WO2020241313A1 - 折りたたみ型ディスプレイ - Google Patents
折りたたみ型ディスプレイ Download PDFInfo
- Publication number
- WO2020241313A1 WO2020241313A1 PCT/JP2020/019485 JP2020019485W WO2020241313A1 WO 2020241313 A1 WO2020241313 A1 WO 2020241313A1 JP 2020019485 W JP2020019485 W JP 2020019485W WO 2020241313 A1 WO2020241313 A1 WO 2020241313A1
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- WIPO (PCT)
- Prior art keywords
- film
- layer
- polyester film
- polarizer
- hard coat
- Prior art date
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Images
Classifications
-
- 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
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/133305—Flexible substrates, e.g. plastics, organic film
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/14—Protective coatings, e.g. hard coatings
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
- G02B5/3016—Polarising elements involving passive liquid crystal elements
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
- G02B5/3025—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state
- G02B5/3033—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid
- G02B5/3041—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid comprising multiple thin layers, e.g. multilayer stacks
- G02B5/305—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid comprising multiple thin layers, e.g. multilayer stacks including organic materials, e.g. polymeric layers
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
- G02B5/3083—Birefringent or phase retarding elements
-
- 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
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors
- G02F1/13363—Birefringent elements, e.g. for optical compensation
-
- G—PHYSICS
- G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
- G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
- G09F9/00—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements
- G09F9/30—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements in which the desired character or characters are formed by combining individual elements
- G09F9/301—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements in which the desired character or characters are formed by combining individual elements flexible foldable or roll-able electronic displays, e.g. thin LCD, OLED
-
- 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
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K59/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic light-emitting element covered by group H10K50/00
- H10K59/80—Constructional details
- H10K59/8793—Arrangements for polarized light emission
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K77/00—Constructional details of devices covered by this subclass and not covered by groups H10K10/80, H10K30/80, H10K50/80 or H10K59/80
- H10K77/10—Substrates, e.g. flexible substrates
- H10K77/111—Flexible substrates
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K59/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic light-emitting element covered by group H10K50/00
- H10K59/80—Constructional details
- H10K59/875—Arrangements for extracting light from the devices
- H10K59/879—Arrangements for extracting light from the devices comprising refractive means, e.g. lenses
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
Definitions
- the present invention relates to a foldable display in which image distortion due to film deformation is unlikely to occur even when folded repeatedly.
- mobile terminal devices are becoming lighter, and mobile terminal devices such as smartphones are becoming widespread. While mobile terminal devices are required to have various functions, they are also required to be convenient. Therefore, popular mobile terminal devices need to have a small screen size of about 6 inches because they can be easily operated with one hand and are supposed to be stored in a pocket of clothes.
- tablet terminals with a screen size of 7 inches to 10 inches are expected to be used not only for video content and music, but also for business, drawing, reading, etc., and have high functionality.
- it cannot be operated with one hand is inferior in portability, and has a problem in convenience.
- Patent Document 1 a method of making it compact by connecting a plurality of displays has been proposed (see Patent Document 1), but since the bezel part remains, the image is cut off and the visibility is deteriorated. It has become a problem and is not widespread.
- the surface of the display could be protected with a non-flexible material such as glass, but in a foldable display, the foldable portion is used.
- a non-flexible material such as glass
- the foldable portion is used in the case of a one-sided display.
- the foldable display since the portion corresponding to a certain foldable portion is repeatedly folded, there is a problem that the film at the portion is deformed with time and the image displayed on the display is distorted.
- the foldable display uses films for various parts such as polarizing plates, retardation plates, touch panel base materials, base materials for display cells such as organic EL, and protective members on the back surface. , These films were also required to have durability against repeated folding.
- Patent Document 2 a method of partially changing the film thickness has been proposed (see Patent Document 2), but there is a problem of poor mass productivity.
- the present invention is intended to solve the problems of conventional display members as described above, is excellent in mass productivity, and does not cause distortion in the image displayed in the folded portion after being repeatedly folded. It seeks to provide a foldable display.
- the present invention has the following configuration.
- a foldable display having at least a surface protective film, a polarizer, and a retardation layer, and the surface protective film is a polyester film having a thickness of 10 to 80 ⁇ m that satisfies the following conditions.
- Refractive index in the bending direction is 1.590 to 1.620
- the refractive index in the direction of the folding part is 1.670 to 1.700.
- Refractive index in the thickness direction is 1.520 or less
- Density is 1.380 g / cm 3 or more (Here, the bending direction means a direction orthogonal to the folding portion when the polyester film is folded.) 2.
- the foldable display according to the first aspect wherein the polyester film has an elastic modulus in the bending direction of 2.7 GPa or less and an elastic modulus in the direction of the folding portion of 4.5 GPa or more. 3.
- the polyester film has a hard coat layer on at least one side thereof, and the hard coat layer is located at least on the surface of the foldable display. 4.
- the polyester film having a hard coat layer on at least one surface has a total light transmittance of 85% or more and a haze of 3% or less. 5.
- the foldable display of the present invention maintains mass productivity, and its surface protective film does not cause cracks in the foldable portion, does not cause deformation after repeated folding, and displays an image in the foldable portion of the display. It does not cause any disturbance.
- a mobile terminal device equipped with a foldable display using a surface protective film as described above provides a beautiful image, is rich in functionality, and is excellent in convenience such as portability.
- the display referred to in the present invention generally refers to a display device, and the types of displays include LCDs, organic EL displays, inorganic EL displays, LEDs, and FEDs, such as LCDs having a bendable structure.
- Organic EL and inorganic EL are preferable.
- organic EL and inorganic EL that can reduce the layer structure are particularly preferable, and organic EL having a wide color gamut is further preferable.
- the foldable display is a display in which one continuous display can be folded in half when carried. By folding, the size can be halved and portability can be improved.
- the bending radius of the foldable display is preferably 5 mm or less, more preferably 3 mm or less. If the bending radius is 5 mm or less, the thickness can be reduced in the folded state. It can be said that the smaller the bending radius is, the better, but the smaller the bending radius, the easier it is to make creases.
- the bending radius is preferably 0.1 mm or more, but may be 0.5 mm or more, or 1 mm or more. Even if the bending radius is 1 mm, it is possible to achieve a practically sufficient thinning when carrying.
- the bending radius when folded is for measuring the portion of reference numeral 11 in the schematic diagram of FIG. 1, and means the radius inside the folded portion when folded.
- the surface protective film described later may be located on the folded outer side or the inner side of the foldable display.
- the foldable display may be folded in three, folded in four, or further, and may be a retractable type called a rollable display, all of which fall within the scope of the foldable display according to the present invention.
- the polyester film for a foldable display used in the present invention and the hard coat film having a hard coat layer on at least one surface thereof may be used for any part as long as it is a constituent member of the foldable display.
- a typical configuration of a foldable display and a portion where the polyester film or the hard coat film in the present invention can be used will be described by taking an organic EL display as an example.
- the above-mentioned hard coat film for display may be simply referred to as a hard coat film in the present invention.
- An essential configuration of the foldable organic EL display is an organic EL module, but if necessary, a circularly polarizing plate, a touch panel module, a front surface protective film, a back surface protective film, and the like are provided.
- Organic EL module The general configuration of an organic EL module consists of an electrode / electron transport layer / light emitting layer / hole transport layer / transparent electrode.
- the foldable display of the present invention is provided with a surface protective film.
- the surface protective film has a role of preventing the circuits of the organic EL module and the touch panel module from being disconnected when an impact is applied to the display from above.
- the surface protective film includes a cover window incorporated in the outermost surface of the display and a replaceable after-sale film that can be attached and detached by the user himself.
- the polyester film and the hard coat film in the present invention are used. Can be suitably used as both of them.
- the polyester film used for these surface protection films preferably has a thickness of 10 to 80 ⁇ m and satisfies the following characteristics (1) to (4).
- Refractive index in the bending direction is 1.590 to 1.620
- the refractive index in the direction of the folding part is 1.670 to 1.700.
- Refractive index in the thickness direction is 1.520 or less
- Density is 1.380 g / cm 3 or more (Here, the bending direction means a direction orthogonal to the folding portion when the polyester film is folded.)
- the foldable display of the present invention does not need to use both the cover window and after surface protective films, and may have at least one surface protective film.
- the polyester film having the above-mentioned specific characteristics may be used for at least one of the cover window and the after-sale surface protective film, and is preferably used for both surface protective films.
- the polyester film used for the surface protection film may be a single-layer film made of one or more types of polyester resins, or when two or more types of polyesters are used, it may be a multi-layered film or a super-multilayer laminated film having a repeating structure. It may be a film.
- polyester resin used for the polyester film examples include polyethylene terephthalate, polybutylene terephthalate, polyethylene-2,6-naphthalate, and a polyester film composed of a copolymer containing the constituent components of these resins as main components. .. Of these, a stretched polyethylene terephthalate film is particularly preferable from the viewpoints of mechanical properties, heat resistance, transparency, price and the like.
- the dicarboxylic acid component of the polyester is, for example, an aliphatic dicarboxylic acid such as adipic acid or sebacic acid; terephthalic acid, isophthalic acid, phthalic acid, 2,6-naphthalenedicarboxylic acid.
- Aromatic dicarboxylic acids such as; polyfunctional carboxylic acids such as trimellitic acid and pyromellitic acid.
- glycol component examples include fatty acid glycols such as ethylene glycol, diethylene glycol, 1,4-butanediol, propylene glycol and neopentyl glycol; aromatic glycols such as p-xylene glycol; and 1,4-cyclohexanedimethanol.
- fatty acid glycols such as ethylene glycol, diethylene glycol, 1,4-butanediol, propylene glycol and neopentyl glycol
- aromatic glycols such as p-xylene glycol
- 1,4-cyclohexanedimethanol examples include fatty acid glycols such as ethylene glycol, diethylene glycol, 1,4-butanediol, propylene glycol and neopentyl glycol; aromatic glycols such as p-xylene glycol; and 1,4-cyclohexanedimethanol.
- Alicyclic glycols polyethylene glycols having an average molecular weight of 150 to
- the ultimate viscosity of at least one type of resin pellet is preferably in the range of 0.50 to 1.0 dl / g.
- the ultimate viscosity is 0.50 dl / g or more, the impact resistance of the obtained film is improved, and it is preferable that the internal circuit of the display is less likely to be broken due to an external impact.
- the ultimate viscosity is 1.00 dl / g or less, the filter pressure increase of the molten fluid does not become too large, and it is preferable that the film production can be operated stably.
- the thickness of the polyester film is preferably 10 to 80 ⁇ m, more preferably 25 to 75 ⁇ m.
- the thickness is 10 ⁇ m or more, the pencil hardness improving effect and the impact resistance improving effect are observed, and when the thickness is 80 ⁇ m or less, it is advantageous for weight reduction and also excellent in flexibility, workability and handleability.
- the surface of the polyester film may be smooth or have irregularities, but since it is used as a surface cover for displays, deterioration of optical characteristics due to irregularities is not preferable.
- the haze is preferably 3% or less, more preferably 2% or less, and most preferably 1% or less. When the haze is 3% or less, the visibility of the image can be improved. The smaller the lower limit of the haze, the better, but from the viewpoint of stable production, 0.1% or more is preferable, and 0.3% or more may be used.
- a polyester resin on the surface layer is used as a method of forming the unevenness in order to give a certain degree of slipperiness from the viewpoint of handling. It can be formed by blending particles into a layer or coating a coat layer containing particles during film formation.
- a known method can be adopted as a method of blending the particles in the polyester resin layer.
- it can be added at any stage in the production of polyester, but is preferably added as a slurry dispersed in ethylene glycol or the like at the stage of esterification or at the stage after the completion of the transesterification reaction and before the start of the polycondensation reaction. Then, the polycondensation reaction may proceed.
- the aggregate inorganic particles are homogeneously dispersed in a monomer solution that is a part of the polyester raw material, and then filtered, and the residue of the polyester raw material before the esterification reaction, during the esterification reaction, or after the esterification reaction is used.
- the method of addition is preferable. According to this method, since the monomer solution has a low viscosity, homogeneous dispersion of particles and high-precision filtration of the slurry can be easily performed, and when added to the rest of the raw material, the dispersibility of the particles is good, which is new. Aggregates are also unlikely to occur. From this point of view, it is particularly preferable to add it to the balance of the raw material in a low temperature state before the esterification reaction.
- the number of protrusions on the film surface can be further reduced by a method (masterbatch method) in which a polyester containing particles is obtained in advance and then the pellets and the pellets containing no particles are kneaded and extruded.
- the polyester film may contain various additives within a range that maintains a preferable range of total light transmittance.
- the additive include an antistatic agent, a UV absorber, and a stabilizer.
- the total light transmittance of the polyester film is preferably 85% or more, more preferably 87% or more. If the transmittance is 85% or more, sufficient visibility can be ensured. It can be said that the higher the total light transmittance of the polyester film, the better, but from the viewpoint of stable production, 99% or less is preferable, and 97% or less may be used.
- the maximum heat shrinkage rate of the polyester film after heat treatment at 150 ° C. for 30 minutes is preferably 6% or less, more preferably 5% or less. If the heat shrinkage rate is 6% or less, it is possible to suppress flat surface defects such as curl and waviness during HC processing. It can be said that the lower the heat shrinkage rate is, the better, but it is preferably -1% or more, and preferably 0% or more. A minus here means that it has expanded after heating, and even if it is less than -1%, a flat surface may be defective.
- the polyester film used in the present invention can give a sufficient pencil hardness to the hard coat layer when the hard coat layer is provided. It is considered that the pencil hardness of the conventional polyester film was lowered due to the deformation of the film in the thickness direction in the pencil hardness evaluation of the pencil hardness of the hard coat film after laminating the hard coat layer. ..
- a high hardness is achieved in the pencil hardness evaluation of the hard coat film by setting the pushing depth after the test force unloading in the film thickness direction by the dynamic ultrafine hardness tester described later to a specific range. be able to.
- the pushing depth after unloading the test force in the film thickness direction is preferably 1.5 ⁇ m or less, more preferably 1.4 ⁇ m or less, and even more preferably 1.3 ⁇ m or less.
- the pushing depth (final deformation amount under load) after unloading the test force is 1.5 ⁇ m or less, the film becomes thicker in the pencil hardness evaluation of the hard coat film after laminating the hard coat layer. It is hard to deform and the pencil hardness can be increased. If the pencil hardness of the hard coat film can be increased, scratches and dents are less likely to occur on the display surface, and the visibility of the display is improved. It can be said that the lower the pushing depth after the test force is unloaded, the better, but in terms of stable production and saturation of the effect, 0.3 ⁇ m or more is preferable, and further, 0.5 ⁇ m or more is preferable.
