WO2015099078A1 - 積層フィルム、及び、複合フィルムの製造方法 - Google Patents
積層フィルム、及び、複合フィルムの製造方法 Download PDFInfo
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- WO2015099078A1 WO2015099078A1 PCT/JP2014/084388 JP2014084388W WO2015099078A1 WO 2015099078 A1 WO2015099078 A1 WO 2015099078A1 JP 2014084388 W JP2014084388 W JP 2014084388W WO 2015099078 A1 WO2015099078 A1 WO 2015099078A1
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- YVTHLONGBIQYBO-UHFFFAOYSA-N zinc indium(3+) oxygen(2-) Chemical compound [O--].[Zn++].[In+3] YVTHLONGBIQYBO-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/02—Details
- H05B33/04—Sealing arrangements, e.g. against humidity
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/10—Apparatus or processes specially adapted to the manufacture of electroluminescent light sources
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- H—ELECTRICITY
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Definitions
- the present invention relates to a laminated film and a method for producing a composite film using the laminated film.
- organic electroluminescence elements various display devices such as liquid crystal display devices and electronic paper; light source devices such as light source devices for illumination; and solar cells
- organic EL elements various display devices such as liquid crystal display devices and electronic paper
- light source devices such as light source devices for illumination
- solar cells In an apparatus, it is known to use a film having a barrier function that prevents the permeation of moisture and oxygen for the purpose of protecting elements constituting the apparatus.
- a film having a small moisture permeability is preferable.
- a composite film in which a base film and an inorganic layer made of various inorganic materials formed on the base film are combined is known (for example, Patent Document 1).
- the composite film is required to be thin. Then, this inventor tried to manufacture a thin composite film by forming an inorganic layer in a thin base film. However, it has been found that when the thickness of the base film is reduced, it is difficult to stably form the inorganic layer.
- the inorganic layer is often formed by a method such as a sputtering method or a CVD (chemical vapor deposition) method.
- a sputtering method or a CVD (chemical vapor deposition) method is usually desired to be performed under high output conditions in order to improve the film quality of the inorganic layer.
- the formation of an inorganic layer at a high output has a large incident energy to the substrate of atoms and molecules that contribute to the film formation, so that the substrate receives damage, particularly damage due to heat. If the thickness of the base film is thin, the base film cannot withstand such heat damage, causing deformation such as wrinkles, or lifting of the base film from the transport roll that transports the base film.
- the substrate film may not be stably conveyed.
- the floating of the base film from the transport roll refers to a phenomenon in which the base film is partially separated from the transport roll when a gap is generated between a part of the base film and the transport roll. . Therefore, when the thickness of the base film is thin, it is difficult to stably form the inorganic layer on the base film.
- the inorganic layer formed at a low output tends to have a low density and a poor film quality.
- performances such as barrier properties and conductivity are low.
- the formation of the inorganic layer at a low output may cause a decrease in production rate.
- the present invention was devised in view of the above problems, and comprises a composite film comprising a base film and an inorganic layer, the thickness of the base film can be reduced, and an inorganic layer formed with high output.
- the purpose is to provide.
- the inventor is a laminated film including a base film made of an alicyclic olefin resin and a protective film made of an alicyclic olefin resin, and the base film and the protection
- the film is directly bonded to the surface on which the activation treatment has been performed, so that the thickness of the base film can be reduced and an inorganic layer can be easily formed on the base film with high output.
- the headline and the present invention were completed. That is, the present invention is as follows.
- the surface of the base film in contact with the protective film or the surface of the protective film in contact with the base film is a laminated film that has been subjected to an activation treatment.
- the activation treatment is at least one selected from the group consisting of plasma treatment, corona treatment, UV ozone treatment, and combustion chemical vapor deposition treatment.
- an inorganic layer is provided on a surface of the base film opposite to the protective film.
- a method for producing a composite film comprising a base film and an inorganic layer,
- the protective film of the base film of a laminated film comprising a base film made of an alicyclic olefin resin and a protective film made of an alicyclic olefin resin provided directly on one surface of the base film Forming an inorganic layer on the opposite side of the surface, Removing the protective film from the base film,
- the surface of the base film in contact with the protective film or the surface of the protective film in contact with the base film is a composite film manufacturing method, wherein the surface is subjected to an activation treatment.
- a composite film including a base film and an inorganic layer the thickness of the base film can be reduced, and an inorganic layer formed with high output can be stably produced.
- the method for producing a composite film of the present invention it is possible to produce a composite film that includes a base film and an inorganic layer, can reduce the thickness of the base film, and includes an inorganic layer formed with high output.
- FIG. 1 is a cross-sectional view schematically showing an example of a layer structure of a laminated film before forming an inorganic layer, which is used in the manufacturing method according to an example of the present invention.
- FIG. 2 is a cross-sectional view schematically showing an example of a layer structure of an intermediate product film used in the manufacturing method according to an example of the present invention.
- FIG. 3 is a cross-sectional view showing an example of an apparatus for forming an inorganic layer by a CVD method.
- FIG. 4 is a cross-sectional view schematically showing an example of a layer structure of a composite film obtained by the manufacturing method according to an example of the present invention.
- (meth) acryl includes both acrylic and methacrylic.
- (Meth) acrylate includes both acrylate and methacrylate.
- the laminated film of the present invention is a film provided with a base film and a protective film.
- This laminated film of the present invention is usually used for producing a composite film comprising a base film and an inorganic layer.
- the laminated film of the present invention includes a base film and a protective film provided directly on one surface of the base film.
- the mode in which the protective film is provided on one surface of the base film is “directly”, and there are other layers such as an adhesive layer and an adhesive layer between the protective film and the base film. This means that no layer is present.
- the base film and the protective film are bonded together by an activation process. That is, the surface of the base film that is in contact with the protective film, or the surface of the protective film that is in contact with the base film is subjected to activation treatment, and depending on the surface subjected to these activation treatments The base film and the protective film are bonded together. At this time, the surface of the base film in contact with the protective film may be an activated surface, and the surface of the protective film in contact with the base film is an activated surface. Both the surface of the base film in contact with the protective film and the surface of the protective film on the side in contact with the base film may be surfaces subjected to the activation treatment.
- the base film is made of an alicyclic olefin resin.
- the alicyclic olefin resin is a resin containing an alicyclic olefin polymer and other optional components as necessary.
- the alicyclic olefin polymer is an amorphous thermoplastic polymer having an alicyclic structure in the main chain and / or side chain.
- the alicyclic olefin polymer usually has a structure obtained by polymerization of an alicyclic olefin.
- a base film made of an alicyclic olefin resin By using a base film made of an alicyclic olefin resin, a composite film having high barrier performance can be obtained. More specifically, since the alicyclic olefin resin has low hygroscopicity, it exhibits mechanical strength as a base film and high water vapor barrier performance, and can improve the barrier performance of the composite film.
- the alicyclic structure in the alicyclic olefin polymer may be a saturated alicyclic hydrocarbon (cycloalkane) structure or an unsaturated alicyclic hydrocarbon (cycloalkene) structure. From the viewpoint of mechanical strength and heat resistance, a cycloalkane structure is preferred.
- the number of carbon atoms constituting one alicyclic structure is usually 4 or more, preferably 5 or more, and usually 30 or less, preferably 20 or less, more preferably 15 or less. When the number of carbon atoms constituting one alicyclic structure is within the above range, properties such as mechanical strength, heat resistance, and film formability are highly balanced, which is preferable.
- the proportion of structural units having an alicyclic structure in the entire alicyclic olefin polymer is preferably 55% by weight or more, more preferably 70% by weight or more, and particularly preferably 90% by weight or more. It is preferable from a transparency and heat resistant viewpoint that the ratio of the structural unit which has an alicyclic structure in an alicyclic olefin polymer exists in this range.
- alicyclic olefin polymer examples include a norbornene polymer, a monocyclic olefin polymer, a cyclic conjugated diene polymer, a vinyl alicyclic hydrocarbon polymer, and hydrogenated products thereof.
- norbornene polymers can be suitably used because of their good transparency and moldability.
- Examples of the norbornene polymer include a ring-opening polymer of a monomer having a norbornene structure, a ring-opening copolymer of a monomer having a norbornene structure and an arbitrary monomer, or a hydrogenated product thereof;
- a hydrogenated product of a ring-opening (co) polymer of a monomer having a norbornene structure is particularly suitable from the viewpoint of moldability, heat resistance, low hygroscopicity, dimensional stability, lightness, and the like. is there.
- (co) polymer refers to a polymer and a copolymer.
