなどの目的のために、光重合開始剤を含んでもよい。
硬化性組成物は、屈折率などの光学特性の調節、又はアンチブロッキング性を高めるなどの目的のために、微粒子を含んでもよい。
硬化性組成物は、粘度、塗工性、及び塗膜の厚さ調整等の目的のために、各成分を溶解又は分散する溶剤を更に含んでいてもよい。
硬化性組成物は、本発明の趣旨を逸脱しない範囲で、その他の成分を含んでいてもよい。
図2は、液晶表示装置の一実施形態を示す断面図である。図2に示す液晶表示装置20は、液晶セル5と、液晶セル5の視認側に設けられた偏光子7と、偏光子7の視認側に設けられた積層フィルム1とを備える。積層フィルム1として、上述の実施形態に係る積層フィルムを用いることができる。偏光子7と積層フィルム1との間に任意の偏光板保護フィルムが設けられていてもよい。
(1)二重結合当量
高分子アクリルアクリレート(アクリル樹脂)の二重結合当量は、合成に用いたアクリル酸のモル数を高分子アクリルアクリレート中の重合性二重結合の数とみなして、式:二重結合当量=(合成に用いたモノマーの総質量部)/(合成に用いたアクリル酸のモル数)によって算出した。この式により算出される二重結合当量は、合成された高分子アクリルアクリレートの二重結合当量の平均値に相当するとみなすことができる。
(B)~(D)成分については、下記式に基づいて二重結合当量を算出した。
二重結合当量=重量平均分子量(メーカー報告値)/同一分子中の重合性二重結合の数
新東科学社製表面性測定機を用い、荷重をかけたスチールウール#0000を、積層フィルムの硬化膜に対して押し付けながら、速度2000mm/分で10回往復させることで、硬化膜の表面を擦った。スチールウールに加えた荷重を段階的に大きくしていき、硬化膜表面に傷が入らないときの最大荷重を求めた。この最大荷重が150gf以上であれば耐擦傷性が十分であるとした。
硬化膜を上にした状態で、積層フィルムの異なる任意の7個所を山折りにしたときに、積層フィルムが割れた個所の数を求めた。積層フィルムが割れた個所の数が0であれば、屈曲性が十分であるとした。総合評価のための点数を以下のとおり設定した。
5点:割れた個所の数が0
3点:割れた個所の数が1~3
1点:割れた個所の数が4以上
JIS K5400における碁盤目セロハンテープ剥離試験に準拠し、1mm角、計100個の碁盤目における残存率(%)に基づいて、基材フィルムと硬化膜との密着性を評価した。残存率が90%以上であれば、密着性が十分であるとした。総合評価のための点数を以下のとおり設定した。
3点:残存率が90%以上~100%以下
2点:残存率が50%以上~90%未満
1点:残存率が0%以上~50%未満
滑り性試験は、HEIDON社製の摺動試験装置を用いて行った。摺動試験装置の摺動部の試料取り付け部に、2枚の積層フィルムを、それぞれの硬化膜同士が重なるように取り付けた。取り付けられた積層フィルムに50gf又は200gfの垂直荷重を加えながら、摺動部を水平方向に移動させたときに、一方の積層フィルムが滑るか否かを確認した。荷重200gfで積層フィルムが滑った場合、積層フィルムが200gf以上の荷重に対して滑り性を有するとみなした。荷重50gfで積層フィルムが滑らなかった場合、積層フィルムが滑り性を有する荷重が50gf未満であるとみなした。積層フィルムが200gf以上の荷重に対して滑り性を有していれば、滑り性が十分であるとした。総合評価のための点数を以下のとおり設定した。
2点:荷重200gfで積層フィルムが滑る。
1点:荷重50gfで積層フィルムが滑らない。
(2)~(5)の評価結果の合計点に基づいて、以下の基準で積層フィルムを総合評価した。
良:合計点が11点~12点
可:合計点が9点~10点
不可:合計点が8点以下
原子間力顕微鏡(Digital Instruments社製 NanoScopeIIIa)を用いて、硬化膜の表面の算術平均粗さ(Ra)を測定した。
JIS K5600-5-4の引っ掻き硬度(鉛筆法)に準拠して、硬化膜の鉛筆硬度を測定した。