- the stretching ratio in the bending direction and the folding direction is adjusted to be high within a range in which the refractive index in the bending direction and the folding direction can be controlled within a preferable range. It is possible to exemplify the setting of conditions such as setting the stretching temperature in the bending direction and the folding direction low, and setting the heat fixing temperature high.
- the elastic modulus of the polyester film in the bending direction is preferably 2.7 GPa or less, more preferably 2.5 GPa or less, and further preferably 2.3 GPa or less.
- the elastic modulus in the folding direction is preferably 4.5 GPa or more, more preferably 4.6 GPa or more, and further preferably 4.7 GPa or more.
- the non-hard coat surface of the hard coat film in the present invention can be surface-treated to improve the adhesion with the adhesive or the hard coat layer.
- Examples of the surface treatment method include sandblasting, solvent treatment, and other unevenness treatment, corona discharge treatment, electron beam irradiation treatment, plasma treatment, ozone / ultraviolet irradiation treatment, flame treatment, chromic acid treatment, hot air treatment, and the like. Oxidation treatment and the like can be mentioned and can be used without particular limitation.
- the adhesiveness can be improved by an adhesiveness improving layer such as an easy adhesive layer.
- an adhesiveness improving layer such as an easy adhesive layer.
- acrylic resin, polyester resin, polyurethane resin, polyether resin and the like can be used without particular limitation, and can be formed by a general coating method, preferably a so-called in-line coat formulation.
- the above-mentioned polyester film has, for example, a polymerization step in which inorganic particles are homogeneously dispersed in a monomer solution that is a part of a polyester raw material, filtered, and then added to the rest of the polyester raw material to polymerize the polyester, and the polyester thereof. It can be produced through a film forming step of forming a base film by melt-extruding it into a sheet through a filter, cooling it, and then stretching it.
- PET polyethylene terephthalate
- the method for producing the polyester film will be described in detail with reference to an example in which polyethylene terephthalate (hereinafter, may be referred to as PET) pellets are used as a raw material for the base film, but the method is not limited thereto. Further, the number of layers is not limited, such as a single-layer structure or a multi-layer structure.
- the PET pellets are mixed and dried at a predetermined ratio, they are supplied to a known melt lamination extruder, extruded into a sheet from a slit-shaped die, and cooled and solidified on a casting roll to form an unstretched film. ..
- a known melt lamination extruder extruded into a sheet from a slit-shaped die, and cooled and solidified on a casting roll to form an unstretched film. ..
- one extruder is sufficient, but in the case of producing a multi-layer film, two or more extruders, two or more layers of manifolds or a merging block (for example, a merging having a square merging part).
- a block can be used to stack a plurality of film layers constituting each outermost layer, extrude two or more sheets from a base, and cool them with a casting roll to form an unstretched film.
- the filter medium used for high-precision filtration of the molten resin is not particularly limited, but the filter medium of the stainless sintered body is excellent in the removal performance of aggregates containing Si, Ti, Sb, Ge and Cu as main components and high melting point organic substances. Therefore, it is preferable.
- the filtered particle size (initial filtration efficiency 95%) of the filter medium is preferably 20 ⁇ m or less, and particularly preferably 15 ⁇ m or less. If the filtered particle size (initial filtration efficiency 95%) of the filter medium exceeds 20 ⁇ m, foreign matter having a size of 20 ⁇ m or more cannot be sufficiently removed. High-precision filtration of the molten resin using a filter medium having a filtered particle size (initial filtration efficiency of 95%) of 20 ⁇ m or less in the filter medium may reduce productivity, but a film with few protrusions due to coarse particles can be obtained. Preferred above.
- the refractive index of the polyester film in at least one of the longitudinal direction (mechanical flow direction) and the width direction is preferably 1.590 to 1.620, and more preferably 1.591 to 1. It is 600.
- the refractive index of the polyester film in the bending direction is preferably 1.590 to 1.620, and more preferably 1.591 to 1.600.
- the bending direction refers to a direction orthogonal to the folding portion (reference numeral 21) assumed in the application of the foldable display, as shown by reference numeral 22 on the polyester film (reference numeral 2) of FIG.
- the refractive index in at least one of the longitudinal direction and the width direction is 1.590 to 1.620, there is little deformation when repeatedly folded, and there is no risk of deteriorating the image quality of the foldable display, which is preferable.
- the refractive index is more preferably 1.591 to 1.600.
- the direction is preferably the above-mentioned bending direction. If it is 1.590 or more, there is no possibility that cracks will occur in the folding portion direction after the bending test described later, and of course, breakage will not occur, so that the visibility of the display can be kept good.
- the refractive index of the polyester film can be effectively adjusted by adjusting the stretching ratio and the stretching temperature. Further, a relaxation step in the stretching direction and multi-step stretching may be used to adjust the refractive index. When performing multi-stage stretching, it is preferable that the stretching ratio of the second and subsequent stages is higher than the stretching ratio of the first stage.
- the refractive index in at least one of the longitudinal direction (mechanical flow direction) and the width direction of the polyester film in the above range more preferably by controlling the refractive index in the bending direction in the above range, at the time of folding. Fatigue due to compressive stress applied to the inside of the fold can be reduced. Fatigue due to compressive stress is thought to occur mainly in the crystal part, and the smaller the number of crystals in the bending direction, the less fatigue. Therefore, it is considered that by lowering the refractive index, the amount of oriented crystals in the bending direction is reduced and compression fatigue is suppressed.
- the creep phenomenon caused by the tensile stress applied to the outside of the fold during folding can be suppressed by reducing the refractive index. Fatigue due to tensile stress is thought to occur mainly in the amorphous part, and the molecular chains are aligned and deformed due to the repeated stress. It can be inferred that the smaller the number of molecular chains aligned in the bending direction, the smaller the deformation due to alignment. Further, since fatigue due to tension can be suppressed when the number of amorphous portions is small, a high crystallinity, that is, a high density is preferable.
- the unstretched polyester sheet preferably has a draw ratio of 1.2 to 2.0 times in at least one of the longitudinal direction (mechanical flow direction) and the width direction, 1.7 to 2. 0 times is more preferable.
- the stretching direction is preferably the bending direction.
- a draw ratio of 1.2 times or more is preferable because there is no deformation in post-processing such as during hard coat coating, and a draw ratio of 2.0 times or less is preferable because uneven film thickness does not occur.
- the stretching temperature is preferably 75 to 120 ° C., more preferably 75 to 105 ° C.
- conventionally known means such as a hot air heating method, a roll heating method, and an infrared heating method can be adopted.
- the stretching temperature By setting the stretching temperature to 75 to 120 ° C., it is possible to prevent large thickness unevenness due to stretching at the above stretching ratio.
- the refractive index in the thickness direction can be reduced by stretching at a low temperature as much as possible within a range that does not cause large thickness unevenness as described above.
- the refractive index of the polyester film in the direction orthogonal to the direction in which the refractive index is 1.590 to 1.620 is preferably 1.670 to 1.700. That is, it is preferable that the refractive index in the direction orthogonal to the bending direction (direction of the folded portion) is 1.670 to 1.700.
- the refractive index in the direction orthogonal to the bending direction is 1.670 to 1.700.
- Examples of the method for adjusting the refractive index in the direction orthogonal to the bending direction include stretching ratio, stretching preheating temperature, stretching temperature, multi-stage stretching, and film relaxation.
- the draw ratio is preferably 4.0 to 6.0 times, more preferably 4.4 to 6.0 times.
- the stretching preheating temperature in the direction orthogonal to the bending direction is preferably 70 to 110 ° C.
- the film may be relaxed by 1 to 10% in either the machine flow direction (longitudinal direction) or the vertical direction (width direction).
- the refractive index in the thickness direction is preferably 1.520 or less. By setting it to 1.520 or less, even if the refractive index in the bending direction is designed to be low, it is possible to suppress a decrease in the hardness of the film surface, and it is possible to achieve both flexibility and surface hardness. .. By setting it to 1.520 or less, the pushing depth after unloading the test force in the thickness direction can be reduced, and the hardness of the film surface, particularly the pencil hardness of the hard coat film after laminating the hard coat layer can be improved. It is more preferably 1.515 or less, further preferably 1.510 or less, particularly preferably 1.505 or less, and most preferably 1.500 or less.
- the refractive index in the thickness direction is preferably low, but 1.3 or more is preferable in terms of stable production, and it may be 1.4 or more. Especially preferably, it is 1.410 or more. It can be said that the above range can be achieved by increasing the stretching ratio in both the bending direction and the folding direction, but the refractive index in the thickness direction is controlled after controlling the refractive index in the bending direction and the width direction within a preferable range. In order to do so, it is preferable to set the conditions while checking the balance of each process condition in the film forming process.
- the method of controlling the refractive index in the thickness direction within the above range is the stretching preheating temperature in the bending direction, the stretching temperature, the stretching ratio, the stretching preheating temperature in the direction of the folding portion, the stretching temperature, the multi-stage stretching, the high magnification stretching, or the heat fixing.
- the stretching preheating temperature in the bending direction is preferably 70 ° C. to 110 ° C.
- the stretching temperature in the bending direction is preferably 75 to 120 ° C.
- the draw ratio in the bending direction is preferably 1.2 to 2.0 times, more preferably 1.7 to 2.0 times.
- the stretching preheating temperature in the folding portion direction is also preferably 75 ° C. to 110 ° C.
- the stretching temperature is preferably 75 to 120 ° C.
- the draw ratio of the folded portion is preferably 4.0 to 6.0 times, more preferably 4.4 to 6.0 times.
- the refractive index in the thickness direction can be effectively reduced while maintaining or reducing the refractive index in the bending direction.
- multi-stage stretching may be used. In that case, it is preferable to make the stretching ratio of the second stage higher than the stretching ratio of the first stage because the refractive index can be effectively controlled.
- a method of stretching again after the crystallization step may be used.
- the heat fixing temperature is preferably 180 to 240 ° C.
- orientation crystallization in the stretching direction proceeds, and the refractive index in the thickness direction can be lowered.
- aromatics such as benzene rings in the molecular chain are oriented in the plane direction to suppress deformation due to stress applied in the thickness direction. It is thought that it has the effect of
- the density of the polyester film is preferably 1.380 g / cm 3 or more. More preferably, it is 1.383 g / cm 3 or more. By setting it to 1.380 g / cm 3 or more, the flexibility can be improved, and the film surface hardness, particularly the pencil hardness of the hard coat film after laminating the hard coat layer can be improved. The higher the density, the more preferable it is, and although it depends to some extent depending on the presence or absence of particles in the film, it is preferably 1.40 g / cm 3 or less. By setting the heat fixing temperature at the time of film formation to 180 to 240 ° C., crystallization can proceed and the density can be effectively increased.
- the bending direction of the polyester film corresponds to the longitudinal direction (machine flow direction). By doing so, it is easy to lower the refractive index in the bending direction at the biaxial stretching and improve the flexibility. That is, it is preferable to stretch the unstretched polyester sheet at a stretching ratio of 1.2 to 2.0 times, more preferably 1.7 to 2.0 times in the longitudinal direction to obtain a polyester film. Then, in the width direction, it can be said that it is preferable to stretch at a stretching ratio of 4.0 to 6.0 times, more preferably 4.4 to 6.0 times.
- the polyester film has (1) a refractive index in the bending direction of 1.590 to 1.620.
- the refractive index in the direction of the folding part is 1.670 to 1.700.
- the refractive index in the thickness direction is 1.520 or less and (4) the density is 1.380 g / cm 3 or more at the same time, but it is within the above-mentioned preferable production conditions.
- the stretching ratio in the bending direction is 1.4 times or less
- the stretching ratio in the folding portion direction is less than 4.4 times
- the heat fixing temperature is 220 ° C. or less.
- the stretching ratio in the bending direction may be increased to 1.7 times or more
- the stretching ratio in the direction of the folding portion may be increased to 4.4 times or more
- the heat fixing temperature may be increased to about 230 ° C.
- the above four characteristics can be satisfied at the same time by fine-tuning any of the conditions or a combination thereof, such as lowering the stretching temperature in the bending direction and / or the folding portion direction.
- any film-forming method such as stretching, relaxation, heat fixation, and surface treatment may be used, but the refractive index and density of the film are described above. It can be said that it is a particularly preferable aspect in the present invention to control the above in a preferable range.
- it is suitable for foldable displays, which can obtain better bending resistance and surface hardness than conventional films, especially high pencil hardness of hard coat film after laminating a hard coat layer.
- Polyester film can be provided.
- PET pellets are sufficiently vacuum-dried, then supplied to an extruder, melt-extruded into a sheet at about 280 ° C., cooled and solidified to form an unstretched PET sheet.
- the obtained unstretched sheet is stretched 1.2 to 2.0 times, more preferably 1.7 to 2.0 times in the longitudinal direction with a roll heated to 75 to 120 ° C. to obtain a uniaxially oriented PET film. ..
- the edge of the film is gripped with a clip and guided to a hot air zone heated to 75 to 120 ° C., and after drying, 4.0 to 6.0 times in the width direction, more preferably 4.4 to 6. Stretch 0 times.
- the heat treatment zone of 180 to 240 ° C. can be guided to perform the heat treatment for 1 to 60 seconds. In this heat treatment step, if necessary, a relaxation treatment of 0 to 10% may be performed in the width direction or the longitudinal direction.
- the ultimate viscosity of the polyester film is preferably in the range of 0.50 to 1.0 dl / g.
- the ultimate viscosity is 0.50 dl / g or more, the impact resistance is improved and the internal circuit of the display is less likely to be disconnected due to an external impact, which is preferable.
- the ultimate viscosity is 1.00 dl / g or less, the film production is stable and preferable without the increase in the filter pressure of the molten fluid becoming too large.
- the easy-adhesion layer in order to improve the adhesiveness between the polyester film and the hard coat layer, it is also preferable to laminate the easy-adhesion layer on the polyester film.
- a coating liquid for forming the easy-adhesive layer is applied to one or both sides of an unstretched or longitudinally uniaxially stretched film, heat-treated and dried as necessary, and further unstretched in at least one direction. It can be obtained by stretching to. Heat treatment can be performed even after biaxial stretching.
- the final coating amount of the easy-adhesion layer is preferably controlled to 0.005 to 0.20 g / m 2 . When the coating amount is 0.005 g / m 2 or more, adhesiveness is obtained, which is preferable. On the other hand, when the coating amount is 0.20 g / m 2 or less, blocking resistance is obtained, which is preferable.
- the resin contained in the coating liquid used for laminating the easy-adhesion layer for example, polyester resin, polyether polyurethane resin, polyester polyurethane resin, polycarbonate polyurethane resin, acrylic resin and the like can be used without particular limitation.
- the cross-linking agent contained in the coating liquid for forming an easy-adhesion layer include melamine compounds, isocyanate compounds, oxazoline compounds, epoxy compounds, and carbodiimide compounds. It is also possible to use a mixture of two or more of each. Due to the nature of the in-line coating, these are preferably coated with an aqueous coating liquid, and the resin or cross-linking agent is preferably a water-soluble or water-dispersible resin or compound.