- Examples of the monomer having a norbornene structure include bicyclo [2.2.1] hept-2-ene (common name: norbornene), tricyclo [4.3.0.1 2,5 ] deca-3,7. -Diene (common name: dicyclopentadiene), 7,8-benzotricyclo [4.3.0.1 2,5 ] dec-3-ene (common name: methanotetrahydrofluorene), tetracyclo [4.4. 0.1 2,5 . 1 7,10 ] dodec-3-ene (common name: tetracyclododecene), and derivatives of these compounds (for example, those having a substituent in the ring).
- examples of the substituent include an alkyl group, an alkylene group, and a polar group. Moreover, these substituents may be the same or different, and a plurality thereof may be bonded to the ring. Moreover, the monomer which has a norbornene structure may be used individually by 1 type, and may be used combining two or more types by arbitrary ratios.
- Examples of the polar group include heteroatoms or atomic groups having heteroatoms.
- Examples of the hetero atom include an oxygen atom, a nitrogen atom, a sulfur atom, a silicon atom, and a halogen atom.
- Specific examples of the polar group include a carboxyl group, a carbonyloxycarbonyl group, an epoxy group, a hydroxyl group, an oxy group, an ester group, a silanol group, a silyl group, an amino group, a nitrile group, and a sulfonic acid group.
- optional monomers capable of ring-opening copolymerization with a monomer having a norbornene structure include, for example, monocyclic olefins such as cyclohexene, cycloheptene, and cyclooctene and derivatives thereof; and cyclic conjugates such as cyclohexadiene and cycloheptadiene. Dienes and derivatives thereof; and the like.
- the optional monomer capable of ring-opening copolymerization with a monomer having a norbornene structure one type may be used alone, or two or more types may be used in combination at any ratio.
- a ring-opening polymer of a monomer having a norbornene structure, and a ring-opening copolymer of any monomer copolymerizable with a monomer having a norbornene structure are, for example, a known ring-opening monomer. It can be produced by polymerization or copolymerization in the presence of a polymerization catalyst.
- ⁇ -olefin is preferable, and ethylene is more preferable.
- the arbitrary monomer which can carry out addition copolymerization with the monomer which has a norbornene structure may be used individually by 1 type, and may be used combining two or more types by arbitrary ratios.
- An addition copolymer of a monomer having a norbornene structure and an addition copolymer of any monomer that can be copolymerized with a monomer having a norbornene structure include, for example, a monomer of a known addition polymerization catalyst. It can be produced by polymerization or copolymerization in the presence.
- An addition polymer and a hydrogenated product of a polymer such as an addition copolymer of a monomer having a norbornene structure and an arbitrary monomer copolymerizable therewith can be produced by any production method.
- the hydrogenated product of the polymer preferably has a carbon-carbon unsaturated bond in the solution of these polymers in the presence of a known hydrogenation catalyst containing a transition metal such as nickel or palladium, preferably 90%. This can be produced by hydrogenation.
- the molecular weight of the alicyclic olefin polymer contained in the alicyclic olefin resin is appropriately selected according to the purpose of use.
- the weight average molecular weight (Mw) of the alicyclic olefin polymer is usually 10,000 or more, preferably 15,000 or more, more preferably 20,000 or more, and usually 100,000 or less, preferably 80,000 or less. More preferably, it is 50,000 or less.
- Mw weight average molecular weight
- the weight average molecular weight of the alicyclic olefin polymer can be measured as a value in terms of polyisoprene by gel permeation chromatography using cyclohexane as a solvent.
- toluene may be used as a solvent.
- the weight average molecular weight can be measured as a value in terms of polystyrene.
- the proportion of the alicyclic olefin polymer in the alicyclic olefin resin is preferably 67% by weight to 100% by weight, more preferably 77% by weight to 100% by weight.
- the alicyclic olefin resin may contain only one kind of these polymers alone, or may contain two or more kinds in combination at any ratio.
- the base film may consist of a plurality of layers of alicyclic olefin resin.
- the alicyclic olefin resin constituting each layer may be the same as or different from the other layers.
- alicyclic olefin resin examples include, for example, antioxidants, heat stabilizers, light stabilizers, ultraviolet absorbers, antistatic agents, dispersants, chlorine scavengers, flame retardants, and crystallization nuclei.
- Agent, reinforcing agent, antiblocking agent, antifogging agent, mold release agent, pigment, organic or inorganic filler, neutralizing agent, lubricant, decomposition agent, metal deactivator, antifouling agent, antibacterial agent optional Examples thereof include additives such as polymers and thermoplastic elastomers. The amount of these additives may be within a range that does not impair the effects of the present invention. For example, the amount of the additive is usually 0 to 50 parts by weight, preferably 0 to 30 parts by weight with respect to 100 parts by weight of the alicyclic olefin polymer contained in the alicyclic olefin resin.
- the alicyclic olefin resin is not necessarily limited to one having high transparency. However, from the viewpoint of making the composite film useful for a portion that is required to transmit light in a display device and a light source device, the alicyclic olefin resin preferably has high transparency. For example, it is preferable that the total light transmittance measured using an alicyclic olefin resin as a test piece having a thickness of 1 mm is usually 70% or more, preferably 80% or more, more preferably 90% or more.
- the alicyclic olefin resin preferably has a heat distortion temperature of 100 ° C. or higher, more preferably 120 ° C. or higher. Thereby, peeling of the protective film from a base film can be suppressed when forming an inorganic layer.
- the upper limit of the heat distortion temperature of the alicyclic olefin resin is not particularly defined, but may be, for example, 300 ° C. or less.
- a method for obtaining a base film by molding an alicyclic olefin resin is not particularly limited.
- the base film can be manufactured by forming a resin into a film by a melt molding method, a solution casting method, or the like.
- a commercially available alicyclic olefin resin film can be used.
- the base film may be a stretched film that has been subjected to a stretching process, or may be an unstretched film that has not been subjected to a stretching process.
- the thickness of the base film can be set according to the application of the composite film, it is preferably thin from the viewpoint of realizing thinning of the composite film.
- the specific range of the thickness of the base film is preferably 150 ⁇ m or less, more preferably 125 ⁇ m or less, and particularly preferably 100 ⁇ m or less.
- the lower limit is not particularly limited, but is usually 10 ⁇ m or more, preferably 15 ⁇ m or more, more preferably 20 ⁇ m or more from the viewpoint of handling properties.
- the surface of the base film that is in contact with the protective film may be a surface that has been activated. That is, the surface of the base film that is in contact with the protective film may be subjected to an activation treatment before being bonded to the surface of the protective film.
- the film of an alicyclic olefin resin has low adhesiveness, it is difficult to stably bond the alicyclic olefin resin films to each other simply by pressure bonding.
- the base film since the base film has a surface subjected to the activation treatment as described above, the base film and the protective film can be stably bonded, so when forming the inorganic layer It can suppress that a protective film peels from a base film.
- the base film and the protective film are bonded together without interposing the adhesive layer and the pressure-sensitive adhesive layer, the protective film can be easily peeled off from the base film after the inorganic layer is formed.
- the surface of the base film that has been activated is activated, and the wettability with water is usually higher than before the treatment.
- the degree of activation treatment can be evaluated by the degree of wettability. Therefore, for example, the degree of activation treatment can be expressed by the contact angle with water.
- the contact angle with respect to pure water of the surface subjected to the activation treatment of the base film is preferably less than 80 °, more preferably 50 ° or less, particularly preferably 40 ° or less, and preferably Is 10 ° or more.
- the surface of the protective film in contact with the base film is an activated surface
- the surface of the base film in contact with the protective film may not necessarily be activated. Good.
- the surface of the base film in contact with the protective film was subjected to the activation treatment. A surface is preferred.
- the activation treatment examples include plasma treatment such as atmospheric pressure plasma treatment and vacuum plasma treatment, corona treatment, UV ozone treatment, combustion chemical vapor deposition treatment and the like.
- the combustion chemical vapor deposition process represents a flame process in which an organosilicon compound is introduced.
- plasma treatment and corona treatment are preferable in that the treatment time is short and the productivity is excellent.
- the plasma treatment is a treatment for activating the surface by performing plasma discharge in a gas atmosphere such as an inert gas and an oxygen gas generated under an atmospheric pressure or a reduced pressure.
- the degree of the reduced pressure can be, for example, 0.1 Torr to 1 Torr.
- the atmospheric pressure plasma treatment which is the treatment under the atmospheric pressure is preferable.
- the plasma treatment can variously modify the treated surface in accordance with the type of gas, it is preferable to appropriately select the type of gas when performing the activation treatment.
- the gas include nitrogen; oxygen; rare gases such as argon and helium; acrylic acid; hydroxyalkyl; fluorine-based compounds such as CF 4 , CHF 3 , and C 2 F 6 ; These gases may be used alone or in combination of two or more at any ratio.
- a preferable gas for example, a mixed gas obtained by mixing about 10% of oxygen with an inert gas such as argon can be cited.