(A)重合性二重結合を有するアクリル樹脂(高分子アクレート)の合成
グリシジルメタクリレート(GMA)80質量部、メチルメタクリレート(MMA)18質量部、及びエチルアクリレート(EA)2質量部を、メチルイソブチルケトン(MIBK)中で常法に従って溶液重合させて、グリシジルメタクリレートに由来するエポキシ基を有するアクリル樹脂を合成した。得られたアクリル樹脂のエポキシ基とアクリル酸との反応により、アクリロイルオキシ基を有するアクリル樹脂(高分子アクリレート)を得た。重合反応に用いたGMA1当量に対して、1当量のアクリル酸を反応に用いた。得られた高分子アクリルアクリレートの重量平均分子量は15000であり、二重結合当量は256であった。
装置:東ソー製 HLC-8320GPC(RI検出器内蔵)
検出器:RI(示差屈折計)
溶媒:純正1級THF(テトラヒドロフラン)
ガードカラム:TSK-guardcolumn SuperMP(HZ)-H(1本)
ガードカラムサイズ:4.6mm(ID)×20mm
カラム:東ソー製 TSK-GEL SuperMulitipore HZ-H(3本連結)
カラムサイズ:4.6mm(ID)×150mm
温度:40℃
試料濃度:0.01g/5mL
注入量:10μL
流量:0.35mL/min
(A)成分として上記高分子アクリレートを用いた。(B)、(C)及び(D)成分として以下を準備した。
(B)多官能重合性化合物
B1:カプロラクトン変性ジペンタエリスリトールヘキサアクリレート(二重結合当量:135、日本化薬株式会社製、KAYARAD DPCA-20、カプロラクトン2モル付加(式(2-2)におけるnが一分子中の合計で平均2)、六官能)
B2:エチレンオキシド変性ポリグリセリンポリアクリレート(二重結合当量:244、新中村化学工業株式会社製、NKエコノマー A-PG5027E、エチレンオキシド27モル付加(式(2-1)におけるeが一分子中の合計で平均27)、九官能)
(C)アルキレンオキシド変性ビスフェノールAジアクリレート
EO変性ビスフェノールAジアクリレート(日立化成株式会社製 ファンクリル FA-323A、式(3)におけるR1が水素原子、fが2、g+hが30である化合物)
(D)ウレタンアクリレート
10官能ウレタンアクリレート(二重結合当量:116、日立化成株式会社製 ヒタロイド HA7909-1)
固形分(溶剤以外の成分)の比率として、(A)成分20質量部、(B)成分のB1を20質量部、(B)成分のB2を52質量部、(C)成分15質量部、(D)成分3質量部、及び溶媒としてのメチルイソブチルケトン(MIBK)150質量部とを混合し、40℃で1時間攪拌して、硬化性成分の溶液を得た。
この硬化性成分の溶液100質量部と、シリカ粒子ゾル(微粒子1)40質量部(シリカ粒子の量として)と、レベリング剤(BYK社製UV-3500)0.5質量部と、光重合開始剤(イルガキュア184、BASF社製)4質量部とをMIBK中で攪拌機を用いて攪拌混合して、塗工用の硬化性組成物を調製した。シリカ粒子ゾルとして、メチルエチルケトンシリカゾル(日産化学工業(株)製MEK-ST-L、数平均粒子径0.056μm、シリカ粒子濃度30質量%、球状)を用いた。この硬化性組成物を積層フィルムの作製のために用いた。
(実施例1)
基材フィルムとして、厚み100μmの環状オレフィン樹脂フィルム(日本ゼオン社製、商品名ZeonorFilm ZF16、ガラス転移温度:163℃)を準備した。この基材フィルムの片面上に、上記硬化性組成物をバーコーターを用いて2.5μmの厚みで塗工した。塗膜を乾燥機中で1分間加熱することにより乾燥した。乾燥後の塗膜にコンベア式高圧水銀ランプを用いて400mJ/cm2の光量の紫外線を照射した。紫外線照射により、硬化性組成物の硬化膜を形成させ、積層フィルムを得た。紫外線照射の際、窒素を導入して酸素濃度を10ppm以下とした。
