WO2013031511A1 - 偏光板離型フィルム用二軸配向ポリエステルフィルムおよびそれを用いた積層体、ならびに、偏光板の製造方法 - Google Patents
偏光板離型フィルム用二軸配向ポリエステルフィルムおよびそれを用いた積層体、ならびに、偏光板の製造方法 Download PDFInfo
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- WO2013031511A1 WO2013031511A1 PCT/JP2012/070313 JP2012070313W WO2013031511A1 WO 2013031511 A1 WO2013031511 A1 WO 2013031511A1 JP 2012070313 W JP2012070313 W JP 2012070313W WO 2013031511 A1 WO2013031511 A1 WO 2013031511A1
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- film
- polyester film
- polarizing plate
- biaxially oriented
- width
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C33/00—Moulds or cores; Details thereof or accessories therefor
- B29C33/56—Coatings, e.g. enameled or galvanised; Releasing, lubricating or separating agents
- B29C33/68—Release sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C55/00—Shaping by stretching, e.g. drawing through a die; Apparatus therefor
- B29C55/02—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets
- B29C55/10—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial
- B29C55/12—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial
- B29C55/14—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial successively
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C55/00—Shaping by stretching, e.g. drawing through a die; Apparatus therefor
- B29C55/02—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets
- B29C55/10—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial
- B29C55/12—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial
- B29C55/14—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial successively
- B29C55/143—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial successively firstly parallel to the direction of feed and then transversely thereto
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2067/00—Use of polyesters or derivatives thereof, as moulding material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2007/00—Flat articles, e.g. films or sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2011/00—Optical elements, e.g. lenses, prisms
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
Definitions
- the present invention relates to a biaxially oriented polyester film for a polarizing plate release film, which is suitably used for a polarizing plate having excellent optical properties in members for liquid crystal display applications and the like, and a method for producing the same.
- LCDs liquid crystal displays
- CTR cathode ray tube
- the visual inspection by the crossed Nicols method is common for the defect inspection of the polarizing plate.
- the crossed Nicols method is a method in which two polarizing plates are made to have a dark field with their orientation principal axes orthogonal, and a product to be measured is sandwiched between them to observe with transmitted light.
- the crossed Nicols method if there is a foreign matter or a defect in the polarizing plate, it appears as a bright spot. Therefore, the defect can be inspected by checking the bright spot.
- the biaxially oriented polyester film is often used as a release film in order to give an adhesive for attaching the polarizing plate to another member to the polarizing plate.
- this release film has optical anisotropy, light leakage occurs from a member in which a polarizing plate, a release film, and an adhesive are combined. This light leakage becomes an obstacle to the inspection by the crossed Nicols method, and there is a problem that it is easy to overlook foreign matters and defects. Further, if the release film has an optical defect, a bright spot derived from the optical defect of the release film is added, which becomes an obstacle to defect inspection. It has been known so far that foreign matters in the release film and scratches on the surface become bright spots during defect inspection.
- the biaxially oriented polyester film is advantageous when used as a polarizing plate release film because it can be easily thinned.
- Patent Document 1 when a polyester film is stretched, a phenomenon called bowing occurs due to the center portion being stretched with respect to the stretched end portion. Therefore, the biaxially oriented polyester film has birefringence (phase difference).
- phase difference phase difference
- Japanese Examined Patent Publication No. 39-029214 Japanese Patent Laid-Open No. 2007-213016 Japanese Patent Laid-Open No. 2004-237451 JP 2001-328159 A Japanese Patent Laid-Open No. 2004-18588 JP 2004-358742 A JP 2008-246665A
- a defect inspection apparatus disclosed in Patent Document 2 is known as an improvement of an automatic inspection instrument using the crossed Nicols method.
- This defect inspection apparatus has an inspection polarizing filter between the light source and the optical path of the camera.
- the birefringence of the film is adjusted by appropriately adjusting the relative angular position of the inspection polarizing filter so that the amount of light received in the background portion where there is no defect of visible light input to the camera is the minimum value. (Phase difference) is cancelled. Therefore, this defect inspection apparatus can inspect defects in the film with a polarizing plate in a crossed Nicol state.