- the plasma output in the plasma treatment is preferably set in the range of 0.2 kW to 3 kW. Further, the conveyance speed of the film subjected to the plasma treatment is preferably 3 m / min to 70 m / min, and more preferably 3 m / min to 50 m / min.
- the frequency range is preferably 10 kHz to 100 kHz.
- the processing time may be about 3 minutes, for example.
- Corona treatment is a method of treating the surface of a film by generating a corona by applying a high voltage at a high frequency between the dielectric and the insulated electrode, and passing the film between the dielectric and the electrode.
- adhesiveness is imparted to the surface subjected to corona treatment according to the type of electrode, electrode spacing, voltage, humidity, and type of film to be treated.
- a material of the electrode for example, ceramics, aluminum and the like are preferable.
- the distance between the electrode and the dielectric is preferably 1 mm to 5 mm, more preferably 1 mm to 3 mm.
- the conveyance speed of the film subjected to the corona treatment is preferably 3 m / min to 70 m / min, and more preferably 3 m / min to 50 m / min.
- the corona output intensity is preferably 0.2 kW or more, more preferably 0.5 kW or more, preferably 3 kW or less, more preferably 1.5 kW or less.
- the protective film is made of an alicyclic olefin resin.
- an alicyclic olefin resin which forms a protective film the thing of the range demonstrated as an alicyclic olefin resin which can be used as a material of a base film can be used arbitrarily.
- an alicyclic olefin resin of a protective film you may use what differs from the alicyclic olefin resin of a base film.
- the alicyclic olefin resin of the protective film is preferably the same as the alicyclic olefin resin of the base film.
- the method for obtaining the protective film by molding the alicyclic olefin resin is not particularly limited.
- a method similar to the method of forming a base film by molding an alicyclic olefin resin can be used.
- the protective film may be a stretched film that has been subjected to a stretching process, or may be an unstretched film that has not been subjected to a stretching process.
- the thickness of the protective film is preferably thicker than the thickness of the base film, usually 75 ⁇ m or more, preferably 100 ⁇ m or more, more preferably 120 ⁇ m or more, and usually 300 ⁇ m or less, preferably 250 ⁇ m or less, more preferably 200 ⁇ m or less. is there.
- the thickness of the protective film equal to or greater than the lower limit of the above range, the mechanical strength of the laminated film of the present invention can be increased, so deformation of the laminated film can be prevented when forming the inorganic layer, It can be formed stably. Furthermore, it can suppress that a protective film peels from a base film when forming an inorganic layer.
- a film can be easily conveyed when forming an inorganic layer because it is below an upper limit. Specifically, for example, the occurrence of film floating from a roll that supports the conveyance of the film can be effectively suppressed.
- the protective film has a multilayer structure including a plurality of resin layers, the total thickness of the plurality of layers is preferably within the above range.
- the ratio T2 / T1 between the thickness T1 of the base film and the thickness T2 of the protective film is usually 1 or more, preferably 1.1 or more, more preferably 1.25 or more, and usually 6 or less, preferably 5 Below, more preferably 4 or less.
- the surface of the protective film on the side in contact with the base film may be a surface subjected to activation treatment. That is, the surface of the protective film on the side in contact with the base film may be subjected to an activation treatment before being bonded to the base film. Since the protective film has a surface subjected to such activation treatment, the base film and the protective film can be stably bonded to each other, so that the protective film is formed when the inorganic layer is formed. It can suppress peeling from. Moreover, since the base film and the protective film are bonded together without interposing the adhesive layer and the pressure-sensitive adhesive layer, the protective film can be easily peeled off from the base film after the inorganic layer is formed.
- the surface of the protective film that has been activated is activated, and the wettability with water is usually higher than before the treatment. Therefore, the degree of the activation treatment of the surface subjected to the activation treatment of the protective film can be represented by the contact angle with respect to water, as with the surface subjected to the activation treatment of the base film.
- the contact angle with respect to the pure water of the surface subjected to the activation treatment of the protective film is preferably less than 80 °, more preferably 50 ° or less, particularly preferably 40 ° or less, and preferably 10 ° or more. .
- the surface of the protective film in contact with the base film is a surface subjected to the activation treatment
- the surface of the protective film in contact with the base film may not necessarily be subjected to the activation treatment. Good.
- the surface of the protective film in contact with the base film was subjected to the activation treatment. A surface is preferred.
- Examples of the activation treatment include the same examples as those exemplified as the activation treatment that can be performed on the base film. Among these, atmospheric pressure plasma treatment and corona treatment are preferable in that the treatment time is short and the productivity is excellent.
- the laminated film of the present invention may include a film other than the base film and the protective film.
- the surface of the protective film opposite to the base film may be provided with an easy-sliding layer, an antistatic layer, and the like.
- the easy slip layer for example, a resin layer containing a polymer and particles can be used.
- the easy adhesion layer containing particles can improve the slipperiness of the surface having the large surface roughness. Therefore, a laminated film provided with such a slippery layer has good handling properties and can stably suppress blocking and wrinkles.
- blocking refers to a phenomenon in which the contacted surfaces adhere to each other in a film wound up as a roll body.
- polyurethane As the polymer contained in the resin forming the easy-sliding layer, for example, polyurethane can be used.
- Polypolyurethane can strongly adhere to a protective film made of an alicyclic olefin resin with low adhesiveness, and therefore effectively prevents the slippery layer from peeling off from the protective film when forming an inorganic layer. Can do.
- polyurethane for example, polyurethane obtained by reacting (i) a component containing an average of 2 or more active hydrogens in one molecule and (ii) a polyvalent isocyanate component can be used.
- a polyurethane produced by chain-extending a prepolymer obtained from the components (i) and (ii) using a chain extender and adding water to form a dispersion. can be used.
- the prepolymer can be produced as a prepolymer containing an isocyanate group by subjecting the component (i) and the component (ii) to a urethanization reaction under an excess of isocyanate groups.
- the urethane reaction can be carried out in an organic solvent that is inert to the reaction and has a high affinity for water. Further, before the chain extension of the prepolymer, the prepolymer obtained by the urethanization reaction may be neutralized. These polyurethanes may contain an acid structure. Furthermore, the acid structure may be partially or completely neutralized.
- Such polyurethane is commercially available as a composition comprising water and a polymer dispersed in the water.
- Examples of such commercially available polyurethanes include the “Adeka Bon titer” series manufactured by Asahi Denka Kogyo Co., Ltd., the “Olestar” series manufactured by Mitsui Toatsu Chemical Co., Ltd., and the “Bondick” manufactured by Dainippon Ink & Chemicals, Inc.
- inorganic particles include inorganic oxides such as silica, titania, alumina, zirconia; calcium carbonate, talc, clay, calcined kaolin, calcined calcium silicate, hydrated calcium silicate, aluminum silicate, magnesium silicate, calcium phosphate Etc.
- inorganic particles include inorganic oxides such as silica, titania, alumina, zirconia; calcium carbonate, talc, clay, calcined kaolin, calcined calcium silicate, hydrated calcium silicate, aluminum silicate, magnesium silicate, calcium phosphate Etc.
- silica is preferable.
- Silica particles are excellent in ability to suppress the generation of wrinkles and transparency, and have good dispersibility and dispersion stability in a resin containing polyurethane.
- amorphous colloidal silica particles are particularly preferable.
- One type of particles may be used alone, or two or more types may be used in combination at any ratio.
- the average particle diameter of the particles is usually 1 nm or more, preferably 5 nm or more, more preferably 10 nm or more, and usually 500 nm or less, preferably 300 nm or less, more preferably 200 nm or less.
- an average particle diameter more than the lower limit of the said range, the slipperiness
- multilayer film can be suppressed by using below an upper limit.
- a particle size distribution is measured by a laser diffraction method, and a particle size in which the cumulative volume calculated from the small diameter side in the measured particle size distribution is 50% is adopted.
- the amount of the particles is usually 0.5 parts by weight or more, preferably 5 parts by weight or more, more preferably 8 parts by weight or more, and usually 20 parts by weight or less, preferably 18 parts by weight or less with respect to 100 parts by weight of the polymer. More preferably, it is 15 parts by weight or less.
- the easy-sliding layer can contain any component other than the polymer and particles.
- Optional components include, for example, crosslinking agents, heat stabilizers, weathering stabilizers, leveling agents, surfactants, antioxidants, antistatic agents, slip agents, antiblocking agents, antifogging agents, lubricants, dyes, pigments Natural oil, synthetic oil, wax and the like. One of these may be used alone, or two or more of these may be used in combination at any ratio.