基材フィルムとして、厚み100μmの環状オレフィン樹脂フィルム(日本ゼオン社製、商品名ZeonorFilm ZF14、ガラス転移温度:136℃)を準備した。この基材フィルムを用いたこと以外は実施例1と同様の手順により、硬化膜を有する積層フィルムを作製した。
環状オレフィン樹脂A1(日本ゼオン社製、「ZEONOR1600」、ガラス転移温度:163℃)のペレットを、空気を流通させた熱風乾燥機を用いて100℃で、4時間乾燥した。乾燥させたペレットを押出機に供給し、押出機内で溶融させた。溶融した樹脂をポリマーパイプおよびポリマーフィルターを通し、Tダイからキャスティングドラム上にシート状に押出し、冷却して、厚みが35μmの基材フィルムを得た。この基材フィルムを用いたこと以外は実施例1と同様の手順により、硬化膜を有する積層フィルムを作製した。
ノルボルネン及びエチレンの共重合体であって、ノルボルネンとエチレンとの共重合比率が82:18である環状オレフィン樹脂A2(ガラス転移温度:170℃、メルトボリュームレイト(MVR):1.5、商品名「TOPAS」、TOPAS Advanced Polymers社製)を準備した。この樹脂を溶融押出法にて樹脂温度300℃、引取りロール温度130℃で成形し、厚み100μmの環状オレフィン樹脂フィルム得た。この環状オレフィン樹脂フィルムを基材フィルムとして用いたこと以外は実施例1と同様の手順により、硬化膜を有する積層フィルムを作製した。
基材フィルムとして、厚み100μmの環状オレフィン樹脂フィルム(日本ゼオン社製、商品名ZeonorFilm ZF16、ガラス転移温度:163℃)を準備した。この基材フィルムを用い、塗工後の硬化性組成物の膜の厚みを1.5μmとしたこと以外は実施例1と同様の手順により、硬化膜を有する積層フィルムを作製した。
「3.硬化性組成物の調製」において調製した硬化性組成物100質量部に対して、ジルコニウムゾル粒子(微粒子2)(日産化学工業社製、OZ-S30K、平均粒子径10nm)30質量部をさらに添加した。添加後の硬化性組成物を使用した以外は実施例1と同様の手順により、硬化膜を有する積層フィルムを作製した。
ジルコニウムゾル粒子(微粒子2)の量を25質量部に変更したこと以外は実施例6と同様の手順により、硬化膜を有する積層フィルムを作製した。
環状オレフィン樹脂A3(日本ゼオン社製、「ZEONOR」、ガラス転移温度:126℃)のペレットを、空気を流通させた熱風乾燥機を用いて、100℃で4時間乾燥した。乾燥させたペレットを押出機に供給し、押出機内で溶融させた。溶融した樹脂をポリマーパイプおよびポリマーフィルターを通し、Tダイからキャスティングドラム上にシート状に押出し、冷却して、厚み70μmの延伸前フィルム(A)を得た。得られた延伸前フィルム(A)をテンター延伸機に供給し、テンター延伸機により、延伸前フィルム(A)に斜め延伸を施して1/4波長板を得た。斜め延伸の延伸条件は、延伸倍率2.36倍、延伸温度144℃であった。得られた1/4波長板の面内のレターデーション値Reは130nm、厚みは47μm、遅相軸の方向はその幅方向に対して45°であった。
基材フィルムとして、この1/4波長板を使用した以外は実施例1と同様の手順により、硬化膜を有する積層フィルムを作製した。
環状オレフィン樹脂A3(日本ゼオン社製、「ZEONOR」、ガラス転移温度:126℃)100質量部、及び、ベンゾトリアゾール系の紫外線吸収剤(ADEKA社製「LA-31」)5.5質量部を、二軸押出機により混合した。次いで、その混合物を、押出機に接続されたホッパーへ投入し、単軸押出機へ供給し溶融押出して、紫外線吸収剤を含む環状オレフィン樹脂組成物J1を得た。この環状オレフィン樹脂組成物J1における紫外線吸収剤の量は5.2質量部で、ガラス転移温度は118℃であった。
得られた多層フィルムを基材フィルムとして使用したこと以外は実施例1と同様の手順により、硬化膜を有する積層フィルムを作製した。