- the average particle size of the fine particles is preferably 2 ⁇ m or less. When the average particle size of the particles exceeds 2 ⁇ m, the particles are likely to fall off from the easy-adhesion layer.
- the particles contained in the easy-adhesion layer include titanium oxide, barium sulfate, calcium carbonate, calcium sulfate, silica, alumina, talc, kaolin, clay, calcium phosphate, mica, hectrite, zirconia, tungsten oxide, and lithium fluoride.
- examples thereof include inorganic particles such as calcium fluoride and organic polymer particles such as styrene-based, acrylic-based, melamine-based, benzoguanamine-based, and silicone-based particles. These may be added to the easy-adhesion layer alone, or may be added in combination of two or more.
- a known method can be used in the same manner as the above-mentioned coating layer.
- the reverse roll coating method, the gravure coating method, the kiss coating method, the roll brush method, the spray coating method, the air knife coating method, the wire bar coating method, the pipe doctor method, etc. can be mentioned, and these methods can be used alone. Alternatively, it can be performed in combination.
- the polyester film preferably has a hard coat layer on at least one side thereof.
- the hard coat layer is preferably located on the surface side of the display on the polyester film and used in the display.
- the hard coat layer may be provided on both sides in order to suppress curl.
- acrylic type, siloxane type, inorganic hybrid type, urethane acrylate type, polyester acrylate type, epoxy type and the like can be used without particular limitation. Further, two or more kinds of materials can be mixed and used, and particles such as an inorganic filler and an organic filler can be added.
- the film thickness of the hard coat layer is preferably 1 to 50 ⁇ m. When it is 1 ⁇ m or more, it is sufficiently cured and the pencil hardness becomes high, which is preferable. Further, by setting the thickness to 50 ⁇ m or less, curling due to curing shrinkage of the hard coat can be suppressed, and the handleability of the film can be improved.
- a Meyer bar, a gravure coater, a die coater, a knife coater and the like can be used without particular limitation, and can be appropriately selected depending on the viscosity and the film thickness.
- a curing method of the hard coat layer energy rays such as ultraviolet rays and electron beams and a curing method by heat can be used, and in order to reduce damage to the film, a curing method using ultraviolet rays and electron beams is preferable.
- the pencil hardness of the hard coat layer is preferably 3H or higher, and more preferably 4H or higher. If the pencil has a hardness of 3H or more, it will not be easily scratched and the visibility will not be deteriorated. Generally, it is preferable that the pencil hardness of the hard coat layer is high, but it may be 9H or less, 8H or less, or 6H or less without any problem in practical use.
- the hard coat layer in the present invention can be used for the purpose of increasing the pencil hardness of the surface as described above to protect the display, and preferably has a high transmittance.
- the transmittance of the hard coat film is preferably 85% or more, more preferably 88% or more. When the transmittance is 87% or more, sufficient visibility can be obtained. Generally, the higher the total light transmittance of the hard coat film, the more preferable, but from the viewpoint of stable production, it is preferably 99% or less, and may be 97% or less.
- the haze of the hard coat film is generally preferably low, preferably 3% or less. The haze of the hard coat film is more preferably 2% or less, and most preferably 1% or less. When the haze is 3% or less, the visibility of the image can be improved. Generally, the lower the haze, the better, but from the viewpoint of stable production, 0.1% or more is preferable, and 0.3% or more may be used.
- the hard coat layer may have other functions added to it.
- a hard coat layer to which functionality such as an antiglare layer having a certain pencil hardness as described above, an antiglare antireflection layer, an antireflection layer, a low reflection layer, an anti-scratch layer, and an anti-static layer is added. Is also preferably applied in the present invention.
- the polyester film as described above as the surface protective film.
- the hard coat layer is preferably arranged on the visual side.
- the foldable display of the present invention has a polarizer.
- polarizers are provided on both sides of the liquid crystal cell, and in an EL display or the like, a circular polarizing element (a laminate of a polarizer and a 1 / 4 ⁇ layer) for reducing reflected light from the internal structure is used.
- the polarizer is used as a polarizing plate having a laminated structure of a polarizer and a polarizer protective film for protecting the polarizer.
- a polarizing element and a retardation layer including a polarizing element protective film and a polarizer protective coating when they are included
- a dichroic dye such as iodine is adsorbed on an alignment film made of a polarizer (also referred to as a polarizing film) polyvinyl alcohol (PVA) resin that can be used in the present invention.
- a polarizer also referred to as a polarizing film
- PVA polyvinyl alcohol
- a production method including a step of dyeing a single layer of a PVA-based resin and a step of stretching.
- a manufacturing method including a step of providing a PVA-based resin layer on a stretching resin base material by coating or the like and stretching the laminated body and a step of dyeing the laminated body can be mentioned.
- this production method even if the PVA-based resin layer is thin, it can be stretched without any trouble such as breakage due to stretching because it is supported by the resin base material for stretching, which is more preferable.
- a manufacturing method including a step of stretching in a boric acid aqueous solution is preferable because it can be stretched at a high magnification and the polarization performance can be improved, and aerial auxiliary stretching is performed before stretching in a boric acid aqueous solution.
- a production method including the step of performing the above is preferable.
- a manufacturing method in which the PVA-based resin layer and the resin base material for stretching are stretched in a laminated state, the PVA-based resin layer is excessively dyed, and then decolorized is also preferable.
- the polarizer produced by these methods can be preferably used in the present invention. It is preferable that the polarizer obtained by the base material layer stretching method is transferred to a polarizer protective film or a retardation film. Further, when the thickness is further reduced without using the polarizer protective film, it is preferable to transfer the image to an image display cell, a touch panel, or a surface protective film.
- the thickness of the polarizer is preferably 12 ⁇ m or less, more preferably 9 ⁇ m or less, still more preferably 1 to 8 ⁇ m, and particularly preferably 3 to 6 ⁇ m. If it is within the above range, it will be a preferable embodiment without inhibiting bending.
- a polarizer using a liquid crystal compound can also be preferably used because it is a thin polarizing element and the absorption axis direction of the polarizer can be provided in any direction.
- Polarizers using liquid crystal compounds are coated on a film such as a polarizer protective film with a polymerizable liquid crystal compound and an organic dichroic dye oriented, or a coating liquid containing a liquid crystal dichroic dye. It can then be dried, oriented, lightly or heat cured to form a polarizer.
- Examples of the method for orienting the liquid crystal polarizer include a method of rubbing the surface of the film to which the coating liquid is applied, and a method of irradiating the coating liquid with polarized ultraviolet rays to cure the liquid crystal compound while aligning it. ..
- the preferred polymerizable liquid crystal compound include, for example, JP-A-2002-308832, JP-A-2007-16207, JP-A-2015-163596, JP-A-2007-510946, JP-A-2013-114131. Gazette, WO2005 / 045485, Lub et al. Recl. Trav. Chim. Examples thereof include those described in Pays-Bas, 115, 321-328 (1996) and the like.
- Preferred dichroic dyes include dyes described in JP-A-2007-126628, JP-A-2010-168570, JP-A-2013-101328, JP-A-2013-210624 and the like.
- an orientation control layer before providing the liquid crystal polarizer.
- an orientation control layer -A method of applying polyvinyl alcohol and its derivative, polyimide and its derivative, acrylic resin, polysiloxane derivative, etc. and rubbing the surface thereof to form an alignment layer (rubbing orientation control layer).
- -A coating liquid containing a polymer or monomer having a photoreactive group such as a cinnamoyl group and a chalcone group and a solvent is applied to a base film, and the orientation is cured by irradiating the substrate film with polarized ultraviolet rays to cure the orientation layer (photoalignment control layer). ) How to And so on.
- photo-orientation control layers for example, JP-A-2006-285197, JP-A-2007-76839, JP-A-2007-138138, JP-A-2007-94071, JP-A-2007-121721, for example. , JP-A-2007-140465, JP-A-2007-156439, JP-A-2007-133184, JP-A-2009-109831, JP-A-2002-229039, JP-A-2002-265541, Open 2002-317013, Japanese Patent Application Laid-Open No. 2003-520878, Japanese Patent Application Laid-Open No. 2004-522220, Japanese Patent Application Laid-Open No. 2013-33248, Japanese Patent Application Laid-Open No. 2015-7702, Japanese Patent Application Laid-Open No. 2015-129210, etc.
- An orientation control layer can be mentioned.
- the liquid crystal polarizer is provided by coating on a polarizer protective film, a retardation film, or the like, and the liquid crystal polarizer is provided on the releasable base material according to the above method and transferred. It may be provided. Further, when the thickness is further reduced without using the polarizer protective film, it is preferable to transfer the image to an image display cell, a touch panel, or a surface protective film.
- the thickness of these liquid crystal polarizers is preferably 0.1 to 7 ⁇ m, more preferably 0.3 to 5 ⁇ m, and particularly preferably 0.5 to 3 ⁇ m.
- the foldable display of the present invention preferably has a retardation layer (also referred to as a retardation film) between the polarizer and the image display cell.
- the retardation layer plays a role of optical compensation that corrects the deviation of the phase difference of the oblique light due to the liquid crystal compound of the cell and reduces the color shift in the case of oblique light. have.
- the image display cell is an EL cell or the like, it has a role as a 1 / 4 ⁇ layer of a circularly polarizing plate.
- the retardation layer is a single layer or a combination of a plurality of retardation layers obtained by stretching a polymer film (phase difference film) or oriented and immobilizing a liquid crystal compound (liquid crystal retardation layer). Can be used.
- Examples of the retardation layer produced by orienting the polymer film by stretching it include polycycloolefin (COP) film, polycarbonate (PC) film, polypropylene (PP) film, acrylic resin (Ac) film, and triacetyl cellulose. (TAC) film and the like.
- COP polycycloolefin
- PC polycarbonate
- PP polypropylene
- Ac acrylic resin
- TAC triacetyl cellulose.
- any suitable stretching method can be adopted depending on the intended purpose.
- the stretching method suitable for the present invention include longitudinal uniaxial stretching, horizontal uniaxial stretching, longitudinal / horizontal simultaneous biaxial stretching, and longitudinal / horizontal sequential biaxial stretching.
- any suitable stretching machine such as a roll stretching machine, a tenter stretching machine, or the like can be used.
- the stretching is preferably carried out by heating the polymer film to a temperature equal to or higher than the glass transition temperature of the resin and lower than the melting point, preferably in the range of the glass transition temperature + 10 to 80 ° C. It is preferable to perform preheating so that the polymer film becomes a stretchable temperature before the start of stretching, and the temperature may be continuously changed in the stretching step. The process may be divided into one time or two or more times.
- the stretching direction is preferably the film width direction (TD direction) or the diagonal direction.
- Diagonal stretching involves continuously delivering the unstretched resin film in the longitudinal direction and continuously stretching the unstretched resin film in a direction forming an angle in the specific range with respect to the width direction. As a result, it is possible to obtain a long retardation film in which the angle (orientation angle ⁇ ) formed by the width direction of the film and the slow phase axis is within the specific range.
- the retardation layer is a retardation layer made of a liquid crystal compound (liquid crystal retardation layer).
- liquid crystal compound include a rod-shaped liquid crystal compound, a polymer-like liquid crystal compound, and a liquid crystal compound having a reactive functional group.
- the liquid crystal compound is preferably a polymerizable liquid crystal compound having a polymerizable group such as a double bond in terms of being able to fix the orientation state. Further, as the liquid crystal compound, a rod-shaped liquid crystal compound, a discotic liquid crystal compound, or the like can be used.
- rod-shaped liquid crystal compound examples include JP-A-2002-030042, JP-A-2004-204190, JP-A-2005-263789, JP-A-2007-119415, JP-A-2007-186430, and special publications. Examples thereof include rod-shaped liquid crystal compounds having a polymerizable group described in Kaihei 11-513360.
- NPh is a 2,6-naphthylene group
- rod-shaped liquid crystal compounds are commercially available from BASF as LC242 and the like, and they can be used.
- a plurality of types of these rod-shaped liquid crystal compounds may be used in combination at any ratio.
- discotic liquid crystal compound examples include benzene derivatives, tolucene derivatives, cyclohexane derivatives, azacrowne-based macrocycles, and phenylacetylene-based macrocycles.
- Various discotic liquid crystal compounds are described in Japanese Patent Application Laid-Open No. 2001-155866, and these are preferably used.
- the method of providing the liquid crystal retardation layer may be a method of coating the composition (paint) for the retardation layer on the polarizer, and the retardation layer (lamination for transfer of the retardation layer) on the releasable substrate may be used. It may be a method of transferring the body) to a polarizer. Further, it may be coated or transferred to a film (base film) such as a COP film, a PC film, a PP film, an Ac film, or a TAC film. Further, a retardation layer is provided on the polarizer on the substrate by the substrate lamination and stretching method, or a retardation layer is provided on the liquid crystal polarizer on the releasable substrate, and this is transferred to the substrate film. May be good.
- the composition for the retardation layer may contain a solvent, a polymerization initiator, a sensitizer, a polymerization inhibitor, a leveling agent, a polymerizable non-liquid crystal compound, a cross-linking agent and the like.
- the same method as the above-mentioned orientation of the liquid layer polarizer can be adopted. That is, a method of applying a composition for a retardation layer and irradiating it with polarized ultraviolet rays, a method of rubbing a polarizer, a releasable substrate, a substrate film, and the like, a method of providing an orientation control layer, and the like can be mentioned.
- a plurality of retardation layers may be provided.
- a plurality of retardation layers may be transferred by using a laminate having a plurality of retardation layers on one releasable substrate.
- a plurality of laminates having one retardation layer on one releasable substrate may be used to transfer the retardation layers one by one.
- the coating method and the transfer method may be combined.
- the liquid crystal retardation layer may be coated or transferred to a retardation film such as a COP film, a PC film, a PP film, an Ac film, or a TAC film.
- the retardation layer in the circular polarizing plate is preferably a 1 / 4 ⁇ layer.
- the 1 / 4 ⁇ layer will be described in detail.
- the 1 / 4 ⁇ layer converts the linearly polarized light that has passed through the polarizer to circularly polarized light, and the circularly polarized light reflected by the wiring in the EL cell, the glass substrate touch panel, etc. is converted to linearly polarized light that is 90 degrees out of alignment with the incident linearly polarized light. Can be converted.
- the 1 / 4 ⁇ layer may be a single 1 / 4 ⁇ layer, or may be a composite 1 / 4 ⁇ layer of a 1 / 4 ⁇ layer and a 1 / 2 ⁇ layer.
- the 1 / 4 ⁇ layer may be provided with a C plate layer or the like.
- 1 / 4 ⁇ layer is a layer capable of imparting a phase difference of 1 / 4 ⁇ including not only a single 1 / 4 ⁇ layer but also a composite 1 / 4 ⁇ layer and a retardation layer such as a C plate layer. It is a general term for.