- the easy-sliding layer is prepared, for example, by preparing a resin composition containing a polymer, particles and a solvent, and optional components as necessary, and applying the resin composition onto the surface of the protective film. Can be produced by curing the layer of the resin composition. Moreover, you may perform surface treatments, such as an activation process, in the surface which forms the slippery layer of a protective film, before forming a slippery layer. Usually, water is used as the solvent of the resin composition. The layer of the resin composition can be cured, for example, by irradiation with active energy rays such as ultraviolet rays, heating, or the like.
- An easy slip layer may be formed before bonding a protective film and a base film, and may be formed after bonding a protective film and a base film.
- intermediate product film laminated film with an inorganic layer
- the step of forming an inorganic layer on the surface of the laminated film opposite to the protective film of the base film Do.
- the film obtained by the step of forming the inorganic layer is a laminated film including a protective film, a base film, and an inorganic layer in this order.
- a laminated film having an inorganic layer on the surface opposite to the protective film of the base film is hereinafter appropriately referred to as an “intermediate film”.
- the inorganic layer can be a layer substantially made of an inorganic material.
- the layer substantially composed of the inorganic material refers to a layer in which the proportion of the inorganic material in the layer is 60% by weight to 100% by weight.
- the inorganic layer is preferably a layer made of only an inorganic material.
- the inorganic layer is preferably a layer containing at least one selected from the group consisting of metal oxides, metal nitrides, and metal oxynitrides.
- the metal means an element including a semimetal such as silicon.
- the inorganic layer may be a single-layered layer composed of one layer or a multilayered layer including two or more layers.
- Examples of the layer included in the inorganic layer include a barrier layer and a conductive film.
- the inorganic layer may include only the barrier layer, may include only the conductive film, or may include a combination of the barrier layer and the conductive film.
- the inorganic layer usually includes the barrier layer and the conductive film in this order from the side closer to the base film.
- the barrier layer is a layer having a function capable of blocking water.
- the barrier layer usually has a water vapor transmission rate of 1.0 g / m 2 ⁇ day or less, preferably 0.2 g / m 2 ⁇ day or less, more preferably 0.1 g / m 2 ⁇ day or less. Is a layer.
- the composite film can prevent deterioration of the member provided with the composite film due to water.
- Examples of the inorganic material forming the barrier layer include metal oxides, metal nitrides, and metal oxynitrides containing silicon or aluminum as a metal element. Among these, metal oxides, metal nitrides, and metal oxynitrides containing silicon are particularly preferable.
- Examples of the composition of silicon-containing metal oxides, metal nitrides, and metal oxynitrides include SiOx (1.5 ⁇ x ⁇ 1.9), SiNy (1.2 ⁇ y ⁇ 1.5), and SiOxNy. Examples include compositions represented by (1 ⁇ x ⁇ 2 and 0 ⁇ y ⁇ 1). By using an inorganic material having such a composition, characteristics such as transparency and barrier properties can be improved. Moreover, these may be used individually by 1 type and may be used combining two or more types by arbitrary ratios.
- the thickness of the barrier layer is preferably 3 nm or more, more preferably 10 nm or more, preferably 2000 nm or less, more preferably 1000 nm or less.
- Examples of the method for forming the barrier layer include vapor deposition, sputtering, ion plating, ion beam assisted vapor deposition, arc discharge plasma vapor deposition, thermal CVD, and plasma CVD.
- the conductive film is a film having a surface resistance of 1000 ⁇ / ⁇ or less.
- Examples of the inorganic material for forming the conductive film include ITO (indium tin oxide), IZO (indium zinc oxide), ZnO (zinc oxide), IWO (indium tungsten oxide), ITiO (indium titanium oxide), and AZO (aluminum zinc).
- Oxide indium tin oxide
- IZO indium zinc oxide
- ZnO zinc oxide
- IWO indium tungsten oxide
- ITiO indium titanium oxide
- AZO aluminum zinc
- Oxide GZO (gallium zinc oxide)
- XZO zinc-based special oxide
- IGZO indium gallium zinc oxide
- the thickness of the conductive film is preferably 30 nm or more, more preferably 50 nm or more, preferably 250 nm or less, more preferably 220 nm or less.
- Examples of the method for forming the conductive film include a sputtering method and a vapor deposition method.
- the intermediate film can include an arbitrary layer other than the above-described layers.
- the intermediate film may include an arbitrary layer on the surface of the inorganic layer opposite to the base film.
- Specific examples of such an arbitrary layer include an antistatic layer, a hard coat layer, and a contamination prevention layer.
- the arbitrary layer can be provided by a method such as a method of applying and curing a material of an arbitrary layer on the inorganic layer, or a method of bonding an arbitrary layer by thermocompression bonding.
- the inorganic layer can be formed by the method exemplified in the description of the inorganic layer.
- the laminated film of the present invention includes not only the base film but also the protective film, when the inorganic layer forming method is performed at a high output, the base film is deteriorated due to thermal damage, from the transport roll.
- the base film can be prevented from floating.
- the base film and the protective film are bonded together by the activation process, it can suppress that a protective film peels off from a base film, even when manufacturing an inorganic layer with high output. Therefore, the inorganic layer can be stably formed at a high output while using the thin base film. For this reason, it is possible to rapidly produce an inorganic layer having good film quality.
- the protective film is peeled off from the base film to obtain a composite film.
- the base film and the protective film are directly bonded together without sandwiching layers such as an adhesive layer and a pressure-sensitive adhesive layer between them. Therefore, it is possible to quickly and easily remove the protective film from the base film.
- the activation treatment performed for bonding the base film and the protective film usually has a property that the bonding strength is reduced in a high humidity environment and the protective film can be easily peeled off from the base film. Therefore, it is preferable to perform the process of peeling a protective film from a base film in a high humidity environment.
- any process other than the above may be performed.
- an arbitrary layer may be formed on the surface of the inorganic layer opposite to the base film, or an arbitrary layer may be formed on the surface of the base film opposite to the inorganic layer. May be.
- a step of cutting the obtained composite film into a desired shape may be performed.
- the composite film thus obtained includes a base film and an inorganic layer.
- the thickness of the base film can be reduced, the thickness of the composite film itself can be reduced.
- the inorganic layer of the composite film is formed by a high-output film forming method and has a good film quality, so that the excellent performance that the inorganic layer should exhibit can be sufficiently exhibited.
- a barrier layer is provided as the inorganic layer, the excellent water vapor blocking ability of the barrier layer can be sufficiently exhibited, so that a low water vapor transmission rate can be realized as the entire composite film.
- the specific water vapor transmission rate of the entire composite film can be, for example, 1 ⁇ 10 ⁇ 6 g / m 2 ⁇ day to 1 ⁇ 10 ⁇ 2 g / m 2 ⁇ day.
- the composite film is usually excellent in transparency.
- the specific total light transmittance of the composite film is usually 85% to 100%, preferably 90% to 100%.
- the light transmittance can be measured with a spectrophotometer (manufactured by JASCO Corporation, ultraviolet-visible near-infrared spectrophotometer “V-570”) in accordance with JIS K0115.
- the haze of the composite film is not particularly limited, it is generally preferable that the composite film has a low haze when used for optical applications not specifically intended to diffuse light.
- the haze of the composite film can be preferably 3.0% or less, more preferably 1.0% or less.
- the haze can be measured according to JIS K7136-1997.
- the composite film can be manufactured as a long film. Moreover, in order to manufacture such a long composite film, a long film can be used as the base film and the protective film.
- the long film refers to a film having a dimension in the length direction that is usually 10 times or more, preferably 50 times or more, more preferably 100 times or more the dimension in the width direction.
- Such a long film can be stored and transported as a roll shape (roll body).
- the composite film can be efficiently manufactured because the inorganic layer can be formed with high output by roll-to-roll.
- the roll-to-roll refers to a mode in which the film fed from the feeding roll is continuously processed, the processed film is wound up, and wound up as a roll body of the product.
- the composite film manufactured as a long film can be cut
- FIG. 1 is a cross-sectional view schematically showing an example of a layer structure of a laminated film before forming an inorganic layer, which is used in the manufacturing method according to an example of the present invention.
- the laminated film before forming the inorganic layer is appropriately referred to as a “support film”.
- the manufacturing method of the composite film using the support body film which has a structure shown in FIG. 1 is mentioned as an example, and it demonstrates.
- the support film 100 includes a base film 110 and a protective film 120 provided directly on one surface 110 ⁇ / b> D of the base film 110.
- the protective film 120 can be equipped with arbitrary layers, such as a slippery layer, in the surface 120D on the opposite side to the base film 110 as needed.
- the surface 110D of the base film 110 made of an alicyclic olefin resin is subjected to an activation process (Step I).
- the surface 120U of the protective film 120 made of an alicyclic olefin resin is subjected to an activation treatment (step II).