- a polarizing plate is arranged so that the field of view at the time of crossed Nicol inspection becomes dark, regardless of a defect that causes a large light amount change. There is a need to. In this case, since the contrast difference is further reduced, detection becomes more difficult.
- Patent Document 7 proposes a cooling process after transverse stretching, and a cooling temperature in the cooling process is specified so that the orientation angle is 5 degrees or less over a width of 5 m. Has been.
- the present invention provides a biaxially oriented polyester film for polarizing plate release film that solves the above-described problems and has good cross-Nicol inspection properties for polarizing plates used especially for large screen TVs and can improve productivity. There is.
- the heat shrinkage rate in the longitudinal direction of the film after heat treatment at 150 ° C. for 30 minutes is 5 to 7%, and the heat shrinkage rate in the film width direction is 7 to 9% ( A biaxially oriented polyester film for releasing a polarizing plate according to 1) or (2).
- Step 1 A step of stretching a non-stretched polyester film in the longitudinal direction at a stretch ratio of 2.5 to 5 to obtain a uniaxially stretched polyester film.
- Step 2 The uniaxially stretched polyester film is stretched at a stretch ratio of 3 to 6 in the width direction and a stretch ratio in the width direction larger than the stretch ratio in the longitudinal direction.
- Obtaining A step of cooling the biaxially stretched polyester film at a film temperature of 25 to 45 ° C. and a film width shrinkage rate of 0.1 to 20% / min to obtain a cooled polyester film.
- Step 4) A step of heat-treating the cooled polyester film at a heat treatment temperature of 180 to 230 ° C. to obtain a biaxially oriented polyester film.
- a laminate comprising the polarizing plate releasing biaxially oriented polyester film according to any one of (1) to (8) provided on at least one side of a polarizer having a width of 1700 mm or more.
- Step 1 A method for producing a biaxially oriented polyester film for a polarizing plate release film according to any one of (1) to (8), comprising the following steps in the order.
- Step 1 A step of stretching a non-stretched polyester film in the longitudinal direction at a stretch ratio of 2.5 to 5 to obtain a uniaxially stretched polyester film.
- Step 2 The uniaxially stretched polyester film is stretched at a stretch ratio of 3 to 6 in the width direction and a stretch ratio in the width direction larger than the stretch ratio in the longitudinal direction.
- Obtaining A step of cooling the biaxially stretched polyester film at a film temperature of 25 to 45 ° C. and a film width shrinkage rate of 0.1 to 20% / min to obtain a cooled polyester film.
- Step 4) A step of heat-treating the cooled polyester film at a heat treatment temperature of 180 to 230 ° C. to obtain a biaxially oriented polyester film.
- Step 1) A step of stretching a non-stretched polyester film in the longitudinal direction at a stretch ratio of 2.5 to 5 to obtain a uniaxially stretched polyester film.
- Step 2 The uniaxially stretched polyester film is stretched at a stretch ratio of 3 to 6 in the width direction and a stretch ratio in the width direction larger than the stretch ratio in the longitudinal direction. Obtaining.
- Step 3 A step of cooling the biaxially stretched polyester film at a film temperature of 25 to 45 ° C. and a film width shrinkage rate of 0.1 to 20% / min to obtain a cooled polyester film.
- Step 4 A step of heat-treating the cooled polyester film at a heat treatment temperature of 180 to 230 ° C. to obtain a biaxially oriented polyester film.
- the present invention even when the inclination of the alignment principal axis with respect to the width direction is the same direction, variation in the inclination angle (orientation angle) of the alignment principal axis with respect to the width direction is suppressed, cross Nicol inspection property is good, and productivity is improved. It is possible to provide a biaxially oriented polyester film for polarizing plate release film that can improve (yield) and a method for producing the same.
- the polyester that can be suitably used in the present invention is not particularly limited as long as it is a polyester that becomes a high-strength film by molecular orientation, but preferably mainly includes polyethylene terephthalate and polyethylene-2,6-naphthalate. Particularly preferred is polyethylene terephthalate which is superior in price.