- the in-plane retardation of the 1 / 4 ⁇ layer is preferably 100 to 180 nm, more preferably 120 to 150 nm.
- the in-plane retardation of the 1 / 2 ⁇ layer is preferably 200 to 360 nm, more preferably 240 to 300 nm.
- the angle formed by the orientation axis (slow phase axis) of the 1 / 4 ⁇ layer and the transmission axis of the polarizer is preferably 35 to 55 degrees, more preferably 40 to 50 degrees, and further. It is preferably 42 to 48 degrees.
- the orientation axis (slow phase axis) of each retardation layer is arranged at an angle such that the phase difference between the two layers is 1 / 4 ⁇ .
- the angle ( ⁇ ) formed by the orientation axis (slow phase axis) of the 1 / 2 ⁇ layer and the transmission axis of the polarizer is preferably 5 to 20 degrees, more preferably 7 to 17 degrees.
- the angle formed by the orientation axis (slow phase axis) of the 1 / 2 ⁇ layer and the orientation axis (slow phase axis) of the 1 / 4 ⁇ layer is preferably in the range of 2 ⁇ + 45 degrees ⁇ 10 degrees, more preferably in the range of 2 ⁇ + 45 degrees ⁇ 5 degrees. It is more preferably in the range of 2 ⁇ + 45 degrees ⁇ 3 degrees.
- each of the retardation layers used in the present invention is preferably 20 ⁇ m or less, more preferably 10 ⁇ m or less, still more preferably 1 to 9 ⁇ m, and particularly preferably 3 to 8 ⁇ m.
- the thickness of the retardation layer is preferably 1 to 5 ⁇ m, more preferably 1.5 to 4 ⁇ m. If it is within the above range, it will be a preferable embodiment without inhibiting bending.
- a polarizer protective film is laminated on the polarizer.
- a film such as a COP film, a PC film, a PP film, an Ac film, a TAC film, or a polyester film can be used. Of these, TAC film and polyester film are preferable in terms of folding durability.
- the thickness of the polarizer protective film is preferably 5 to 60 ⁇ m, more preferably 10. It is about 40 ⁇ m, more preferably 10 to 30 ⁇ m, and a surface treatment layer such as an anti-glare layer or an antireflection layer can be appropriately provided. If it is within the above range, it will be a preferable embodiment without inhibiting bending.
- the polarizer protective film may be provided on both sides of the polarizer, or may be provided on only one side. When the polarizer protective film is provided on only one side of the polarizer, it is preferable that the retardation layer is provided on the opposite surface. In this case, the retardation layer of the polymer film may be used to have the function of the polarizer protective layer.
- Preferred specific configurations include the following configurations. (1a) Polarizer Protective Film / Polarizer / Phase Difference Film (1b) Polarizer Protective Film / Polarizer / Liquid Liquid Phase Difference Layer / Phase Difference Film (1c) Polarizer Protective Film / Polarizer / Liquid Liquid Phase Difference Layer / ( Base film (of retardation layer)
- polarizer protective coat It is also preferable to apply a protective coating (polarizer protective coating) to the polarizer instead of the polarizer protective film.
- polarizer protective coat those used as a coating agent for a film such as polyester, polyamide, polyurethane, acrylic, and amino resin are preferable. Further reduction in thickness is possible by using a polarizer protective coat instead of the polarizer protective film.
- the polarizer protective coat may be provided not only by direct coating but also by transfer. If the polarizer or the retardation layer transfers a liquid crystal compound, the protective coat layer is placed on the releasable substrate. And a polarizer or a retardation layer may be provided and transferred as a unit.
- the thickness of the polarizer protective coat is preferably 1 to 30 ⁇ m, more preferably 3 to 20 ⁇ m, and even more preferably 5 to 10 ⁇ m. Both sides of the polarizer may be protective coatings, one side of the polarizer may be a polarizer protective film and the other side may be a polarizer protective coating, or both sides of the polarizer may be a polarizer protective coating. Good. Preferred specific configurations include the following configurations.
- Polarizer Protective Coat / Polarizer / Polarizer Protective Coat / Phase Difference Film (4a) Polarizer Protective Coat / Polarizer / Polarizer Protective Coat / Phase Difference Film (4b) Polarizer Protective Coat / Polarizer / Polarizer Protective Coat / Liquid Crystal Phase Difference Layer / Phase Difference Film (4c) Polarizer Protective Coat / Polarizer / Polarizer protective coating / Liquid crystal retardation layer / Base film (of retardation layer)
- a protective coat may be provided on the retardation layer instead of the base film (of the retardation layer) in c of the above-mentioned specific laminated configurations 1 to 4.
- the material and method of providing the retardation layer protective coat are the same as those of the polarizer protective coat.
- an adhesive layer and an adhesive layer exist between the layers except when the liquid crystal polarizer or the liquid crystal retardation layer is directly coated, but they are omitted here.
- the above-mentioned polarizing element is preferably laminated with another member (image display cell, touch panel, surface protective film, etc.) via an adhesive layer.
- the pressure-sensitive adhesive may be directly provided on the polarizer or the liquid crystal retardation layer and bonded without providing the polarizer protective coating or the retardation layer protection coating on the surface of the other member of the polarizer.
- the material of the adhesive layer is not particularly limited, and for example, rubber-based adhesive, acrylic-based adhesive, silicone-based adhesive, urethane-based adhesive, vinyl alkyl ether-based adhesive, polyvinyl alcohol-based adhesive, and polyvinylpyrrolidone-based adhesive.
- examples thereof include agents, polyacrylamide-based adhesives, and cellulose-based adhesives.
- an acrylic pressure-sensitive adhesive is preferable from the viewpoint of transparency, weather resistance, heat resistance, and the like.
- the adhesive layer include a method of providing the polarizing element by coating, a method of using a commercially available optical adhesive sheet, and the like.
- FIG. 1 is a schematic view for showing the bending radius when the foldable display is folded, and in consideration of the case where the polyester film is arranged on the inner surface of the folded form, FIG.
- the bending test is performed as a model assuming that the location of reference numeral 11 is set to 1.5 mm. After the bending treatment was completed, the sample was placed on a flat surface with the inside of the bending facing down, and visually observed. ⁇ : No cracks or deformation can be confirmed in the sample. ⁇ : The sample has cracks or creases, and when placed horizontally, the maximum height is 5 mm or more.
- FIG. 1 is a schematic view for showing the bending radius when the foldable display is folded, and in consideration of the case where the polyester film is arranged on the inner surface of the folded form, FIG.
- the bending test is performed as a model assuming that the location of reference numeral 11 is set to 0.5 mm.
- the film surface on the outside of the bent portion was observed at 700 times that of a digital microscope (RH8800 manufactured by HIROX), and the presence or absence of wrinkles (cracks) was observed.
- Refractive index In accordance with JIS K 7142: 2008 "Method for measuring the refractive index of plastics (Method A)", an Abbe refractive index meter (manufactured by Atago, NAR-4T, measurement wavelength 589 nm) is used in the longitudinal direction. The refractive index, the refractive index in the width direction, and the refractive index in the thickness direction were determined.
- Pencil hardness Using the pencil hardness of the hard coat film as a sample, the measurement was performed at a load of 750 g and a speed of 1.0 mm / s according to JIS K 5600-5-4: 1999. In the present invention, 3H or more was regarded as acceptable.
- Total light transmittance was measured using a haze haze meter (NDH5000, manufactured by Nippon Denshoku Kogyo Co., Ltd.).
- Density The density was measured according to a method (density gradient tube method) conforming to JIS K 7112: 1999. (Unit: g / cm 3 ).
- Test force Pushing depth after unloading The sample is cut into a square of about 2 cm, and the opposite side of the measurement surface is glued (Cemedine (registered trademark) high) on the micro cover glass 18 x 18 mm (manufactured by Matsunami Glass Co., Ltd.). It was fixed at Super 30). After sticking and fixing, leave it at room temperature for 12 hours or more, and then use a dynamic ultra-micro hardness tester "DUH-211" (manufactured by Shimadzu Corporation) under the following conditions to push in depth after unloading the test force ( ⁇ m) was measured.
- a dynamic ultra-micro hardness tester "DUH-211" manufactured by Shimadzu Corporation
- Test mode Load-unload test Indenter used: Ridge angle 115 degrees, triangular pyramid indenter Indenter modulus: 1.140 ⁇ 10 6 N / mm 2 Indenter Poisson's ratio: 0.07 Test power: 50mN Load speed: 4.44 mN / sec Load holding time: 2 sec Unloading retention time: 0 sec
- the sample film is cut and measured separately in both the bending direction and the folding direction so that the vertical and horizontal directions are different, and the data in the direction in which the measured value is large is defined as the maximum heat shrinkage rate (%).
- esterification reaction device a continuous esterification reaction device consisting of a three-stage complete mixing tank having a stirrer, a splitter, a raw material charging port and a product extraction port is used, the TPA is 2 tons / hr, and the EG is TPA1.
- the amount of antimony trioxide is 2 mol per mol
- the amount of Sb atom is 160 ppm with respect to the produced PET, and these slurries are continuously supplied to the first esterification reaction can of the esterification reaction apparatus at normal pressure.
- the reaction was carried out at 255 ° C. with an average residence time of 4 hours.
- the reaction product in the first esterification reaction can is continuously taken out of the system and supplied to the second esterification reaction can, and distilled from the first esterification reaction can in the second esterification reaction can.
- 8% by mass of the EG to be produced is supplied to the produced polymer (produced PET), and an EG solution containing magnesium acetate in an amount of 65 ppm of Mg atoms with respect to the produced PET and 20 ppm of P atoms with respect to the produced PET.
- An EG solution containing an amount of TMPA was added, and the reaction was carried out at normal pressure at an average residence time of 1.5 hours and at 260 ° C.
- the reaction product in the second esterification reaction can is continuously taken out of the system and supplied to the third esterification reaction can, and further contains TMPA in an amount of 20 ppm of P atoms with respect to the produced PET.
- An EG solution was added, and the reaction was carried out at normal pressure at an average residence time of 0.5 hours and at 260 ° C.
- the esterification reaction product produced in the third esterification reaction can is continuously supplied to a three-stage continuous polycondensation reaction apparatus to perform polycondensation, and further, a filter medium of a stainless sintered body (nominal filtration accuracy of 5 ⁇ m). The particles were filtered through 90% of the particles) to obtain polyethylene terephthalate pellets (a) having an ultimate viscosity of 0.62 dl / g.
- reaction solution reached a predetermined amine equivalent.
- reaction solution was cooled to 40 ° C., and then 9.03 parts by mass of triethylamine was added to obtain a polyurethane prepolymer D solution.
- 450 g of water was added to a reaction vessel equipped with a homodisper capable of high-speed stirring, adjusted to 25 ° C., and while stirring and mixing at 2000 min-1, the isocyanate group-terminated prepolymer was added and water dispersed. did. Then, under reduced pressure, acetonitrile and a part of water were removed to prepare a water-soluble polyurethane resin (A) having a solid content of 35% by mass.
- Polyethylene terephthalate pellet (a) was supplied to the extruder and melted at 285 ° C. This polymer is filtered through a stainless sintered filter medium (nominal filtration accuracy of 10 ⁇ m particles 95% cut), extruded into a sheet from the base, and then cast into a casting drum with a surface temperature of 30 ° C. using an electrostatic application casting method. They were brought into contact and cooled and solidified to form an unstretched film. This unstretched film was uniformly heated to 75 ° C. using a heating roll and heated to 85 ° C. with a non-contact heater to perform 1.4 times roll stretching (longitudinal stretching).
- the above-mentioned coating liquid for forming an easy-adhesive layer was applied to both sides of the obtained uniaxially stretched film by a roll coating method, and then dried at 80 ° C. for 20 seconds.
- the final (after biaxial stretching) coating amount after drying was adjusted to 0.06 g / m 2 . Then, it is guided to a tenter, preheated at 105 ° C., laterally stretched 4.0 times at 95 ° C., fixed in width, heat-fixed at 230 ° C. for 5 seconds, and further relaxed by 4% in the width direction at 180 ° C.
- a polyester film 1 having a thickness of 50 ⁇ m was obtained.
- polyester film 2-3 A polyester film and a hard coat film were obtained in the same manner as the polyester film 1 except that the draw ratio was changed in the longitudinal direction shown in Table 1.
- polyester film 4 A polyester film and a hard coat film were obtained in the same manner as the polyester film 1 except that the draw ratio in the width direction was changed to 4.4 times and the heat fixing temperature was changed to 220 ° C.
- polyester film 5-6 A polyester film and a hard coat film were obtained in the same manner as the polyester film 4 except that the draw ratio was changed in the longitudinal direction as shown in Table 1.
- polyester film 7 A polyester film and a hard coat film were obtained in the same manner as the polyester film 1 except that the draw ratio in the width direction was changed to 5.5 times and the heat fixing temperature was changed to 190 ° C.
- polyester film 8-9 A polyester film and a hard coat film were obtained in the same manner as the polyester film 7 except that the draw ratio was changed in the longitudinal direction as shown in Table 1.
- polyester film 10 In the manufacturing process of the polyester film 5, a polyester film and a hard coat film were obtained in the same manner as the polyester film 5 except that the polyester film 5 was stretched in the longitudinal direction and then subjected to a relaxation heat treatment at 100 ° C. by 10%.
- polyester film 11 In the manufacturing process of the polyester film 5, a polyester film and a hard coat film were obtained in the same manner as in Example 5 except that the clip was opened at 200 ° C. after heat fixing and relaxation heat treatment was performed in the longitudinal direction and the width direction. In the longitudinal direction, the tenter speed and the take-up roll speed were adjusted so that the relaxation rate was 3%. Relaxation in the width direction was left free.
- polyester film 12 A polyester film and a hard coat film were obtained in the same manner as the polyester film 1 except that the temperature at the time of stretching in the longitudinal direction was changed to 75 ° C. and the heat fixing temperature was changed to 220 ° C.
- polyester film 13 The temperature at the time of stretching in the longitudinal direction was changed to 75 ° C., the stretching ratio was changed to 1.2 times, and then the stretching ratio was changed to 5.0 times in the width direction, and the same was applied to the polyester film 1. A polyester film and a hard coat film were obtained.
- polyester film 14 The stretching in the longitudinal direction of the polyester film 3 was set to two-step stretching, the stretching ratio of the first step was set to 1.2 times, and the stretching ratio of the second step was set to 1.67 times in the same manner as the polyester film 3. A polyester film and a hard coat film were obtained. The total stretching ratio in the longitudinal direction is about 2.0 times.
- polyester film 15 A polyester film and a hard coat film were obtained in the same manner as the polyester film 5 except that the preheating temperature at the time of stretching in the width direction was changed to 95 ° C. and the heat fixing temperature was changed to 190 ° C.