- the base film 110 and the protective film 120 are bonded so that the surfaces 110D and 120U subjected to the activation treatment are in contact (step III).
- This bonding can be performed by a method such as pressing the base film 110 and the protective film 120 in a heated state as necessary.
- the support body film 100 as shown in FIG. 1 is obtained.
- Such a support film 100 is preferably manufactured as a long product by a roll-to-roll operation, and can be used for the next step after it is in a roll state. By making the support film 100 into the state of a roll body, it can be easily supplied to the apparatus that performs the operation under the next reduced pressure while maintaining the long shape.
- FIG. 2 is a cross-sectional view schematically showing an example of a layer structure of an intermediate product film used in the manufacturing method according to an example of the present invention.
- the inorganic layer 130 is formed on the surface 110U of the base film 110 of the support film 100 opposite to the protective film 120 ( Step IV).
- the inorganic layer 130 can be formed by, for example, an evaporation method such as CVD and an operation such as sputtering.
- middle goods film 140 provided with the protective film 120, the base film 110, and the inorganic layer 130 in this order is obtained.
- FIG. 3 is a cross-sectional view showing an example of a film forming apparatus for forming the inorganic layer 130 by the CVD method.
- a film forming apparatus 200 is a film winding type plasma CVD apparatus, and continuously forms an inorganic layer 130 on a support film 100 fed out from a roll body 201 of the support film 100 by CVD. Then, a series of operations for winding the intermediate product film 140 as the roll body 202 is performed.
- the film forming apparatus 200 includes a guide roll 211, a can roll 212, and a guide roll 213, whereby the fed support film 100 is guided in the direction indicated by the arrow A ⁇ b> 21 and used for the formation process of the inorganic layer 130. be able to.
- the support film 100 is guided by the can roll 212 while being guided by the can roll 212. It will be in the state which adhered to.
- the can roll 212 rotates in the direction indicated by the arrow A22, and the support film 100 thereon is conveyed in a state of approaching the reaction tube 221. At that time, electric power is applied from the power source 223 to the electrode 222, while the can roll 212 is grounded by an appropriate grounding member (not shown), and the gas of the material of the inorganic layer 130 from the gas inlet 224 in the direction of arrow A23. Is introduced. Thereby, the inorganic layer 130 can be continuously formed on the surface of the support film 100. Such a series of operations is performed in a space surrounded by the vacuum chamber 290. The pressure in the vacuum chamber 290 can be reduced by operating the vacuum exhaust device 230 and adjusted to a pressure suitable for CVD.
- the base film is likely to float from the can roll 212, and it is difficult to continuously form a good inorganic layer.
- the formation method of the inorganic layer at a high output was often performed under high temperature conditions, when the base film was thin, the base film was deteriorated due to thermal damage, and the inorganic layer was stably formed. Sometimes became difficult.
- a substrate film having generally high optical performance generally has a smooth surface, blocking is likely to occur.
- the predetermined protective film 120 on the surface of the base film 110, the support film 100 can be prevented from being lifted, deteriorated, and blocked.
- FIG. 4 is a cross-sectional view schematically showing an example of the layer structure of the composite film 150 obtained by the manufacturing method according to an example of the present invention.
- the protective film 120 is peeled off from the base film 110 (step V).
- the composite film 150 provided with the base film 110 and the inorganic layer 130 is obtained.
- a protective film is bonded to a base film with an adhesive layer, an adhesive layer, or the like, it is difficult to smoothly peel the protective film from the base film.
- the base film 110 and the protective film 120 are directly bonded to the surfaces 110D and 120U that have been subjected to the activation treatment, so that the peeling can be performed easily and smoothly. Therefore, the composite film 150 can be manufactured efficiently.
- the manufacturing method shown in the above example may be further modified.
- another layer may be provided on the surface 130U of the inorganic layer 130 opposite to the base film 110.
- a barrier layer may be formed as the inorganic layer 130
- a conductive film (not shown) may be formed on the surface 130U of the inorganic layer 130.
- another layer may be provided on the obtained composite film 150.
- [6. Application] Applications of the composite film manufactured by the above-described manufacturing method include, for example, display devices having organic EL elements, various display devices such as liquid crystal display devices and electronic paper; light source devices such as illumination light source devices; devices such as solar cells Can be used.
- display devices having organic EL elements various display devices such as liquid crystal display devices and electronic paper
- light source devices such as illumination light source devices
- devices such as solar cells Can be used.
- it if it is a composite film provided with a barrier layer as an inorganic layer, it can be used as a sealing film having a barrier function that prevents the permeation of moisture and oxygen for the purpose of protecting elements constituting the device.
- it is a composite film provided with an electrically conductive film as an inorganic layer, it can be used as an electrode or wiring provided in the apparatus.
- the surface resistance of the conductive film was measured by “Loresta GP” manufactured by Mitsubishi Chemical Analytech.
- Example 1 (1-1. Production of COP base material) Pellets of alicyclic olefin resin (“ZEONOR 1430R” manufactured by Nippon Zeon Co., Ltd., glass transition temperature: 138 ° C.) were melted with a short screw extruder at a temperature of 240 ° C. A long resin film 1 (thickness 188 ⁇ m) and a long resin film 2 (thickness 47 ⁇ m) were produced.
- ZEONOR 1430R manufactured by Nippon Zeon Co., Ltd., glass transition temperature: 138 ° C.
- the water-based resin composition 1 was applied to the surface of the resin film 1 subjected to the discharge treatment using a roll coater so that the dry film thickness was 0.5 ⁇ m. Thereafter, the applied aqueous resin composition 1 was dried at 140 ° C. over 40 seconds to form an easy-sliding layer on the surface of the resin film 1.
- a normal pressure plasma surface treatment was applied as an activation treatment to the surface of the resin film 1 on which the easy slip layer was formed, on the side opposite to the easy slip layer. Moreover, a normal pressure plasma surface treatment was performed on one side of the resin film 2 as an activation treatment.
- These atmospheric pressure plasma surface treatments are performed using an atmospheric pressure plasma surface treatment apparatus (“AP-T03-L” manufactured by Sekisui Chemical Co., Ltd.) with an output of 1.5 kW, a frequency of 25 kHz, a nitrogen gas flow rate of 50 L / min, and an irradiation rate of 30 cm. Per minute.
- the contact angle of the surface subjected to the activation treatment was measured.
- the surface of the resin film 1 subjected to the activation treatment and the surface of the resin film 2 subjected to the activation treatment were combined and pressure-bonded using a laminator (“ML-300T” manufactured by MCK).
- the lamination conditions at this time were a pressure of 0.4 MPa and a temperature of 130 ° C.
- barrier layer (1-5. Formation of barrier layer (CVD method)
- a barrier layer was formed on the surface of the laminated film A on the resin film 2 side by a CVD method.
- the operation of forming the barrier layer was performed using a film forming apparatus (film winding type plasma CVD apparatus) shown in FIG.
- the conditions for forming the barrier layer are: tetramethylsilane (TMS) flow rate 10 sccm, oxygen (O 2 ) flow rate 100 sccm, output 0.8 kW, total pressure 5 Pa, film transport speed 0.5 m / min, and RF plasma discharge.
- TMS tetramethylsilane
- O 2 oxygen
- the inorganic layer was formed.
- a 300 nm thick barrier layer made of SiOx was formed, and a laminated film B having a layer configuration of (barrier layer) / (resin film 2) / (resin film 1) / (sliding layer) was obtained.
- the water vapor transmission rate of the barrier layer was measured, it was 0.03 g / m 2 / day or less.
- the obtained laminated film B was wound up into a roll body.
- ⁇ Film suitability Good The protective film does not peel off even when exposed to high temperatures during CVD. Defective ... The protective film peels off when exposed to high temperatures during CVD.
- a conductive film was formed on the surface of the laminated film B on the barrier layer side by a sputtering method.
- the operation of forming the conductive film was performed using a film winding type magnetron sputtering apparatus.
- a sputtering target an In 2 O 3 —SnO 2 ceramic target was used.
- Other conditions for forming the conductive film were an argon (Ar) flow rate of 150 sccm, an oxygen (O 2 ) flow rate of 10 sccm, an output of 4.0 kw, a degree of vacuum of 0.3 Pa, and a film conveyance speed of 0.5 m / min.
- a conductive film made of ITO having a thickness of 100 nm is formed, and a laminated film C having a layer structure of (conductive film) / (barrier layer) / (resin film 2) / (resin film 1) / (sliding layer).
- a laminated film C having a layer structure of (conductive film) / (barrier layer) / (resin film 2) / (resin film 1) / (sliding layer).
- ⁇ Film suitability Good The protective film does not peel even when exposed to high temperatures during sputtering. Defective ... The protective film peels off when exposed to high temperatures during sputtering.