- polyester copolymer component other than ethylene terephthalate examples include diol components such as diethylene glycol, propylene glycol, neopentyl glycol, polyethylene glycol, p-xylylene glycol, and 1,4-cyclohexanedimethanol, adipine Films intended for dicarboxylic acid components such as acid, sebacic acid, phthalic acid, isophthalic acid, 5-sodium sulfoisophthalic acid, polyfunctional dicarboxylic acid components such as trimellitic acid and pyromellitic acid, and p-oxyethoxybenzoic acid It can be used as long as the physical properties are not impaired.
- dicarboxylic acid components such as acid, sebacic acid, phthalic acid, isophthalic acid, 5-sodium sulfoisophthalic acid, polyfunctional dicarboxylic acid components such as trimellitic acid and pyromellitic acid, and p-oxyethoxybenzoic acid It
- Such a polyester can be produced, for example, by the method shown below.
- a method in which a dicarboxylic acid component and a diol component are directly esterified, and then the product of this reaction is heated under reduced pressure to perform polycondensation while removing excess diol components For example, a dialkyl ester of a dicarboxylic acid is used as a component, and after transesterification with a diol component, polycondensation is performed in the same manner as described above.
- an alkali metal, an alkaline earth metal, manganese, cobalt, zinc, antimony, germanium, or a titanium compound can be used as a reaction catalyst as necessary.
- the polyester has an intrinsic viscosity of preferably 0.4 to 0.9, more preferably 0.5 to 0.7, and still more preferably 0.55 to 0.65.
- the biaxially oriented polyester film for polarizing plate release film of the present invention has an inclination angle (orientation angle) variation of the orientation main axis with respect to the width direction within 3.7 degrees and a film width of 1700 mm or more. is there. Moreover, it is preferable that the inclination of the orientation main axis with respect to the film width direction is the same direction.
- the orientation angle represents the angle of inclination of the orientation main axis.
- the orientation angle can be measured by evaluating the orientation by transmitting an ultrasonic pulse through the film in all directions and measuring the propagation speed.
- the orientation angle was defined as 0 degree when parallel to the film width direction, + for the clockwise inclination with respect to the film width direction, and-for the counterclockwise direction.
- the inclination of the orientation main axis with respect to the film width direction being the same direction defines that both ends in the film width direction of the stretched film show the same sign in the measurement of the inclination of the orientation main axis described above.
- the inclination of the orientation main axis is caused by the bowing phenomenon that occurs during the heat treatment process from the stretching process.
- the bowing phenomenon is caused by the fact that the film in the heat treatment process from the stretching process constitutes a catenary curve (catenary curve), so in the biaxially oriented polyester film, from the width direction center to the width direction end of the film.
- the inclination of the orientation main axis tends to increase as it goes.
- it has the inclination of the orientation principal axis of a reverse direction, respectively.
- orientation angle variation referred to in the present invention is defined as the maximum and minimum difference in the orientation angle at any position in the film measured as described above.
- the orientation angle variation is more preferably within 3.5 degrees, and further preferably within 3.2 degrees.
- the biaxially oriented polyester film for releasing the polarizing plate of the present invention is collected from a film having an inclination angle (orientation angle) of the orientation main axis with respect to the film width direction of 3.7 degrees or less over a width of at least 5 m. Since productivity can be improved, it is preferable.
- Alignment angle variation is a cause of variation in the amount of light leakage in a normal part without defects in the film when the film is in a crossed Nicol state.
- This variation in the amount of light leakage is a variation in the amount of received light in the background portion where there is no defect in the background portion where there is no defect in the crossed Nicol inspection device described in “(9) Evaluation with a crossed Nicol inspection device” described later. Can be confirmed.
- the inspection property changes according to the position of the film (according to the variation in the orientation angle), and the oversight of the defect may occur. An example is shown below.
- Detection test 1 Sample: A polyester film having surface defects generated when a polyester film is processed at room temperature. However, this polyester film is a small piece, and there is almost no variation in the orientation angle in the film plane.
- Measuring device The crossed Nicol tester shown in “(9) Evaluation with a crossed Nicol tester” described later. Baseline: In the crossed Nicols tester, it is necessary to determine the baseline of the amount of light received in the background portion without any defects at the time of inspection.