- polyester film 16 The stretching in the width direction of the polyester film 2 was set to two-step stretching, the stretching ratio of the first step was 1.5 times, the stretching ratio of the second step was 4.0 times, and the heat fixing temperature was changed to 190 ° C. A polyester film and a hard coat film were obtained in the same manner as the polyester film 2. The total stretching ratio in the width direction is 6.0 times.
- polyester film 17-18 A polyester film and a hard coat film were obtained in the same manner as the polyester film 2 except that the thickness was changed as shown in Table 2.
- polyester film 19 A polyester film and a hard coat film were obtained in the same manner as the polyester film 1 except that the relaxation heat treatment in the width direction was not performed in the production process of the polyester film 1.
- polyester film 20 After preparing an unstretched film in the same manner as the polyester film 1, the unstretched film was preheated with a tenter at 75 ° C. and laterally stretched 1.4 times at 85 ° C. The above-mentioned coating liquid for forming an easy-adhesive layer was applied to both sides of the obtained uniaxially stretched film by a roll coating method, and then dried at 80 ° C. for 20 seconds. The final (after biaxial stretching) coating amount after drying was adjusted to 0.06 g / m 2 . Uniformly heat to 105 ° C. using a heating roll and heat to 95 ° C. with a non-contact heater. Roll stretching (longitudinal stretching) was performed 4.0 times. The width was fixed and heat-fixed at 230 ° C. for 5 seconds to obtain a polyester film having a thickness of 50 ⁇ m and a hard coat film.
- polyester film 21 A polyester film and a hard coat film were obtained in the same manner as the polyester film 1 except that the film was stretched only in the width direction and stretched in the lateral uniaxial direction without stretching in the longitudinal direction.
- polyester film 22 A polyester film and a hard coat film were obtained in the same manner as the polyester film 7, except that the film was stretched only in the width direction and stretched in the lateral uniaxial direction without stretching in the longitudinal direction.
- polyester film 23-27 A polyester film and a hard coat film were obtained in the same manner as in the polyester film 1 except that the heat fixing temperature was changed to 220 ° C. and the PET pellets and thicknesses shown in Tables 1 and 2 were set. Comparative Examples 3 to 7 are a combination of each condition level which is not the best in the condition range in which the heat fixing temperature is lower than that of Example 1 and the stretching ratio in the longitudinal direction and the width direction is preferable as described above. As described in No. 2, the refractive index in the thickness direction increased, the pushing depth after unloading the test force was large, and the pencil hardness after laminating the hard coat layer was smaller than in each example.
- polyester film 28 A polyester film and a hard coat film were obtained in the same manner as the polyester film 1 except that the stretching ratio in the longitudinal direction was changed to 2.7 times and the heat fixing temperature was changed to 220 ° C.
- polyester film 29 A polyester film and a hard coat film were obtained in the same manner as the polyester film 1 except that the draw ratio in the longitudinal direction was changed to 3.4 times.
- polyester film 30 A polyester film and a hard coat film were obtained in the same manner as the polyester film 4 except that the heat fixing temperature was changed to 100 ° C.
- polyester film 31 A polyester film and a hard coat film were obtained in the same manner as the polyester film 13 except that the stretching temperature in the longitudinal direction was changed to 130 ° C.
- polyester film 32 A polyester film and a hard coat film were obtained in the same manner as the polyester film 1 except that the preheating temperature in the width direction was changed to 120 ° C.
- polyester film 33 A polyethylene terephthalate film having a thickness of 50 ⁇ m was obtained in the same manner as in the polyester film 1, and then a hard coat film coated with the hard coat coating liquid b was obtained.
- Example, comparative example (Creation and evaluation of foldable displays with surface protective film, polarizer, retardation layer) Using the above polyester film as a surface protective film, a model of a foldable display having a polarizer and a retardation layer was created.
- thermoplastic resin base material polyethylene terephthalate having an ultimate viscosity of 0.62 dl / d was melted and kneaded with an extruder and then extruded into a sheet on a cooling roll to prepare an unstretched film having a thickness of 100 ⁇ m.
- An aqueous solution of polyvinyl alcohol having a degree of polymerization of 2400 and a degree of saponification of 99.9 mol% was applied to and dried on one side of this unstretched film to form a PVA layer.
- the obtained laminate was stretched twice in the longitudinal direction between rolls having different peripheral speeds at 120 ° C. and wound up.
- the obtained laminate was treated with a 4% boric acid aqueous solution for 30 seconds, and then immersed in a mixed aqueous solution of iodine (0.2%) and potassium iodide (1%) for 60 seconds for staining. Subsequently, it was treated with a mixed aqueous solution of potassium iodide (3%) and boric acid (3%) for 30 seconds. Further, this laminate is uniaxially stretched in the longitudinal direction in a mixed aqueous solution of boric acid (4%) and potassium iodide (5%) at 72 ° C., subsequently washed with a 4% potassium iodide aqueous solution, and the aqueous solution is prepared with an air knife.
- the solution was dried in an oven at 80 ° C., both ends were slit and wound up to obtain a PVA polarizer transfer laminate having a width of 50 cm and a length of 1000 m.
- the total draw ratio was 6.5 times, and the thickness of the polarizer was 5 ⁇ m.
- the thickness was read by embedding a substrate laminated polarizer in an epoxy resin, cutting out a section, and observing it with an optical microscope.
- TAC triacetyl cellulose
- composition paint for retardation layer LC242 (manufactured by BASF) 95 parts by mass Trimethylolpropane triacrylate 5 parts by mass Irgacure 379 3 parts by mass Surfactant 0.1 parts by mass Methyl ethyl ketone 250 parts by mass
- a polarizer having a thickness of 10 ⁇ m.
- a saponified 20 ⁇ m-thick triacetyl cellulose TAC film was laminated on one side of the obtained polarizing element with the retardation layer surface of the 1 / 4 ⁇ plate on the other surface to obtain a circular polarizing plate B.
- An ultraviolet curable adhesive was used for bonding.
- the following dye (e) was synthesized with reference to the method for producing the compound of the general formula (1) of Japanese Patent Publication No. 63-1357.
- the polarizing element surface of the obtained polarizing plate and the retardation layer surface of the 1 / 4 ⁇ plate were bonded together using an ultraviolet curable adhesive to obtain a circular polarizing plate C.
- composition for protective coat layer Urethane Acrylate AH-600 (manufactured by Kyoeisha Chemical Co., Ltd.) 25 parts by mass Polymerizer Irgacure 184 (manufactured by Ciba Specialty Chemicals) 1.25 parts by mass Isopropyl alcohol 75 parts by mass
- a polyester film (a surface protective film is diverted) assuming a touch panel on the side surface of the retardation layer of the circular polarizing plate of the laminated body, two Upirex (registered trademarks) S having a thickness of 50 ⁇ m assuming an organic EL cell, and a back surface protective film ( (Diverted surface protection film) was laminated.
- the front and back surface protective films assuming the touch panel used for lamination were the same as the surface protection film laminated with the circularly polarizing plate, and the slow axes of the films were made parallel.