- the resin film 1 that is a protective film is peeled from the resin film 2 that is a base film of the laminated film C, and has a layer structure of (conductive film) / (barrier layer) / (resin film 2). A composite film was obtained. The resin film 1 could be peeled smoothly.
- Example 2 As an activation treatment for the surface opposite to the slippery layer of the resin film 1 and one surface of the resin film 2 in the step (1-4), a corona treatment was performed instead of the atmospheric pressure plasma surface treatment. This corona treatment was performed under conditions of an output of 0.6 kW and a treatment speed of 5 m / min. Except for the above items, the laminated films B and C and the composite film were produced and evaluated in the same manner as in Example 1.
- Example 3 In the step (1-4), UV ozone treatment was performed instead of atmospheric pressure plasma surface treatment as the activation treatment of the surface opposite to the slippery layer of the resin film 1 and one surface of the resin film 2. This UV ozone treatment was performed under the conditions of an irradiation time of 5 m / min and an irradiation distance of 10 mm. Except for the above items, the laminated films B and C and the composite film were produced and evaluated in the same manner as in Example 1.
- Example 4 In the step (1-4), as the activation treatment of the surface opposite to the slippery layer of the resin film 1 and one surface of the resin film 2, a combustion chemical vapor deposition treatment was performed instead of the atmospheric pressure plasma surface treatment. .
- This combustion chemical vapor deposition treatment was carried out using a silicic acid flame treatment apparatus with a flame of a fuel gas containing 1,2-dichlorotetramethylsilane, which is a silane compound, at a treatment speed of 1000 mm / second. Except for the above items, the laminated films B and C and the composite film were produced and evaluated in the same manner as in Example 1.
- Example 5 The resin film 2 produced in the step (1-1) was stretched using a tenter apparatus under conditions of 140 ° C. and a film conveyance speed of 20 m / min.
- This tenter device was provided with a gripper capable of gripping both ends of the film in the width direction and a rail capable of guiding the gripper.
- the rail was set so that the slow axis of the film obtained after stretching was inclined by 45 ° with respect to the flow direction.
- a stretched film having a thickness of 23 ⁇ m and a slow axis angle of 45 ° with respect to the flow direction was obtained.
- the stretched film thus obtained was used in place of the resin film 2.
- the laminated films B and C and the composite film were produced and evaluated in the same manner as in Example 1.
- step (1-4) the surface of the resin film 1 opposite to the slippery layer and the one surface of the resin film 2 were not activated. Except for the above items, the production and evaluation of the laminated films B and C and the composite film were tried in the same manner as in Example 1. However, since a good barrier layer was not obtained in step (1-5) and a conductive film could not be formed thereon, the evaluation in step (1-5) was conducted until step (1-6) ) And (1-7) were not performed.
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Abstract
Description
すなわち、本発明は以下の通りである。
前記基材フィルムの前記保護フィルムと接する側の面、又は、前記保護フィルムの前記基材フィルムと接する側の面は、活性化処理を施された面である、積層フィルム。
〔2〕 前記活性化処理が、プラズマ処理、コロナ処理、UVオゾン処理及び燃焼化学気相蒸着処理からなる群より選ばれる少なくとも一つである、〔1〕記載の積層フィルム。
〔3〕 前記基材フィルムの前記保護フィルムとは反対側の面に、無機層を備える、〔1〕又は〔2〕記載の積層フィルム。
〔4〕 前記無機層が、金属酸化物、金属窒化物及び金属酸化窒化物からなる群より選ばれる少なくとも1つを含む、〔3〕記載の積層フィルム。
〔5〕 前記無機層が、バリア層を含む、〔3〕又は〔4〕記載の積層フィルム。
〔6〕 前記無機層が、導電膜を含む、〔3〕~〔5〕のいずれか一項に記載の積層フィルム。
〔7〕 前記活性化処理を施された面の、純水に対する接触角が80°未満である、〔1〕~〔6〕のいずれか一項に記載の積層フィルム。
〔8〕 基材フィルム及び無機層を備えた複合フィルムの製造方法であって、
脂環式オレフィン樹脂からなる基材フィルム、及び、前記基材フィルムの一方の面に直接に設けられた脂環式オレフィン樹脂からなる保護フィルムを備える積層フィルムの、前記基材フィルムの前記保護フィルムとは反対側の面に、無機層を形成する工程と、
前記基材フィルムから前記保護フィルムを剥がす工程とを含み、
前記基材フィルムの前記保護フィルムと接する側の面、又は、前記保護フィルムの前記基材フィルムと接する側の面は、活性化処理を施された面である、複合フィルムの製造方法。
本発明の複合フィルムの製造方法によれば、基材フィルム及び無機層を備え、基材フィルムの厚みを薄くでき、且つ、高出力で形成された無機層を備える複合フィルムを製造できる。
以下の説明において、「(メタ)アクリル」とは、アクリル及びメタクリルの両方を包含する。また、「(メタ)アクリレート」は、アクリレートとメタクリレートの両方を包含する。
本発明の積層フィルムは、基材フィルム及び保護フィルムを備えるフィルムである。この本発明の積層フィルムは、通常、基材フィルム及び無機層を備える複合フィルムを製造するために用いられる。
本発明の積層フィルムは、基材フィルム、及び、前記基材フィルムの一方の面に直接に設けられた保護フィルムを備える。ここで、保護フィルムが基材フィルムの一方の面に設けられる態様が「直接」である、とは、保護フィルムと基材フィルムとの間には、接着剤層、粘着剤層のような他の層が介在していないことを表す。
基材フィルムは、脂環式オレフィン樹脂からなる。脂環式オレフィン樹脂は、脂環式オレフィン重合体と、必要に応じてその他の任意の成分とを含有する樹脂である。