- test 1A a test in which the baseline of the received light amount in the background portion without defects (light leakage amount in the normal portion without defects) is in the range of 10 to 30 in 256 gradations is set as test 1A, and the background portion without defects is A test in which the baseline of the amount of received light was in the range of 30 to 50 with 256 gradations was designated as Test 1B.
- the baseline was adjusted by adjusting both the angle of the second polarizing filter on the light receiving means side and the angle of the first polarizing filter installed on the illumination side.
- Test result When the sample was inspected under the conditions of Test 1A, the surface defect portion of the film showed the amount of light received in the background portion having no defect as high as 40 from the baseline.
- the surface defect portion of the film showed the amount of light received in the background portion having no defect as high as 17 from the baseline.
- the inspection property is high (sensitive).
- the test results are shown in FIG. In FIG. 1, the black portion indicates that the received light amount is small in the background portion without defects, and the white portion indicates that the received light amount is large in the background portion without defects.
- the orientation angle varies depending on the position of the film, so that the baseline of the received light amount in the background portion without any defects changes. Specifically, even if the baseline of the received light amount in the background portion where there is no defect is set to 20 at the position where the orientation angle is 0 degree, there is no defect at the position where the orientation angle is other than 0 degree. The baseline of the received light amount in the background portion changes from 20. Then, when the baseline of the amount of light received in the background portion having no defect changes, the inspection property changes.
- Detection test 2 Sample A polyester film having a surface defect generated during production of a polyester film (particularly during heat stretching). However, this polyester film is a small piece, and there is almost no variation in the orientation angle in the film plane.
- Measuring device The crossed Nicol tester shown in “(9) Evaluation with a crossed Nicol tester” described later.
- Baseline In the crossed Nicols tester, it is necessary to determine the baseline of the amount of light received in the background portion without any defects at the time of inspection. Therefore, a test in which the baseline of the received light amount in the background portion having no defect is in a range of 10 to 30 in 256 gradations is set as Test 2A, and the baseline of the received light amount in the background portion without defects is set to 30 in 256 gradations.
- Tests in the range of ⁇ 50 were designated as test 2B.
- the baseline was adjusted by adjusting both the angle of the second polarizing filter on the light receiving means side and the angle of the first polarizing filter installed on the illumination side.
- Test result When the sample was inspected under the conditions of Test 2A, the surface defect of the film showed the amount of light received in the background portion having no defect as high as 80 from the baseline. On the other hand, when the same sample was inspected under the conditions of Test 2B, the surface defect portion of the film showed the amount of light received in the background portion having no defect as high as 70 from the baseline.
- the measured size of surface defects, under the conditions of the test 2A is observed as large as 0.475 mm 2, under the conditions of the test 2A is observed as large as 0.588mm 2.
- test results are shown in FIG. Conclusion: From the above test results, it was shown that the testability (particularly, the magnitude of the defect indicated as a measured value) changes depending on the baseline of the amount of light received in the background portion where there is no defect. Then, if there is a variation in the orientation angle in the plane of the polyester film, the baseline of the amount of light received at the background portion where there is no defect changes depending on the position of the film. Then, when the baseline of the amount of light received in the background portion having no defect changes, the inspection property changes.
- the biaxially oriented polyester film of the present invention preferably has an orientation angle variation (hereinafter referred to as MD orientation angle unevenness) of 1.5 degrees or less with respect to the longitudinal direction of the film.
- MD orientation angle unevenness means that the orientation angles at both ends in the film width direction are measured at 10 points every 1000 mm in the film longitudinal direction, and the absolute value of the difference between the maximum value and the minimum value at each film end is measured. Find the value and define it as the value with the larger absolute value.
- the MD orientation angle unevenness is preferably 1.5 degrees or less, more preferably 1.2 degrees or less, and further preferably 1.0 degrees or less.
- the absolute value of the orientation angle at the film end position decreases in the biaxially oriented polyester film of the present invention. It is preferable to form a film.
- the biaxially oriented polyester film of the present invention needs to have a film width of at least 1700 mm.