- the side surface of the polarizer is a TAC film surface to which the polarizers of the PVA polarizer transfer laminate are bonded, and the side surface of the retardation layer is the TAC film surface of the 1 / 4 ⁇ plate.
- the side surface of the polarizing element of the circular polarizing plate B is the TAC film surface to which the PVA polarizer is bonded, and the side surface of the retardation layer is the TAC film surface of the 1 / 4 ⁇ plate.
- the side surface of the polarizer of the circular polarizing plate C is a TAC film surface provided with a liquid crystal polarizer, and the side surface of the retardation layer is the TAC film surface of a 1 / 4 ⁇ plate.
- the side surface of the polarizing plate of the circular polarizing plate D is the polarizing plate surface, and the side surface of the retardation layer is the TAC film surface of the 1 / 4 ⁇ plate.
- the thermoplastic resin base material of the PVA polarizer transfer laminate was peeled off immediately before being bonded to the surface protective film.
- the side surface of the polarizer of the circular polarizing plate E is the polarizer surface, and the side surface of the retardation layer is the protective coating surface.
- thermoplastic resin base material of the laminate for PVA polarizer transfer was peeled off immediately before being bonded to the surface protective film, and then the biaxially stretched polyester film (A4100 manufactured by Toyo Spinning Co., Ltd.) was peeled off.
- the obtained foldable display model was set to a bending radius of 3.0 mm, and a bending resistance test was performed 200,000 times in the same manner as the bending resistance of the above-mentioned laminated body.
- a bending resistance test was performed 200,000 times in the same manner as the bending resistance of the above-mentioned laminated body.
- no creases, cracks, etc. were observed, and excellent bending resistance was exhibited.
- the foldable display using the hard coat film for a foldable display of the present invention deforms after the polyester film or hard coat film located on the surface of the foldable display is repeatedly folded while maintaining mass productivity. Since it does not occur, the image is not distorted at the folded portion of the display.
- the portable terminal device or image display device equipped with the foldable display of the present invention provides beautiful images, is rich in functionality, and is excellent in convenience such as portability.
- Folding display 11 Bending radius 2: Polyester film for surface protection film of folding display 21: Folding part 22: Bending direction (direction orthogonal to the folding part)
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Abstract
Description
1. 少なくとも表面保護フィルム、偏光子、位相差層を有する折りたたみ型ディスプレイであり、表面保護フィルムが下記条件を満足する厚みが10~80μmであるポリエステルフィルムである折りたたみ型ディスプレイ。
(1)屈曲方向の屈折率が1.590~1.620
(2)折りたたみ部の方向の屈折率が1.670~1.700
(3)厚み方向の屈折率が1.520以下
(4)密度が1.380g/cm3以上
(ここで、屈曲方向とは、ポリエステルフィルムを折りたたむ際の折りたたみ部と直交する方向をいう。)
2. 前記ポリエステルフィルムの屈曲方向の弾性率が2.7GPa以下, 折りたたみ部の方向の弾性率が4.5GPa以上である上記第1に記載の折りたたみ型ディスプレイ。3. 前記ポリエステルフィルムの少なくとも片面上にハードコート層を有し、ハードコート層が少なくとも折りたたみ型ディスプレイの表面に位置している上記第1又は第2に記載の折りたたみ型ディスプレイ。
4. 前記の少なくとも片面上にハードコート層を有するポリエステルフィルムの全光線透過率が85%以上、ヘイズが3%以下である上記第3に記載の折りたたみ型ディスプレイ。
5. 折りたたみ型ディスプレイの折りたたみ部を介して連続した単一の表面保護フィルムが配されている上記第1~第4のいずれかに記載の折りたたみ型ディスプレイ。
6. 前記位相差板が、1/4λ板である上記第1~第5のいずれかに記載の折りたたみ型ディスプレイ。
7. 上記第6に記載の折りたたみ型ディスプレイを有する携帯端末機器。
本発明で言うディスプレイとは、表示装置を全般に指すものであり、ディスプレイの種類としては、LCD、有機ELディスプレイ、無機ELディスプレイ、LED、FEDな
どあるが、折曲げ可能な構造を有するLCDや、有機EL、無機ELが好ましい。特に層構成を少なくすることができる有機EL、無機ELが特に好ましく、色域の広い有機ELがさらに好ましい。
折りたたみ型ディスプレイは、連続した1枚のディスプレイが、携帯時は2つ折りなどに折りたたむことができるものである。折りたたむことでサイズを半減させ、携帯性を向上させることができる。折りたたみ型ディスプレイの屈曲半径は5mm以下が好ましく、3mm以下がさらに好ましい。屈曲半径が5mm以下であれば、折りたたんだ状態での薄型化が可能となる。屈曲半径は小さいほど良いと言えるが、屈曲半径が小さいほど折り跡がつきやすくなる。屈曲半径は0.1mm以上が好ましいが、0.5mm以上であってもよく、1mm以上であってもよい。屈曲半径が1mmであっても、携帯時には実用的に十分な薄型化を達成することができる。折りたたんだ際の屈曲半径とは、図1の模式図の符号11の箇所を測定するもので、折りたたんだ際の折りたたみ部分の内側の半径を意味している。なお、後述する表面保護フィルムは、折りたたみ型ディスプレイの折りたたんだ外側に位置していてもよいし、内側に位置していてもよい。
また、折りたたみ型ディスプレイは3つ折り、4つ折りであってもよく、さらに、ローラブルといわれる巻き取り型であってもよく、これらいずれも本発明でいう折りたたみ型ディスプレイの範囲に入るものとする。
折りたたみ型有機ELディスプレイの必須構成としては、有機ELモジュールであるが、さらに必要に応じて、円偏光板、タッチパネルモジュール、表面保護フィルム、裏面保護フィルムなどが設けられる。
(有機ELモジュール)
有機ELモジュールの一般的な構成は、電極/電子輸送層/発光層/ホール輸送層/透明電極からなる。
(1)屈曲方向の屈折率が1.590~1.620
(2)折りたたみ部の方向の屈折率が1.670~1.700
(3)厚み方向の屈折率が1.520以下
(4)密度が1.380g/cm3以上
(ここで、屈曲方向とは、ポリエステルフィルムを折りたたむ際の折りたたみ部と直交する方向をいう。)
中でコーティングすることで形成することができる。
くるという点で、0.3μm以上が好ましく、さらには、0.5μm以上が好ましい。
ルムを製造する場合には、2台以上の押出機、2層以上のマニホールドまたは合流ブロック(例えば、角型合流部を有する合流ブロック)を用いて、各最外層を構成する複数のフィルム層を積層し、口金から2層以上のシートを押し出し、キャスティングロールで冷却して未延伸フィルムを形成することができる。
本発明において、ポリエステルフィルムの長手方向(機械流れ方向)及び幅方向の少なくともいずれか一方向の屈折率は1.590~1.620であることが好ましく、更に好ましくは、1.591~1.600である。そして、ポリエステルフィルムの屈曲方向の屈折率が1.590~1.620であることが好ましく、1.591~1.600であることがより好ましい。ここで、屈曲方向とは、図2のポリエステルフィルム(符号2)上の符号22に示すように、折りたたみ型ディスプレイの用途において想定される折りたたみ部(符号21)と直交する方向を指している。長手方向及び幅方向の少なくともいずれか一方向の屈折率が1.590~1.620であると、繰り返し折りたたんだ際の変形が少なく、折りたたみ型ディスプレイの画質を低下させるおそれがなく好ましい。屈折率は1.591~1.600であることがより好ましい。もちろん、その方向は前記の屈曲方向であることが好ましい。1.590以上であると後述の屈曲試験後に折りたたみ部方向にクラックが入るおそれがなく、もちろん破断も起こらないため、ディスプレイの視認性を良好に保つことができる。ポリエステルフィルムの屈折率は、延伸倍率、延伸温度を調節することで効果的に調節することができる。また、屈折率の調整のために延伸方向の緩和工程、多段延伸を用いても良い。多段延伸を行う場合には、1段目の延伸倍率よりも2段目以降の延伸倍率を高くすることが好ましい。
ましい。延伸温度としては、75~120℃が好ましく、75~105℃が更に好ましい。なお延伸時の加熱方法は、熱風加熱方式、ロール加熱方式、赤外加熱方式など従来公知の手段を採用することができる。延伸温度を75~120℃にすることで、上記延伸倍率での延伸による大きな厚みムラを防ぐことができる。また、前記のように大きな厚みムラを生じない範囲でなるべく低温で延伸することで、厚み方向の屈折率を低下させることができる。
上記のポリエステルフィルムの屈折率が1.590~1.620である方向と直交する方向の屈折率は、1.670~1.700であることが好ましい。即ち、屈曲方向と直交する方向(折りたたみ部の方向)の屈折率が1.670~1.700であることが好ましい。1.670~1.700にすることで屈曲方向に折りたたんだ際の変形を少なくすることができる。1.700以下にすることで折りたたみ部の方向にクラックが入ったり、破断することを抑制することができる。1.670以上にすることで屈曲方向の屈曲性を向上させること、表面硬度を向上させることができる。1.680~1.695がより好ましい。屈曲方向と直交する方向の屈折率を調整する方法として、延伸倍率、延伸予熱温度、延伸温度、多段延伸、フィルム弛緩が挙げられる。延伸倍率は4.0~6.0倍であることが好ましく、より好ましくは、4.4~6.0である。また、屈曲方向と直交する方向の延伸予熱温度は70~110℃であることが好ましい。屈曲方向と直交する方向に多段延伸する場合、1段目より2段目以降の延伸倍率を高くする方が好ましい。フィルム弛緩は機械流れ方向(長手方向)、垂直方向(幅方向)に何れにおいても1~10%行っても良い。
厚み方向の屈折率は1.520以下であることが好ましい。1.520以下にすることで、屈曲方向の屈折率を低く設計しても、フィルム表面の硬度の低下を抑制することができ、屈曲性と表面硬度の両立を実現することができるためである。1.520以下にすることで厚み方向の試験力除荷後の押し込み深さが低減し、フィルム表面の硬度、特にハードコート層積層後のハードコートフィルムの鉛筆硬度を向上することができる。より好ましくは1.515以下、更に好ましくは1.510以下、特に好ましくは1.505以下、最も好ましくは1.500以下である。厚み方向の屈折率は低いことが好ましいが、安定した生産の面で1.3以上が好ましく、さらには1.4以上であってもよい。特に好ましくは1.410以上である。上記範囲は屈曲方向と折りたたみ方向に延伸倍率を両方に増加させていくことで達成できると言えるが、屈曲方向と幅方向の屈折率を好ましい範囲に制御した上で、厚み方向の屈折率を制御するためには、製膜工程の各工程条件のバランスを確認しながら条件設定することが好ましい。
熱固定温度は180~240℃が好ましい。熱固定を行うことで延伸方向への配向結晶化が進み、厚み方向の屈折率を下げることができる。
厚み方向の屈折率を下げることでフィルム表面の硬度が向上する理由は必ずしも明確ではないが、分子鎖内のベンゼン環等の芳香族が面方向に配向し、厚み方向にかかる応力による変形を抑制する効果があると考えられる。
ポリエステルフィルムの密度は1.380g/cm3以上であることが好ましい。1.383g/cm3以上であることがより好ましい。1.380g/cm3以上にすることで屈曲性を向上させること、フィルム表面硬度、特に、ハードコート層を積層した後のハードコートフィルムの鉛筆硬度を向上させることができる。密度は高いほど好ましく、フィルム中の粒子の有無等によっても多少左右されるが、1.40g/cm3以下であることが好ましい。製膜時の熱固定温度を180~240℃に設定することで結晶化を進行させ密度を効果的に増大させることができる。
(1)屈曲方向の屈折率が1.590~1.620
(2)折りたたみ部の方向の屈折率が1.670~1.700
(3)厚み方向の屈折率が1.520以下
(4)密度が1.380g/cm3以上
の4つの特性を同時に具備させることが特に好ましい態様と言えるが、上述の好ましい製造条件の範囲内での組合せであっても、例えば、屈曲方向の延伸倍率が1.4倍以下、折りたたみ部の方向の延伸倍率が4.4倍未満であり、かつ、熱固定温度が220℃以下の組合せであるような、各々の好ましい製造条件範囲の中において最善とは言えない条件の組合せの場合、必ずしも上記の4つの特性を同時に満足するものが得られない場合が起こり得る。この場合には、屈曲方向の延伸倍率延伸倍率を1.7倍以上に高めたり、折りたたみ部の方向の延伸倍率が4.4倍以上に高めたり、熱固定温度を230℃程度に高めたり、あるいは屈曲方向及び/又は折りたたみ部の方向の延伸温度を低くするなど、いずれかの条件の微調整またはそれらの組合せによって、上記の4つの特性を同時に満足させることができる。
本発明において、ポリエステルフィルムとハードコート層などとの接着性を向上させるため、ポリエステルフィルムに易接着層を積層することも好ましい。易接着層は、易接着層形成のための塗布液を未延伸又は縦方向の1軸延伸フィルムの片面または両面に塗布した後、必要に応じて熱処理乾燥し、さらに延伸されていない少なくとも一方向に延伸して得ることができる。二軸延伸後にも熱処理することができる。最終的な易接着層の塗布量は、0.005~0.20g/m2に管理することが好ましい。塗布量が0.005g/m2以上であると、接着性が得られて好ましい。一方、塗布量が0.20g/m2以下であると、耐ブロッキング性が得られて好ましい。
ポリエステルフィルムは、その少なくとも片面上にハードコート層を有していることが好ましい。ハードコート層は、ポリエステルフィルム上のディスプレイ表面側に位置させてディスプレイにおいて用いられることが好ましい。カールを抑制するためにハードコート層は両面に設けても良い。ハードコート層を形成する樹脂としては、アクリル系、シロキサン系、無機ハイブリッド系、ウレタンアクリレート系、ポリエステルアクリレート系、エポキシ系など特に限定なく使用できる。また、2種類以上の材料を混合して用いることもできるし、無機フィラーや有機フィラーなどの粒子を添加することもできる。