これらの添加剤の量は、本発明の効果を損なわない範囲としうる。例えば、前記の添加剤の量は、脂環式オレフィン樹脂に含まれる脂環式オレフィン重合体100重量部に対して、通常0~50重量部、好ましくは0~30重量部である。
一般に、脂環式オレフィン樹脂のフィルムは、接着性が低いので、単に圧着するだけでは脂環式オレフィン樹脂のフィルム同士を安定して貼り合せることは難しい。これに対し、基材フィルムが前記のように活性化処理を施された面を有することにより、基材フィルムと保護フィルムとを安定して貼り合せることができるので、無機層を形成する際に保護フィルムが基材フィルムから剥離することを抑制することができる。また、接着剤層及び粘着剤層等の層を介さずに基材フィルムと保護フィルムと貼り合せているので、無機層の形成後に、基材フィルムから保護フィルムを容易に剥がすことができる。
保護フィルムは、脂環式オレフィン樹脂からなる。保護フィルムを形成する脂環式オレフィン樹脂としては、基材フィルムの材料として用いうる脂環式オレフィン樹脂として説明した範囲のものを、任意に用いうる。保護フィルムの脂環式オレフィン樹脂としては、基材フィルムの脂環式オレフィン樹脂と異なるものを用いてもよい。ただし、保護フィルムの脂環式オレフィン樹脂は、基材フィルムの脂環式オレフィン樹脂と同様のものを用いることが好ましい。これにより、基材フィルム及び保護フィルムの線膨張係数を同じにできるので、本発明の積層フィルムの反り及びシワ等の変形を生じ難くできる。そのため、無機層の形成時における積層フィルムの挙動を安定させることができるので、膜質の良い無機層を安定して製造できる。
本発明の積層フィルムは、前記の基材フィルム及び保護フィルム以外の膜を備えていてもよい。
例えば、保護フィルムの基材フィルムとは反対側の面に、易滑層及び帯電防止層などを備えていてもよく、中でも易滑層を備えることが好ましい。
また、重合体は、1種類を単独で用いてもよく、2種類以上を任意の比率で組み合わせて用いてもよい。
上述したように基材フィルム及び保護フィルムを備える積層フィルムを用いて複合フィルムを製造する際には、その積層フィルムの基材フィルムの保護フィルムとは反対側の面に無機層を形成する工程を行なう。無機層を形成する工程により得られるフィルムは、保護フィルム、基材フィルム及び無機層をこの順に備える積層フィルムである。このように、本発明の積層フィルムのうち、基材フィルムの保護フィルムとは反対側の面に無機層を備える積層フィルムのことを、以下、適宜「中間品フィルム」と呼ぶ。
無機層は、無機材料から実質的になる層としうる。ここで無機材料から実質的になる層とは、当該層における無機材料の割合が60重量%~100重量%である層を表す。特に、無機層は、無機材料のみからなる層であることが好ましい。また、無機層は、金属酸化物、金属窒化物及び金属酸化窒化物からなる群より選ばれる少なくとも1つを含む層とすることが好ましい。ここで金属は、ケイ素等の半金属を包含する元素を意味する。
また、無機層は、1層からなる単層構造の層であってもよく、2層以上の層を備える複層構造の層であってもよい。
ケイ素を含む金属酸化物、金属窒化物、及び金属酸化窒化物の組成の例としては、SiOx(1.5<x<1.9)、SiNy(1.2<y<1.5)及びSiOxNy(1<x<2および0<y<1)で表される組成が挙げられる。このような組成を有する無機材料を用いることにより、透明性及びバリア性等の特性を良好なものとしうる。
また、これらは、1種類を単独で用いてもよく、2種類以上を任意の比率で組み合わせて用いてもよい。
中間フィルムは、上述した層以外にも、任意の層を備えうる。
例えば、中間フィルムは、無機層の基材フィルムとは反対側の面に、任意の層を備えていてもよい。このような任意の層の具体例を挙げると、帯電防止層、ハードコート層、及び汚染防止層等が挙げられる。任意の層は、例えば、無機層上に任意の層の材料を塗布し硬化させる方法、熱圧着により任意の層を貼り合せる方法、などの方法により設けうる。
上述した積層フィルムを用いて複合フィルムを製造する場合、例えば、基材フィルム及び保護フィルムを備える積層フィルムの、基材フィルムの保護フィルムとは反対側の面に、無機層を形成して、中間品フィルムを得る工程と、その中間品フィルムの基材フィルムから保護フィルムを剥がして、基材フィルム及び無機層を備える複合フィルムを得る工程とを含む製造方法を行なう。
例えば、無機層としてバリア層を備える場合、当該バリア層が有する優れた水蒸気遮断能を十分に発揮できるので、複合フィルム全体として低い水蒸気透過率を実現できる。複合フィルム全体の具体的な水蒸気透過率は、例えば、1×10-6g/m2・day~1×10-2g/m2・dayとしうる。
本発明の複合フィルムの製造方法の好ましい例として、基材フィルムの表面に活性化処理を施す工程Iと、保護フィルムの表面に活性化処理を施す工程IIと、基材フィルム及び保護フィルムを、活性化処理を施した面が接するように貼り合せる工程IIIと、基材フィルムの保護フィルムとは反対側の面に無機層を形成する工程IVと、基材フィルムから保護フィルムを剥がす工程Vとを含む方法が挙げられる。以下において、この方法について説明する。
図1において、支持体フィルム100は、基材フィルム110と、基材フィルム110の一方の面110Dに直接に設けられた保護フィルム120とを備える。また、保護フィルム120は、必要に応じて、基材フィルム110とは反対側の面120Dに、易滑層等の任意の層を備えうる。
このような支持体フィルム100は、好ましくはロールトゥロールの操作により長尺の製品として製造し、これをロール体の状態としてから次の工程に供することができる。支持体フィルム100をロール体の状態とすることにより、次の減圧下での操作を行なう装置に長尺の形状のまま容易に供給をすることができる。
前記のように基材フィルム110と保護フィルム120とを貼り合わせた後で、支持体フィルム100の基材フィルム110の、保護フィルム120とは反対側の面110Uに、無機層130を形成する(工程IV)。無機層130の形成は、例えばCVD等の蒸着法及びスパッタリング等の操作により行ないうる。これにより、図2に示すように、保護フィルム120、基材フィルム110及び無機層130をこの順に備える中間品フィルム140が得られる。
また、一般に脂環式オレフィン樹脂からなる基材フィルム及び保護フィルム等のフィルムは接着性が低いが、本例に係る製造方法では基材フィルム110及び保護フィルム120を活性化処理を施した面110D及び120Uで貼り合せているので、高出力での無機層130の形成を行なう環境においても、基材フィルム110及び保護フィルム120の剥離を抑制できる。
そのため、本例に係る製造方法では、良好な無機層130の連続的な形成を、効率よく達成することが可能である。
前記のようにして基材フィルム110の面110Uに無機層130を形成した後で、基材フィルム110から保護フィルム120を剥がす(工程V)。これにより、図4に示すように、基材フィルム110及び無機層130を備える複合フィルム150が得られる。
例えば接着剤層及び粘着剤層等によって保護フィルムを基材フィルムに貼り合わせた場合には、基材フィルムから保護フィルムを円滑に剥がすことは困難である。しかし、本例に係る製造方法では、基材フィルム110及び保護フィルム120は活性化処理を施した面110D及び120Uを直接に貼り合わせられているので、剥離を容易且つ円滑に行なうことができる。したがって、複合フィルム150の製造を効率よく行なうことが可能である。
例えば、無機層130を形成した後で、基材フィルム110から保護フィルム120を剥がす前に、無機層130の基材フィルム110とは反対側の面130Uに、更に別の層を設けてもよい。具体例を挙げると、まず無機層130としてバリア層を形成し、その無機層130の面130Uに導電膜(図示せず)を形成してもよい。
また、例えば、基材フィルム110から保護フィルム120を剥離した後で、得られた複合フィルム150に更に別の層を設けてもよい。
上述した製造方法で製造される複合フィルムの用途は、例えば、有機EL素子を有する表示装置、液晶表示装置及び電子ペーパー等の各種表示装置;照明用光源装置等の光源装置;太陽電池等の装置において用いうる。この場合、例えば無機層としてバリア層を備える複合フィルムであれば、装置を構成する素子の保護などの目的で、水分及び酸素の透過を妨げるバリア機能を有する封止フィルムとして用いうる。また、例えば無機層として導電膜を備える複合フィルムであれば、装置に設けられる電極又は配線として用いうる。
以下の説明において、量を表す「%」及び「部」は、別に断らない限り重量基準である。また、以下の操作は、別に断らない限り、常温常圧大気中にて行った。さらに、以下の説明において、「sccm」は気体の流量の単位であり、1分間当たりに流れる気体の量を、その気体が25℃、1atmである場合の体積(cm3)で示す。
(バリア層の水蒸気透過率の測定方法)
バリア層の水蒸気透過率は、Technolox社製「DELTAPERM」により測定した。
導電膜の表面抵抗は、三菱化学アナリテック社製「ロレスタGP」により測定した。
接触角計(協和界面科学社製「Drop Master DM500」)を用いて、樹脂フィルムの面に純水を滴下し、滴下してから5秒後に接触角を測定した。
(1-1.COP基材の製造)
脂環式オレフィン樹脂(日本ゼオン社製「ゼオノア1430R」、ガラス転移温度138℃)のペレットを、温度240℃の短軸押出機で溶融し、温度240℃でT型ダイから溶融押出しして、長尺の樹脂フィルム1(厚み188μm)と、長尺の樹脂フィルム2(厚み47μm)を製造した。
極性基を有する重合体としてのポリウレタンの水分散体(第一工業製薬社製「スーパーフレックス210」、カルボキシル基を含有するエステル系ポリウレタン樹脂)を、当該水分散体に含まれるポリウレタンが100部となる量だけとった。この水分散体に、エポキシ化合物(ナガセケムテックス社製「デナコールEX-521」)20部と、セバシン酸ジヒドラジド5部と、シリカ粒子(平均粒子径100nm)8部と、水とを配合して、固形分5%の液状の水系樹脂組成物1を得た。
コロナ処理装置(春日電機社製)を用いて、出力300W、電極長240mm、ワーク電極間3.0mm、搬送速度4m/minの条件で、樹脂フィルム1の片面に放電処理を施した。