- the orientation angle takes a behavior that increases with respect to the distance from the center of the formed film, it becomes difficult to suppress the variation in the orientation angle and the orientation angle as the film width increases. Therefore, conventionally, in a biaxially oriented polyester film having a film width of 1700 mm or more, the variation in the orientation angle could not be 3.7 degrees or less. Since the biaxially oriented polyester film of the present invention has a film width of at least 1700 mm or more and an orientation angle variation of 3.7 degrees or less, the polarization of a large screen (specifically, 32 inches or more) LCD It is preferably used for a release film for plate inspection.
- a film width of 1900 mm or more is more preferable because it can be suitably used for LCDs for larger screens, and productivity is improved.
- the upper limit of the film width is not particularly limited, but the film width is preferably 10,000 mm or less from the viewpoint of manufacturing equipment cost.
- the biaxially oriented polyester film of the present invention preferably has the same orientation of the orientation main axis with respect to the film width direction.
- the inclination of the orientation main axis tends to increase as it goes from the center in the width direction to the end in the width direction of the film.
- the two directions from the center in the width direction toward the end in the width direction have inclinations of the orientation main axes in opposite directions. Therefore, in order to widen the orientation angle variation to the minimum, the width is centered so that the center in the width direction of the film to be widened is the same as the center in the width direction of the film after being widened. .
- the product can be collected only in the central part in the width direction of the film by this width measurement.
- chamfering is performed so that the inclinations are in the same direction, variations in orientation angle and MD orientation angle unevenness tend to increase.
- the biaxially oriented polyester film of the present invention is biaxially oriented with good productivity and good testability because the variation in the orientation angle is small even when the orientation of the orientation main axis with respect to the film width direction is chamfered in the same direction. Polyester can be obtained.
- the biaxially oriented polyester film of the present invention preferably has a thermal shrinkage of 5 to 7% and 7 to 9% in the film longitudinal direction and film width direction after heat treatment at 150 ° C. for 30 minutes, respectively. .
- they are 5.5 to 6.5% and 7.5 to 8.5%, respectively.
- the heat shrinkage rate can be adjusted by the relaxation rate in the heat treatment and the heat treatment temperature.
- annealing is separately performed after film formation. Since it is necessary to perform the treatment, productivity and efficiency are lowered, which is not preferable.
- the biaxially oriented polyester film for polarizing plate release film of the present invention preferably has a haze value of 7 to 13%. Preferably it is 8 to 12%, more preferably 9 to 11%.
- the haze value is less than 7%, the reflected light is too strong when inspecting the polarizing plate.
- the haze value exceeds 13% the reflected light is weak, which may hinder the inspection.
- the reflected light under crossed Nicol is difficult to distinguish the difference between the defective portion and the formation (background portion) regardless of whether the reflected light is strong or weak. This effect is particularly noticeable when visual inspection is performed.
- the reflected light is strong when the haze is low, and the uneven brightness of the texture (background part) is emphasized, making it difficult to distinguish between the defective part and the texture (background part), and scattering when the haze is high.
- the light is strong and the luminescent spot of the defective part becomes ambiguous and the detectability is lowered.
- the haze value of the film is in the above range.
- the film of the present invention may be a single layer or a composite film composed of two or more layers, but it is particularly suitable when the film has a three-layer composite film in order to keep the haze value of the film within the above range.
- the polymer composition of the layer constituting the film surface (lamination part), the particle type or particle content to be contained may be different, and the A / B / C structure may be used.
- An A / B / A configuration may be used in which the composition, the contained particle type, or the particle content is the same.
- composition of A / B / A having the same composition of the polymer composition of the layer (lamination part) constituting the film surface and the contained particle type or particle content is simple in terms of equipment and is preferable from the viewpoint of productivity. . Furthermore, when the three-layer composite film has an A / B / A configuration, it is preferable that the thickness of both layers constituting the film surface side is substantially the same because quality design is easy. Further, the thickness of the layer (laminate) constituting the film surface is preferably 0.5 to 2.5 ⁇ m, and particularly preferably 1.0 to 2.0 ⁇ m.
- a method of containing inert particles in the film is preferably used.
- the film of the present invention is a three-layer composite film
- the haze value is set to a desired range. This is preferable because it can be performed.