偏光子(「HLC2-5618S」サンリッツ社製)を用意した。この偏光子の片面と、実施例8で作成した積層フィルムの基材フィルム側の面とを、紫外線硬化型のアクリル接着剤を介して貼り合せて、偏光板を作製した。基材フィルムの遅相軸が偏光子の透過軸に対して45°の角度をなすように、積層フィルムを偏光子に貼り合せた。
Claims (17)
- 基材フィルムと、該基材フィルムの片面又は両面上に設けられ、硬化した硬化性組成物である硬化膜と、を備える積層フィルムであって、
前記基材フィルムが環状オレフィン樹脂を含むフィルムであり、
前記硬化性組成物が、
(A)重合性二重結合を有するアクリル樹脂、
(B)3個以上の重合性二重結合を有し、該重合性二重結合を含む基として下記一般式(2-1)又は(2-2)で表される一価の基を1個以上有する多官能重合性化合物、及び
(C)下記一般式(3)で表されるアルキレンオキシド変性ビスフェノールAジ(メタ)アクリレートを含み、
二重結合当量が、式:二重結合当量=分子量/同一分子中の重合性二重結合の数、によって定義されるときに、前記多官能重合性化合物の二重結合当量が130以上500以下であり、
前記多官能重合性化合物が、前記アクリル樹脂とは異なる化合物である、
積層フィルム。 - 前記アクリル樹脂の二重結合当量が220以上2500以下である、請求項1に記載の積層フィルム。
- 前記アクリル樹脂の重量平均分子量が5000以上200000以下である、請求項1又は2に記載の積層フィルム。
- 前記多官能重合性化合物の二重結合当量が130以上300以下である、請求項1~3のいずれか一項に記載の積層フィルム。
- 式(3)におけるfが2である、請求項1~4のいずれか一項に記載の積層フィルム。
- 前記硬化性組成物が(D)ウレタン基及び2個以上の(メタ)アクリロイル基を有するウレタン(メタ)アクリレートを更に含む、請求項1~5のいずれか一項に記載の積層フィルム。
- 前記硬化性組成物が、
前記アクリル樹脂を8質量部以上40質量部以下、
前記多官能重合性化合物を40質量部以上80質量部以下、
前記アルキレンオキシド変性ビスフェノールAジ(メタ)アクリレートを4質量部以上40質量部以下の比率で含む、
請求項1~5のいずれか一項に記載の積層フィルム。 - 前記硬化性組成物が、(D)ウレタン基及び2個以上の(メタ)アクリロイル基を有するウレタン(メタ)アクリレートを、0.5質量部以上15質量部以下の比率で含む、請求項7に記載の積層フィルム。
- 前記硬化性組成物が(E)光重合開始剤を更に含む、請求項1~8のいずれか一項に記載の積層フィルム。
- 前記硬化性組成物が(F)微粒子を更に含む、請求項1~9のいずれか一項に記載の積層フィルム。
- 前記環状オレフィン樹脂のガラス転移温度が100℃以上180℃以下である、請求項1~10のいずれか一項に記載の積層フィルム。
- 前記基材フィルムが延伸フィルムである、請求項1~11のいずれか一項に記載の積層フィルム。
- 前記延伸フィルムが斜め延伸フィルムである、請求項12に記載の積層フィルム。
- 前記基材フィルムが多層フィルムである、請求項1~13のいずれか一項に記載の積層フィルム。
- 前記多層フィルムが第一表面層、中間層及び第二表面層を備え、前記第一表面層、前記中間層及び前記第二表面層がこの順に積層されており、前記中間層が紫外線吸収剤を含み、前記多層フィルムの厚みが10μm以上100μm以下である、請求項14に記載の積層フィルム。
- 液晶セルと、
偏光子と、
請求項1~15のいずれか一項に記載の積層フィルムと、
を備え、
前記液晶セルの視認側に前記偏光子及び前記積層フィルムがこの順に積層され、
前記積層フィルムが、前記基材フィルム及び前記硬化膜が前記液晶セル側からこの順に配置される向きで積層されている、
液晶表示装置。 - 前記液晶セルが、IPS方式の液晶セルである、請求項16に記載の液晶表示装置。
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