易滑層を形成した樹脂フィルム1の易滑層とは反対側の面に、活性化処理として常圧プラズマ表面処理を施した。また、樹脂フィルム2の片面に、活性化処理として常圧プラズマ表面処理を施した。これらの常圧プラズマ表面処理は、常圧プラズマ表面処理装置(積水化学社製「AP-T03-L」)を用いて、出力1.5kw、周波数25kHz、窒素ガス流量50L/分、照射速度30cm/分の条件で行なった。活性化処理を施された樹脂フィルム1及び樹脂フィルム2の一部を用いて、活性化処理を施した面の接触角を測定した。
積層フィルムAの樹脂フィルム2側の面に、CVD法によりバリア層を形成した。バリア層の形成の操作は、図3に示す成膜装置(フィルム巻き取り式プラズマCVD装置)を用いて行った。バリア層を形成する際の条件は、テトラメチルシラン(TMS)流量10sccm、酸素(O2)流量100sccm、出力0.8kW、全圧5Pa、フィルム搬送速度0.5m/minとし、RFプラズマ放電させて無機層の形成を行った。その結果、SiOxからなる厚み300nmのバリア層が形成され、(バリア層)/(樹脂フィルム2)/(樹脂フィルム1)/(易滑層)の層構成を有する積層フィルムBを得た。バリア層の水蒸気透過率を測定したところ、0.03g/m2/day以下であった。得られた積層フィルムBは巻き取ってロール体にした。
良・・・ブロッキングも、搬送ロールからの浮きも無い。
不良・・・ブロッキングが発生するか、又は搬送ロールからの浮きが発生して搬送が困難になる。
良・・・CVD時の高温に曝されても保護フィルムが剥離しない。
不良・・・CVD時の高温に曝された際に保護フィルムが剥離する。
積層フィルムBのバリア層側の面上に、スパッタリング法により導電膜を形成した。導電膜の形成の操作は、フィルム巻き取り式マグネトロンスパッタリング装置を用いて行った。スパッタリングのターゲットとしては、In2O3-SnO2セラミックターゲットを用いた。導電膜を形成する際のその他の条件は、アルゴン(Ar)流量150sccm、酸素(O2)流量10sccm、出力4.0kw、真空度0.3Pa、フィルム搬送速度0.5m/minとした。その結果、ITOからなる厚み100nmの導電膜が形成され、(導電膜)/(バリア層)/(樹脂フィルム2)/(樹脂フィルム1)/(易滑層)の層構成を有する積層フィルムCを得た。導電膜の表面抵抗を測定したところ、50Ω/□以下であった。得られた積層フィルムCは巻き取ってロール体にした。
良・・・ブロッキングも、搬送ロールからの浮きも無い。
不良・・・ブロッキングが発生するか、又は搬送ロールからの浮きが発生して搬送が困難になる。
良・・・スパッタリング時の高温に曝されても保護フィルムが剥離しない。
不良・・・スパッタリング時の高温に曝された際に保護フィルムが剥離する。
高湿環境において、積層フィルムCの基材フィルムである樹脂フィルム2から保護フィルムである樹脂フィルム1を剥離して、(導電膜)/(バリア層)/(樹脂フィルム2)の層構成を有する複合フィルムを得た。樹脂フィルム1の剥離は円滑に行なうことができた。
前記工程(1-4)における樹脂フィルム1の易滑層とは反対側の面及び樹脂フィルム2の片面の活性化処理として、常圧プラズマ表面処理の代わりにコロナ処理を施した。このコロナ処理は、出力0.6kw、処理速度5m/minの条件で行なった。
以上の事項以外は実施例1と同様にして、積層フィルムB及びC並びに複合フィルムの製造及び評価を行なった。
前記工程(1-4)における樹脂フィルム1の易滑層とは反対側の面及び樹脂フィルム2の片面の活性化処理として、常圧プラズマ表面処理の代わりにUVオゾン処理を施した。このUVオゾン処理は、照射時間5m/min、照射距離10mmの条件で行なった。
以上の事項以外は実施例1と同様にして、積層フィルムB及びC並びに複合フィルムの製造及び評価を行なった。
前記工程(1-4)における樹脂フィルム1の易滑層とは反対側の面及び樹脂フィルム2の片面の活性化処理として、常圧プラズマ表面処理の代わりに燃焼化学気相蒸着処理を施した。この燃焼化学気相蒸着処理は、ケイ酸化炎処理装置を用いて、シラン化合物である1,2-ジクロロテトラメチルシランを含む燃料ガスの火炎により、処理速度1000mm/秒の条件で行なった。
以上の事項以外は実施例1と同様にして、積層フィルムB及びC並びに複合フィルムの製造及び評価を行なった。
前記工程(1-1)において製造した樹脂フィルム2を、140℃、フィルム搬送速度20m/minの条件で、テンター装置を用いて延伸した。このテンター装置は、フィルムの幅方向両端を把持しうる把持子と、前記把持子を案内しうるレールとを備えていた。このとき、このテンター装置では、延伸後に得られるフィルムにおいて流れ方向に対して遅相軸が45°傾くように、レールを設定した。これにより、厚さ23μm、流れ方向に対する遅相軸の角度45°の延伸フィルムを得た。こうして得られた延伸フィルムを樹脂フィルム2の代わりに用いた。
以上の事項以外は実施例1と同様にして、積層フィルムB及びC並びに複合フィルムの製造及び評価を行なった。
工程(1-4)における樹脂フィルム1の易滑層とは反対側の面及び樹脂フィルム2の片面の活性化処理を行わなかった。
以上の事項以外は実施例1と同様にして、積層フィルムBの及びC並びに複合フィルムの製造及び評価を試みた。しかし、工程(1-5)において良好なバリア層が得られず、その上に導電膜を形成することができなかったので、工程(1-5)における評価までを行い、工程(1-6)及び(1-7)は行わなかった。
樹脂フィルム1として、脂環式オレフィン樹脂のフィルムの代わりにポリカーボネート樹脂のフィルム(帝人社製「パイラントシートPC-2515」、厚み125μm)を用いた。
以上の事項以外は実施例1と同様にして、積層フィルムBの及びC並びに複合フィルムの製造及び評価を試みた。しかし、工程(1-5)において良好なバリア層が得られず、その上に導電膜を形成することができなかったので、工程(1-5)における評価までを行い、工程(1-6)及び(1-7)は行わなかった。
樹脂フィルム1として、脂環式オレフィン樹脂のフィルムの代わりにポリエチレン樹脂のフィルム(東レフィルム加工社製「トレテック7332」、厚み250μm)を用いた。
以上の事項以外は実施例1と同様にして、積層フィルムBの及びC並びに複合フィルムの製造及び評価を試みた。しかし、工程(1-5)において良好なバリア層が得られず、その上に導電膜を形成することができなかったので、工程(1-5)における評価までを行い、工程(1-6)及び(1-7)は行わなかった。
前記の実施例及び比較例の結果を、表1及び表2に示す。表1及び表2において、接触角の値は、貼り合わせられた面の純水に対する接触角の値を示す。また、表1及び表2において、略称の意味は、以下の通りである。
COP:脂環式オレフィン樹脂
PC:ポリカーボネート樹脂
PE:ポリエチレン樹脂
表2から変わるように、実施例においてはいずれも良好な無機層を安定して製造できた。このことから、本発明により、厚みの薄い基材フィルムに、高出力で無機層を形成することができることが確認された。
110 基材フィルム
110D 基材フィルムの面
110U 基材フィルムの面
120 保護フィルム
120D 保護フィルムの面
130 無機層
130U 無機層の面
140 中間品フィルム(無機層を備える積層フィルム)
150 複合フィルム
200 成膜装置
201 複層物のロール体
202 積層フィルムのロール体
211 ガイドロール
212 キャンロール
213 ガイドロール
221 反応管
222 電極
223 電源
224 ガス導入口
230 真空排気装置
290 真空槽
Claims (8)
- 脂環式オレフィン樹脂からなる基材フィルム、及び、前記基材フィルムの一方の面に直接に設けられた脂環式オレフィン樹脂からなる保護フィルムを備え、
前記基材フィルムの前記保護フィルムと接する側の面、又は、前記保護フィルムの前記基材フィルムと接する側の面は、活性化処理を施された面である、積層フィルム。 - 前記活性化処理が、プラズマ処理、コロナ処理、UVオゾン処理及び燃焼化学気相蒸着処理からなる群より選ばれる少なくとも一つである、請求項1記載の積層フィルム。
- 前記基材フィルムの前記保護フィルムとは反対側の面に、無機層を備える、請求項1又は2記載の積層フィルム。
- 前記無機層が、金属酸化物、金属窒化物及び金属酸化窒化物からなる群より選ばれる少なくとも1つを含む、請求項3記載の積層フィルム。
- 前記無機層が、バリア層を含む、請求項3又は4記載の積層フィルム。
- 前記無機層が、導電膜を含む、請求項3~5のいずれか一項に記載の積層フィルム。
- 前記活性化処理を施された面の、純水に対する接触角が80°未満である、請求項1~6のいずれか一項に記載の積層フィルム。
- 基材フィルム及び無機層を備えた複合フィルムの製造方法であって、
脂環式オレフィン樹脂からなる基材フィルム、及び、前記基材フィルムの一方の面に直接に設けられた脂環式オレフィン樹脂からなる保護フィルムを備える積層フィルムの、前記基材フィルムの前記保護フィルムとは反対側の面に、無機層を形成する工程と、
前記基材フィルムから前記保護フィルムを剥がす工程とを含み、
前記基材フィルムの前記保護フィルムと接する側の面、又は、前記保護フィルムの前記基材フィルムと接する側の面は、活性化処理を施された面である、複合フィルムの製造方法。
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EP14875743.8A EP3088178A4 (en) | 2013-12-25 | 2014-12-25 | Laminated film, and method for manufacturing composite film |
US15/104,907 US10156662B2 (en) | 2013-12-25 | 2014-12-25 | Laminated film, and method for manufacturing composite film |
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US10156662B2 (en) | 2018-12-18 |
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