ハードコート層の膜厚としては、1~50μmが好ましい。1μm以上であると十分に硬化し、鉛筆硬度が高くなり好ましい。また厚みを50μm以下にすることで、ハードコートの硬化収縮によるカールを抑制し、フィルムのハンドリング性を向上させることができる。
ハードコート層の塗布方法としては、マイヤーバー、グラビアコーター、ダイコーター、ナイフコーターなど特に限定なく使用でき、粘度、膜厚に応じて適宜選択できる。
ハードコート層の硬化方法としては、紫外線、電子線などのエネルギー線や、熱による硬化方法など使用でき、フィルムへのダメージを軽減させるために、紫外線や電子線などによる硬化方法が好ましい。
ハードコート層の鉛筆硬度としては、3H以上が好ましく、4H以上が更に好ましい。3H以上の鉛筆硬度があれば、容易に傷がつくことはなく、視認性を低下させない。一般にハードコート層の鉛筆硬度は高い方が好ましいが9H以下で構わず、8H以下でも構わず、6H以下でも実用上は問題なく使用できる。
本発明におけるハードコート層は、上述のような表面の鉛筆硬度を高めてディスプレイの保護をする目的に使用できるものであり、透過率が高いことが好ましい。ハードコートフィルムの透過率としては、85%以上が好ましく、88%以上がさらに好ましい。透過率が87%以上あれば、十分な視認性が得られる。ハードコートフィルムの全光線透過率は、一般的に高いほど好ましいが、安定した生産の面から99%以下が好ましく、97%以下であってもよい。また、ハードコートフィルムのヘイズは、一般的に低いことが好ましく、3%以下が好ましい。ハードコートフィルムのヘイズは2%以下がより好ましく、1%以下が最も好ましい。ヘイズが3%以下であれば、画像の視認性を向上させることができる。ヘイズは一般的には低いほどよいが、安定した生産の面から0.1%以上が好ましく、0.3%以上であってもよい。
本発明の折りたたみ型ディスプレイは偏光子を有する。液晶ディスプレイでは、液晶セルの両側に偏光子が設けられ、ELディスプレイ等では内部構造からの反射光を低減するための円偏光素子(偏光子と1/4λ層との積層体)が用いられることが好ましい。
偏光子は、偏光子と偏光子を保護するための偏光子保護フィルムの積層構成である偏光板として用いられることが、折りたたみ型ディスプレイ製造時の取り扱いの面で好ましい形態の一つである。
なお、本明細書において、偏光子および位相差層(偏光子保護フィルムや偏光子保護コートを有する場合はこれらも含めて)を一体物として偏光素子という場合がある。
73563号公報、特開2012-073563号公報、特開2011-2816号公報を参考にすることができる。これらの方法で作成された偏光子を本発明では好ましく用いることができる。
基材性層延伸法で得られた偏光子は、偏光子保護フィルムや位相差フィルムに転写して設けることが好ましい。また、偏光子保護フィルムを用いずにさらに薄型にする場合には、画像表示セルやタッチパネル、表面保護フィルムに転写して設けることも好ましい。
液晶化合物を用いた偏光子は偏光子保護フィルムなどのフィルムに、重合性液晶化合物と有機系の二色性色素を配向させたものや液晶性の二色性色素を含有するコート液を塗工後、乾燥、配向、光または熱硬化させて偏光子とすることができる。液晶偏光子を配向させる方法としては、コート液を塗工するフィルムの表面をラビング処理する方法、コート液を塗工後に偏光の紫外線を照射して液晶化合物を配向させながら硬化させる方法が挙げられる。
好ましい二色性色素としては、特開2007-126628号公報、特開2010-168570号公報、特開2013-101328号公報、特開2013-210624号公報等に記載の色素が挙げられる。
配向制御層としては、
・ポリビニルアルコールおよびその誘導体、ポリイミドおよびその誘導体、アクリル樹脂、ポリシロキサン誘導体などを塗工しその表面をラビング処理して配向層(ラビング配向制御層)とする方法、
・シンナモイル基及びカルコン基等の光反応性基を有するポリマー又はモノマーと溶剤とを含む塗工液を基材フィルムに塗布し、偏光紫外線を照射することによって配向硬化させ配向層(光配向制御層)とする方法、
等が挙げられる。
本発明の折りたたみ型ディスプレイは偏光子と画像表示セルとの間に位相差層(位相差フィルムともいう)を有していることが好ましい。位相差層は、画像表示セルが液晶セルである場合には、斜めからの光では、セルの液晶化合物による斜めからの光の位相差のずれを補正して色ズレを低減させる光学補償の役割を持つ。
また、画像表示セルがELセル等の場合であれば、円偏光板の1/4λ層としての役割を持つ。
液晶化合物としては、例えば、棒状の液晶化合物、ポリマー状の液晶化合物、反応性の官能基を有する液晶化合物等が挙げられる。
CH2=CHCOO-(CH2)m-O-Ph1-COO-Ph2-OCO-Ph1-O-(CH2)n-OCO-CH=CH2
CH2=CHCOO-(CH2)m-O-Ph1-COO-NPh-OCO-Ph1-O-(CH2)n-OCO-CH=CH2
CH2=CHCOO-(CH2)m-O-Ph1-COO-Ph2-OCH3
CH2=CHCOO-(CH2)m-O-Ph1-COO-Ph1-Ph1-CH2CH(CH3)C2H5
(式中、
m及びnは2~6の整数であり、
Ph1及びPh2は1,4-フェニレン基(Ph2は2位にメチル基が置換されていてもよい)であり、
NPhは2,6-ナフチレン基である)
が挙げられる。
また、基材積層延伸法で基材上の偏光子に位相差層を設けたり、離型性基材上の液晶偏光子に位相差層を設けたりし、これを基材フィルムに転写してもよい。
また、COPフィルムやPCフィルム、PPフィルム、Acフィルム、TACフィルムなどの位相差フィルムに液晶位相差層を塗工や転写してもよい。
円偏光板における位相差層は1/4λ層であることが好ましい。以下、1/4λ層について詳しく説明する。
1/4λ層は、偏光子を通過した直線偏光を円偏光に変換し、ELセル内の配線、ガラス基板タッチパネルなどで反射された円偏光を入射した直線偏光とは90度ずれた直線偏光に変換することができる。1/4λ層は単層の1/4λ層であってもよく、1/4λ層と1/2λ層との複合1/4λ層であってもよい。1/4λ層には、Cプレート層などが設けられていてもよい。本明細書において、1/4λ層と言う場合、単層の1/4λ層だけでなく複合1/4λやさらにCプレート層などの位相差層を含む、1/4λの位相差を付与できる層の総称である。
単層の1/4λ層を用いる場合、1/4λ層の配向軸(遅相軸)と偏光子の透過軸がなす角度は35~55度が好ましく、より好ましくは40度~50度、さらに好ましくは42~48度である。
本発明の折りたたみ型ディスプレイでは、偏光子に偏光子保護フィルムが積層されて用いられていることも好ましい。偏光子保護フィルムとしては、COPフィルムやPCフィルム、PPフィルム、Acフィルム、TACフィルム、ポリエステルフィルムなどのフィルムなどを用いることができる。なかでも、TACフィルム、ポリエステルフィルムが折りたたみ耐久性の面で好ましい。
~40μmであり、更に好ましくは10~30μmであり、適宜、アンチグレア層や反射防止層などの表面処理層を設けることができる。前記範囲内であれば、屈曲を阻害することなく、好ましい態様となる。
好ましい具体的構成としては、下記の構成が挙げられる。
(1a)偏光子保護フィルム/偏光子/位相差フィルム
(1b)偏光子保護フィルム/偏光子/液晶位相差層/位相差フィルム
(1c)偏光子保護フィルム/偏光子/液晶位相差層/(位相差層の)基材フィルム
偏光子保護フィルムの代わりに偏光子に保護コート(偏光子保護コート)を行うことも好ましい。
偏光子保護コートは、ポリエステル、ポリアミド、ポリウレタン、アクリル、アミノ樹脂、など、フィルムのコート剤として用いられるものが好適なものとして挙げられる。偏光子保護フィルムの代わりに偏光子保護コートとすることでさらなる薄型化が可能となる。偏光子保護コートは直接塗工されるだけでなく、転写により設けられてもよく、偏光子や位相差層が液晶化合物を転写するものである場合は、離型性基材上に保護コート層と偏光子や位相差層を設けて一体として転写してもよい。
偏光子保護コートの厚さは1~30μmであることが好ましく、より好ましくは3~20μm、さらに好ましくは5~10μmである。
偏光子の両面が保護コートであってもよく、偏光子の片面が偏光子保護フィルムであり他面が偏光子保護コートであってもよく、偏光子の両面が偏光子保護コートであってもよい。好ましい具体的構成としては、下記の構成が挙げられる。
(2b)偏光子保護フィルム/偏光子/偏光子保護コート/液晶位相差層/位相差フィルム
(2c)偏光子保護フィルム/偏光子/偏光子保護コート/液晶位相差層/(位相差層の)基材フィルム
(3b)偏光子保護コート/偏光子/液晶位相差層/位相差フィルム
(3c)偏光子保護コート/偏光子/液晶位相差層/(位相差層の)基材フィルム
(4b)偏光子保護コート/偏光子/偏光子保護コート/液晶位相差層/位相差フィルム(4c)偏光子保護コート/偏光子/偏光子保護コート/液晶位相差層/(位相差層の)基材フィルム
上記の偏光素子は、本発明の折りたたみ型ディスプレイにおいて、他の部材(画像表示セル、タッチパネル、表面保護フィルムなど)と粘着層を介して積層されていることが好ましい。この場合、偏光子の他の部材面の偏光子保護コートや位相差層保護コートを設けず、偏光子や液晶位相差層上に直接粘着剤を設けて貼り合わせてもよい。
粘着層の材料としては特に制限されないが、例えば、ゴム系粘着剤、アクリル系粘着剤、シリコーン系粘着剤、ウレタン系粘着剤、ビニルアルキルエーテル系粘着剤、ポリビニルアルコール系粘着剤、ポリビニルピロリドン系粘着剤、ポリアクリルアミド系粘着剤、セルロース系粘着剤などが挙げられる。
これらのうち、透明性、耐候性、耐熱性などの観点から、アクリル系粘着剤であるのが好ましい。
粘着層は偏光素子に塗工により設ける方法、市販の光学粘着剤シートを用いる方法などが挙げられる。
フィルムまたはポリエステル樹脂を粉砕して乾燥した後、フェノール/テトラクロロエタン=60/40(質量比)の混合溶媒に溶解した。この溶液に遠心分離処理を施して無機粒子を取り除いた後に、ウベローデ粘度計を用いて、30℃で0.4(g/dl)の濃度の溶液の流下時間及び溶媒のみの流下時間を測定し、それらの時間比率から、Hugginsの式を用い、Hugginsの定数が0.38であると仮定して極限粘度を算出した。
幅方向20mm×流れ方向110mmの大きさのポリエステルフィルムサンプルを用意する。無負荷U字伸縮試験機(ユアサシステム機器社製、DLDMLH-FS)を用いて、屈曲半径1.5mmに設定し、1回/秒の速度で、20万回屈曲させた。その際、サンプルは長辺側両端部10mmの位置を固定して、屈曲する部位は20mm×90mmとした。ここで、図1は、折りたたみ型ディスプレイを折りたたんだ際の屈曲半径を示すための模式図であり、その折りたたんだ態様の内側表面にポリエステルフィルムが配されている場合を考慮して、図1の符号11の個所を1.5mmに設定したものとしてモデル的に屈曲試験をしている。屈曲処理終了後、サンプルの屈曲内側を下にして平面に置き、目視による観察を行った。
○ :サンプルにクラック及び変形を確認できない。
× :サンプルにクラックまたは折跡があり、水平に置いた際、浮き上がり最大高さが5mm以上。
上記屈曲試験と同様の方法で、屈曲半径0.5mmに設定し1回/秒の速度で20万回屈曲させた。ここで、図1は、折りたたみ型ディスプレイを折りたたんだ際の屈曲半径を示すための模式図であり、その折りたたんだ態様の内側表面にポリエステルフィルムが配されている場合を考慮して、図1の符号11の個所を0.5mmを設定したものとしてモデル的に屈曲試験をしている。屈曲部の外側のフィルム表面をデジタルマイクロスコープ(HIROX社製RH8800)の700倍で観察し、シワ(クラック)の有無を観察した。上記の屈
曲半径1.5mmの耐屈曲性目視テストとは別に、屈曲半径を0.5mmに小さくした本テストを行うことで、ハードコート層や他の部材が積層又は貼着された、折りたたみ型ディスプレイの実際の使用状態に近い状態での評価することを企図している。前記屈曲半径1.5mmによる目視観察とは別に、目視では検出しにくい微細な欠点である、破断しやすいまたはクラックが入りやすい欠点を検出するためのテストである。
○ :屈曲外側のフィルム表面に欠陥がない。
× :破断した、または屈曲外側のフィルム表面にシワ(クラック)が確認できる。
上記屈曲試験と同様の方法で、屈曲半径3.0mmに設定し1回/秒の速度でハードコートフィルムを20万回屈曲させた。ハードコート層が一方のみの場合は、ハードコート層を内側にした試験と、ハードコート層を外側にした試験をそれぞれ行った。
○ :ハードコート層に割れがない、ハードコートフィルムに変形が確認できない。
× :破断した、またはハードコート層に割れを確認できる、またはハードコートフィルムに変形が確認できる。
JIS K 7142:2008「プラスチックの屈折率測定方法(A法)」に準拠して、アッベ屈折率計(アタゴ社製、NAR-4T、測定波長589nm)を用いて、長手方向の屈折率、幅方向の屈折率、厚み方向の屈折率を求めた。
ハードコートフィルムの鉛筆硬度をサンプルとして、JIS K 5600-5-4:1999に準拠し、荷重750g、速度1.0mm/sで測定した。本発明においては3H以上を合格とした。
ヘイズメーター(日本電色工業社製、NDH5000)を用いて測定した。
JIS K 7112:1999準拠の方法(密度勾配管法)に従って密度を測定した。(単位:g/cm3)。
試料を約2cm角に切り取り、マイクロカバーガラス18×18mm(マツナミガラス社製)上に、測定面の反対面を接着剤(セメダイン(登録商標)ハイスーパー30)にて固定した。貼着固定後、12時間以上室温で放置し、その後、ダイナミック超微小硬度計「DUH-211」(島津製作所製)を用いて、次の条件で、試験力除荷後の押し込み深さ(μm)を測定した。
≪測定条件≫
試験モード :負荷-除荷試験
使用圧子 :稜間角115度、三角錐圧子
圧子弾性率:1.140×106N/mm2
圧子ポアソン比:0.07
試験力 :50mN
負荷速度 :4.44mN/sec
負荷保持時間 :2sec
除荷保持時間 :0sec
試料フィルムをタテ10mm×ヨコ250mmにカットし、長辺を測定したい方向に合わせて、200mm間隔で印をつけ、5gの一定張力下で印の間隔Aを測った。続いて、試料フィルムを無荷重で150℃の雰囲気のオーブン中で30分間放置した後、オーブンから取り出し室温まで冷却した。その後、5gの一定張力下で印の間隔Bを求め、下記式により熱収縮率(%)を求めた。なお、上記熱収縮率は試料フィルムの幅方向に3等分した位置で測定し、3点の平均値を熱収縮率(%)とする
熱収縮率(%)=[(A-B)×100]/A
屈曲方向と折りたたみ方向の双方向についてそれぞれ別個に試料フィルムのタテ、ヨコが異なるようにカットして測定し、測定値が大きい方向のデータを最大熱収縮率(%)とする。
JIS K7127に準拠してポリエステルフィルムの屈曲方向および折りたたみ方向
の引張弾性率を23℃にて測定した。
エステル化反応装置として、攪拌装置、分縮器、原料仕込口および生成物取り出し口を有する3段の完全混合槽よりなる連続エステル化反応装置を用い、TPAを2トン/hrとし、EGをTPA1モルに対して2モルとし、三酸化アンチモンを生成PETに対してSb原子が160ppmとなる量とし、これらのスラリーをエステル化反応装置の第1エステル化反応缶に連続供給し、常圧にて平均滞留時間4時間で、255℃で反応させた。次いで、上記第1エステル化反応缶内の反応生成物を連続的に系外に取り出して第2エステル化反応缶に供給し、第2エステル化反応缶内に第1エステル化反応缶から留去されるEGを生成ポリマー(生成PET)に対し8質量%供給し、さらに、生成PETに対してMg原子が65ppmとなる量の酢酸マグネシウムを含むEG溶液と、生成PETに対してP原子が20ppmのとなる量のTMPAを含むEG溶液を添加し、常圧にて平均滞留時間1.5時間で、260℃で反応させた。次いで、上記第2エステル化反応缶内の反応生成物を連続的に系外に取り出して第3エステル化反応缶に供給し、さらに生成PETに対してP原子が20ppmとなる量のTMPAを含むEG溶液を添加し、常圧にて平均滞留時間0.5時間で、260℃で反応させた。上記第3エステル化反応缶内で生成したエステル化反応生成物を3段の連続重縮合反応装置に連続的に供給して重縮合を行い、さらに、ステンレス焼結体の濾材(公称濾過精度5μm粒子90%カット)で濾過し、極限粘度0.62dl/gのポリエチレンテレフタレートペレット(a)を得た。
ポリエチレンテレフタレートペレット(a)の製造工程について、第3エステル化反応の滞留時間を調節した他は同様の方法にて極限粘度を0.580dl/gに調整し、ポリエチレンテレフタレートペレット(b)を得た。
ポリエチレンテレフタレートペレット(a)を、回転型真空重合装置を用い、0.5mmHgの減圧下、220℃で時間を変えて固相重合を行い、極限粘度0.75dl/gのポリエチレンテレフタレートペレット(c)を作成した。
撹拌機、ジムロート冷却器、窒素導入管、シリカゲル乾燥管、及び温度計を備えた4つ口フラスコに、1,3-ビス(イソシアネートメチル)シクロヘキサン72.96質量部、ジメチロールプロピオン酸12.60質量部、ネオペンチルグリコール11.74質量部、数平均分子量2000のポリカーボネートジオール112.70質量部、及び溶剤としてアセトニトリル85.00質量部、N-メチルピロリドン5.00質量部を投入し、窒素雰囲気下、75℃において3時間撹拌し、反応液が所定のアミン当量に達したことを確認した。次に、この反応液を40℃にまで降温した後、トリエチルアミン9.03質量部を添加し、ポリウレタンプレポリマーD溶液を得た。次に、高速攪拌可能なホモディスパーを備えた反応容器に、水450gを添加して、25℃に調整して、2000min-1で攪拌混合しながら、イソシアネート基末端プレポリマーを添加して水分散した。その後、減圧下で、アセトニトリルおよび水の一部を除去することにより、固形分35質量%の水溶性ポリウレタン樹脂(A)を調製した。
温度計、窒素ガス導入管、還流冷却器、滴下ロート、および攪拌機を備えたフラスコにイソホロンジイソシアネート200質量部、カルボジイミド化触媒の3-メチル-1-フェニル-2-ホスホレン-1-オキシド4質量部を投入し、窒素雰囲気下、180℃において10時間撹拌し、イソシアネート末端イソホロンカルボジイミド(重合度=5)を得た。次いで、得られたカルボジイミド111.2g、ポリエチレングリコールモノメチルエーテル(分子量400)80gを100℃で24時間反応させた。これに水を50℃で徐々に加え、固形分40質量%の黄色透明な水溶性カルボジイミド化合物(B)を得た。
下記の塗剤を混合し、塗布液を作成した。
水 16.97質量部
イソプロパノール 21.96質量部
ポリウレタン樹脂(A) 3.27質量部
水溶性カルボジイミド化合物(B) 1.22質量部
粒子 0.51質量部
(平均粒径40nmのシリカゾル、固形分濃度40質量%)
界面活性剤 0.05質量部
(シリコーン系、固形分濃度100質量%)
ハードコート材料(JSR社製、オプスター(登録商標)Z7503、濃度75%)100質量部に、レベリング剤(ビックケミージャパン社製、BYK307、濃度100%)0.1質量部を添加し、メチルエチルケトンで希釈して固形分濃度40質量%のハードコート塗布液aを調製した。
ペンタエリスリトールトリアクリレート(新中村化学工業社製、A-TMM-3、固形分濃度100%)95質量部、光重合開始剤(BASFジャパン社製、イルガキュア(登録商標)907、固形分濃度100%)5質量部、レベリング剤(ビックケミージャパン社製、BYK307、固形分濃度100%)0.1質量部を混合し、トルエン/MEK=1/1の溶媒で希釈して、濃度40質量%のハードコート塗布液bを調製した。
ポリエチレンテレフタレートのペレット(a)を押出機に供給し、285℃で融解した。このポリマーを、ステンレス焼結体の濾材(公称濾過精度10μm粒子95%カット)で濾過し、口金よりシート状にして押し出した後、静電印加キャスト法を用いて表面温度30℃のキャスティングドラムに接触させ冷却固化し、未延伸フィルムを作った。この未延伸フィルムを加熱ロールを用いて75℃に均一加熱し、非接触ヒーターで85℃に加熱して1.4倍のロール延伸(縦延伸)を行った。得られた一軸延伸フィルムに上記の易接着層形成用塗布液をロールコート法で両面に塗布した後、80℃で20秒間乾燥した。なお、最終(二軸延伸後)の乾燥後の塗布量が0.06g/m2になるように調整した。そ
の後、テンターに導き105℃で予熱後、95℃で4.0倍に横延伸し、幅固定して230℃で5秒間の熱固定を施し、さらに180℃で幅方向に4%緩和させることにより、厚み50μmポリエステルフィルム1を得た。作製したフィルムの一方の面にマイヤーバーを用いて、ハードコート塗布液aを乾燥後の膜厚が5μmになるように塗布し、80℃で1分間乾燥させた後、紫外線を照射し(積算光量200mJ/cm2)、ハードコートフィルムを得た。評価結果を表1、2に示す。
表1に記載の長手方向の延伸倍率に変更した他はポリエステルフィルム1と同様にしてポリエステルフィルムおよびハードコートフィルムを得た。
幅方向の延伸倍率を4.4倍に、熱固定温度を220℃に変更した他はポリエステルフィルム1と同様にしてポリエステルフィルムおよびハードコートフィルムを得た。
表1に記載のように長手方向の延伸倍率に変更した他はポリエステルフィルム4と同様にしてポリエステルフィルムおよびハードコートフィルムを得た。
幅方向の延伸倍率を5.5倍に、熱固定温度を190℃に変更した他はポリエステルフィルム1と同様にしてポリエステルフィルムおよびハードコートフィルムを得た。
表1に記載のように長手方向の延伸倍率に変更した他はポリエステルフィルム7と同様にしてポリエステルフィルムおよびハードコートフィルムを得た。
ポリエステルフィルム5の製造工程において、長手方向に延伸した後に100℃で10%の弛緩熱処理を施した他はポリエステルフィルム5と同様にして、ポリエステルフィルムおよびハードコートフィルムを得た。
ポリエステルフィルム5の製造工程において、熱固定後に200℃でクリップを開放し、長手方向、幅方向に弛緩熱処理した他は実施例5と同様にして、ポリエステルフィルムおよびハードコートフィルムを得た。長手方向は弛緩率が3%になるようテンター速度と巻き取りロール速度を調整した。幅方向の弛緩はフリー状態とした。
長手方向延伸時の温度を75℃に変更し、熱固定温度を220℃に変更した他はポリエステルフィルム1と同様にしてポリエステルフィルムおよびハードコートフィルムを得た。
長手方向延伸時の温度を75℃に変更し、延伸倍率1.2倍に変更して延伸した後、幅方向に延伸倍率5.0倍に変更して延伸した他はポリエステルフィルム1と同様にしてポリエステルフィルムおよびハードコートフィルムを得た。
ポリエステルフィルム3の長手方向の延伸を2段延伸とし、その1段目の延伸倍率を1.2倍とし、2段目の延伸倍率を1.67倍とした他はポリエステルフィルム3と同様にしてポリエステルフィルムおよびハードコートフィルムを得た。トータルでの長手方向の延伸倍率は約2.0倍である。
幅方向延伸時の予熱温度を95℃に変更し、熱固定温度を190℃に変更した他はポリエステルフィルム5と同様にしてポリエステルフィルムおよびハードコートフィルムを得た。
ポリエステルフィルム2の幅方向の延伸を2段延伸とし、その1段目の延伸倍率を1.5倍とし、2段目の延伸倍率を4.0倍とし、熱固定温度を190℃に変更した他はポリ
エステルフィルム2と同様にしてポリエステルフィルムおよびハードコートフィルムを得た。トータルの幅方向の延伸倍率は6.0倍である。
表2に記載のように厚みを変更した他はポリエステルフィルム2と同様にしてポリエステルフィルムおよびハードコートフィルムを得た。
ポリエステルフィルム1の製造工程において幅方向の弛緩熱処理を行わなかった他はポリエステルフィルム1と同様にしてポリエステルフィルムおよびハードコートフィルムを得た。
ポリエステルフィルム1と同様に未延伸フィルムを作成後、未延伸フィルムをテンターで75℃で予熱し、85℃で1.4倍に横延伸した。得られた一軸延伸フィルムに上記の易接着層形成用塗布液をロールコート法で両面に塗布した後、80℃で20秒間乾燥した。なお、最終(二軸延伸後)の乾燥後の塗布量が0.06g/m2になるように調整した
。加熱ロールを用いて105℃に均一加熱し、非接触ヒーターで95℃に加熱し.4.0倍にロール延伸(縦延伸)を行った。幅固定して230℃で5秒間の熱固定を施し、厚み50μmポリエステルフィルムおよびハードコートフィルムを得た。
長手方向の延伸を行わずに、幅方向のみ延伸し横1軸延伸とした他はポリエステルフィルム1と同様にしてポリエステルフィルムおよびハードコートフィルムを得た。
長手方向の延伸を行わずに、幅方向のみ延伸し横1軸延伸とした他はポリエステルフィルム7と同様にしてポリエステルフィルムおよびハードコートフィルムを得た。
熱固定温度を220℃に変更し、表1、2記載のPETペレット、厚みとした他はポリエステルフィルム1と同様にしてポリエステルフィルムおよびハードコートフィルムを得た。
比較例3~7は、前記の通り実施例1よりも熱固定温度が低く、長手方向、幅方向の延伸倍率が好ましい条件範囲の中では最善とは言えない各条件水準の組合せであり、表2に記載したように厚み方向の屈折率が増加し、試験力除荷後の押し込み深さが大きく、ハードコート層積層後の鉛筆硬度が各実施例に比較して小さくなった。
長手方向の延伸倍率を2.7倍に変更し、熱固定温度を220℃に変更した他はポリエステルフィルム1と同様にしてポリエステルフィルムおよびハードコートフィルムを得た。
長手方向の延伸倍率を3.4倍に変更した他はポリエステルフィルム1と同様にしてポリエステルフィルムおよびハードコートフィルムを得た。
熱固定温度を100℃に変更した他はポリエステルフィルム4と同様にしてポリエステルフィルムおよびハードコートフィルムを得た。
長手方向の延伸温度を130℃に変更した他はポリエステルフィルム13と同様にしてポリエステルフィルムおよびハードコートフィルムを得た。
幅方向予熱温度を120℃に変更した他はポリエステルフィルム1と同様にしてポリエステルフィルムおよびハードコートフィルムを得た。
ポリエステルフィルム1と同様に厚み50μmポリエチレンテレフタレートフィルムを得た後、ハードコート塗布液bを塗布したハードコートフィルムを得た。
(表面保護フィルム、偏光子、位相差層を有する折りたたみ型ディスプレイの作成および評価)
上記のポリエステルフィルムを表面保護フィルムとして用い、偏光子、位相差層を有する折りたたみ型ディスプレイのモデルを作成した。
厚さ20μmのトリアセチルセルロース(TAC)フィルムの片面をけん化処理し、鹸化処理面に紫外線硬化型接着剤を用いてPVA偏光子転写用積層体の偏光子面と貼り合わせた後、熱可塑性樹脂基材を剥離した。
剥離面(偏光子面)に紫外線硬化型接着剤を用いて1/4λ板の位相差層面と貼り合わせ円偏光板Aを得た。
なお、PVA偏光子転写用積層体および位相差板は以下のようにして作成した。
熱可塑性樹脂基材として極限粘度0.62dl/dのポリエチレンテレフタレートを押出機で溶融・混練後、冷却ロール上にシート状に押出、厚さ100μmの未延伸フィルムを作成した。この未延伸フィルムの片面に、重合度2400、ケン化度99.9モル%のポリビニルアルコールの水溶液を塗布および乾燥して、PVA層を形成した。
得られた積層体を、120℃で周速の異なるロール間で長手方向に2倍に延伸して巻き取った。次に、得られた積層体を4%のホウ酸水溶液で30秒間の処理を行った後、ヨウ素(0.2%)とヨウ化カリウム(1%)の混合水溶液で60秒間浸漬し染色し、引き続き、ヨウ化カリウム(3%)とホウ酸(3%)の混合水溶液で30秒間処理した。
さらに、この積層体を72℃のホウ酸(4%)とヨウ化カリウム(5%)混合水溶液中で長手方向に一軸延伸を行い、引き続き、4%ヨウ化カリウム水溶液で洗浄、エアナイフで水溶液を除去した後に80℃のオーブンで乾燥し、両端部をスリットして巻き取り、幅50cm、長さ1000mのPVA偏光子転写用積層体を得た。合計の延伸倍率は6.5倍で、偏光子の厚みは5μmであった。なお、厚みは基材積層偏光子をエポキシ樹脂に包埋して切片を切り出し、光学顕微鏡で観察して読み取った。
厚さ20μmのトリアセチルセルロース(TAC)フィルムの片面をけん化処理し、鹸化処理面に配向制御層用塗料組成物を塗布、100℃で乾燥させ、厚さ0.5μmの配向制御層を設けた。さらに配向制御層をナイロン製の起毛布が巻かれたラビングロールで処理した。ラビング方向はフィルムの流れ方向に対して45度になるよう行った。
引き続き、ラビング処理を施した面に位相差層用組成物塗料を塗布後、110℃で3分間加熱して溶剤を蒸発させると共に、液晶性化合物を配向させた。引き続き、110℃の環境下で紫外線を30秒間照射し、TACフィルムに1/4λ層を有するPVA偏光子転写用積層体を得た。
・下記変性ポリビニルアルコール 10質量部
・水 371質量部
・メタノール 119質量部
・グルタルアルデヒド 0.5質量部
LC242(BASF社製) 95質量部
トリメチロールプロパントリアクリレート 5質量部
イルガキュア379 3質量部
界面活性剤 0.1質量部
メチルエチルケトン 250質量部
ポリビニルアルコールフィルムを、速度比の異なるロール間において、30℃、0.3%濃度のヨウ素溶液中で1分間染色しながら、3倍まで延伸した。その後、60℃、4%濃度のホウ酸、10%濃度のヨウ化カリウムを含む水溶液中に0.5分間浸漬しながら総合延伸倍率が6倍まで延伸した。次いで、30℃、1.5%濃度のヨウ化カリウムを含む水溶液中に10秒間浸漬することで洗浄した後、50℃で4分間乾燥を行い、厚さ10μmの偏光子を得た。得られた偏光子の片面に、けん化処理した厚さ20μmのトリアセチルセルロースTACフィルムを他方の面に上記1/4λ板の位相差層面と貼り合わせ円偏光板Bを得た。貼り合わせは紫外線硬化型接着剤を用いた。
厚さ20μmのトリアセチルセルロース(TAC)フィルムの片面をけん化処理し、鹸化処理面に上記配向制御層用塗料組成物を塗布、100℃で乾燥させ、厚さ0.5μmの配向制御層を設けた。さらに配向制御層をナイロン製の起毛布が巻かれたラビングロールで処理した。ラビング方向はフィルムの流れ方向に対して平行になるよう行った。
引き続き、ラビング処理を施した面に下記液晶偏光膜用塗料を塗布し、110℃で3分間乾燥し、厚み2μmの膜を形成し、引き続き紫外線を照射して、TACフィルム上に液晶化合物の偏光子を有する偏光板を得た。
(液晶偏光膜用塗料)
(重合性液晶化合物の合成)
特表2007-510946号公報の[0134]段落の記載および、Lub et al.Recl.Trav.Chim.Pays-Bas,115,321-328(1996)を参考にして、下記化合物(a)、(b)を合成した。
(a)75質量部、(b)25質量部、(c)2.5質量部、(d)2.5質量部、(e)2.5質量部、IRGACURE(R) 369E(BASF社製)6質量部、オルトキシレン250質量部を混合、溶解させた。
上記記1/4λ板の位相差層面と上記PVA偏光子転写用積層体の偏光子面とを紫外線硬化型接着剤を用いて貼り合わせた。その後、PVA偏光子転写用積層体の熱可塑性基材を剥離し、円偏光板Dを得た。
二軸延伸ポリエステルフィルム(東洋紡株式会社製A4100)の非易接着面に下記保護コート組成物を塗布、乾燥後紫外線を照射した。さらにこの保護コート面に1/4λ層の作成と同様にして、配向制御層、1/4λ層を設けた。引き続き、1/4λ層上に配向制御層を設け、この配向制御層上に円偏光板Cの作成と同様にして液晶化合物からなる偏光子を設けた。
ウレタンアクリレート AH-600(共栄社化学製)25質量部
重合開始剤 イルガキュア184(チバスペシャルティケミカルズ製)1.25質量部
イソプロピルアルコール 75質量部
表面保護フィルム(ハードコートフィルム)と円偏光板の偏光子側面とを光学用の基材レス粘着剤シート(厚み25μm)を用いて貼り合わせた。
さらに、上記積層体の円偏光板の位相差層側面にタッチパネルを想定したポリエステルフィルム(表面保護フィルムを転用)、有機ELセルを想定した厚み50μmのユーピレックス(登録商標)S2枚、裏面保護フィルム(表面保護フィルムを転用)を積層した。積層に用いたタッチパネルを想定した表面保護フィルムおよび裏面保護フィルムは円偏光板と積層した表面保護フィルムと同じものを用い、フィルムの遅相軸は平行になるようにした。
円偏光板Bの偏光子側面はPVA偏光子を貼り合わせたTACフィルム面であり、位相差層側面は1/4λ板のTACフィルム面である。
円偏光板Cの偏光子側面は液晶偏光子を設けたTACフィルム面であり、位相差層側面は1/4λ板のTACフィルム面である。
円偏光板Dの偏光子側面は偏光子面であり、位相差層側面は1/4λ板のTACフィルム面である。円偏光板Dでは表面保護フィルムに貼り合わせる直前にPVA偏光子転写用積層体の熱可塑性樹脂基材を剥離した。
円偏光板Eの偏光子側面は偏光子面であり、位相差層側面は保護コート面である。円偏光板Eでは表面保護フィルムに貼り合わせる直前にPVA偏光子転写用積層体の熱可塑性樹脂基材を剥離し、その後、二軸延伸ポリエステルフィルム(東洋紡株式会社製A4100)を剥離した。
ハードコートフィルムのサンプル評価と同様にして、表面保護フィルムと円偏光板の積層体に対して屈曲半径3.0mmの耐屈曲性を評価した。評価においてはハードコートを屈曲の内側にした。
得られた折りたたみ型ディスプレイのモデルを屈曲半径3.0mmにし、上記積層体の耐屈曲性と同様に20万回の耐屈曲性試験を行った。表面保護フィルム1~20を用いた実施例1~20のものは、いずれも折り跡、クラック等は認められず優れた耐屈曲性を示した。
11: 屈曲半径
2 : 折りたたみ型ディスプレイの表面保護フィルム用ポリエステルフィルム
21: 折りたたみ部
22: 屈曲方向(折りたたみ部と直交する方向)
Claims (7)
- 少なくとも表面保護フィルム、偏光子、位相差層を有する折りたたみ型ディスプレイであり、表面保護フィルムが下記条件を満足する厚みが10~80μmであるポリエステルフィルムである折りたたみ型ディスプレイ。
(1)屈曲方向の屈折率が1.590~1.620
(2)折りたたみ部の方向の屈折率が1.670~1.700
(3)厚み方向の屈折率が1.520以下
(4)密度が1.380g/cm3以上
(ここで、屈曲方向とは、ポリエステルフィルムを折りたたむ際の折りたたみ部と直交する方向をいう。) - 前記ポリエステルフィルムの屈曲方向の弾性率が2.7GPa以下, 折りたたみ部の方向の弾性率が4.5GP以上である請求項1に記載の折りたたみ型ディスプレイ。
- 前記ポリエステルフィルムの少なくとも片面上にハードコート層を有し、ハードコート層が少なくとも折りたたみ型ディスプレイの表面に位置している請求項1又は2に記載の折りたたみ型ディスプレイ。
- 前記の少なくとも片面上にハードコート層を有するポリエステルフィルムの全光線透過率が85%以上、ヘイズが3%以下である請求項3に記載の折りたたみ型ディスプレイ。
- 折りたたみ型ディスプレイの折りたたみ部を介して連続した単一の表面保護フィルムが配されている請求項1~4のいずれかに記載の折りたたみ型ディスプレイ。
- 前記位相差板が、1/4λ板である請求項1~5のいずれかに記載の折りたたみ型ディスプレイ。
- 請求項6に記載の折りたたみ型ディスプレイを有する携帯端末機器。
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CN113874767A (zh) | 2021-12-31 |
EP3978967A1 (en) | 2022-04-06 |
KR20220013394A (ko) | 2022-02-04 |
TW202101031A (zh) | 2021-01-01 |
JP6940004B2 (ja) | 2021-09-22 |
US20220236468A1 (en) | 2022-07-28 |
EP3978967A4 (en) | 2023-07-12 |
JPWO2020241313A1 (ja) | 2021-09-13 |
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