- inorganic particles such as spherical silica, aluminum silicate, titanium dioxide, calcium carbonate, and other organic polymer particles include crosslinked polystyrene resin particles, crosslinked silicone resin particles, crosslinked acrylic resin. Particles, crosslinked styrene-acrylic resin particles, crosslinked polyester particles, polyimide particles, melamine resin particles and the like are preferably used. These 1 type (s) or 2 or more types can also be selected and used.
- an inert particle-containing slurry of ethylene glycol, which is a glycol component, is prepared, and the inert particle-containing slurry is added after the ester exchange before polycondensation or at the oligomer stage after esterification.
- the polycondensation reaction By carrying out the polycondensation reaction, inert particle-containing polyethylene terephthalate can be obtained.
- the slurry of inert particles before addition can be dispersed by a sand grinder or the like, separated by coarse particles by centrifugal sedimentation, or subjected to high-precision filtration to make the particle size distribution uniform and coarse particles. Can be effectively removed to reduce the coarse protrusions of the film.
- the layer (laminate) constituting the film surface has an average particle diameter of 0.5 to 1.5 ⁇ m, preferably 0. It is preferable that 0.2 to 1.0% by weight, more preferably 0.3 to 0.8% by weight of inert particles of 0.8 to 1.3 ⁇ m are contained.
- the layer (base layer part) that does not constitute the film surface contains 0.02 to 0.1% by weight of inert particles having an average particle size of 0.5 to 1.5 ⁇ m, preferably 0.8 to 1.3 ⁇ m.
- the inert particle species contained in the layer (laminate portion) constituting the film surface and the layer (base layer portion) not constituting the film surface be the same because production facilities can be simplified.
- the thickness unevenness in the film longitudinal direction is preferably less than 2.0 ⁇ m, more preferably 0.5 to 1.5 ⁇ m, It is particularly preferable that the particle diameter is ⁇ 1.2 ⁇ m.
- the thickness unevenness in the film longitudinal direction referred to in the present invention represents a value measured by the method described later in “(5) thickness unevenness in the film longitudinal direction”. When the thickness unevenness exceeds 1.5 ⁇ m, the unevenness of the intensity of light leaking from the polarizing plate in the crossed Nicol method for inspecting the polarizing plate becomes strong, which may hinder the inspection.
- the thickness unevenness exceeds 2.0 ⁇ m, stretching unevenness often occurs, and since the texture (background portion) is not uniform due to the stretching unevenness, the crossed Nicols inspection property is remarkably deteriorated and the polarizing plate is released. It is not preferred as a biaxially oriented polyester film for film. On the other hand, in order to manufacture a film having a thickness unevenness of 0.5 ⁇ m or less, production management becomes complicated, which is not preferable.
- the thickness of the film of the present invention is preferably 25 to 70 ⁇ m, more preferably 30 to 50 ⁇ m, and still more preferably 35 to 45 ⁇ m. When the thickness of the film is within this range, it is easy to adjust the haze value of the film within the above range, which is preferable.
- the biaxially oriented polyester film for polarizing plate release film of the present invention can be obtained by, for example, stretching an unstretched film in the longitudinal direction, then stretching in the transverse direction, and heat-treating it through a cooling step, and in particular, the bowing phenomenon.
- the film temperature is cooled to 25 to 45 ° C. in the cooling process, and the film width shrinks in the cooling process. It is important to heat-treat after controlling the speed at 0.1 to 20% / min.
- the mechanism that can lower the orientation angle by controlling the width shrinkage rate in addition to the temperature in the cooling step after stretching is cooled from the transverse stretching step.
- the width shrinkage rate By controlling the width shrinkage rate during the transitional period when the film temperature decreases over the process, the lateral orientation relaxation is physically suppressed, or the width shrinkage in the cooling process is physically suppressed from acting on the film immediately after the stretching process.
- the bowing phenomenon can be sufficiently suppressed more than in the past.
- the width shrinkage rate of the film in the cooling step is preferably 0.1% to 20% / min, and preferably 0.2% to 18%. % / Min is more preferable. If the width shrinkage rate is less than 0.1% / min, the film tension due to the suppression of the width shrinkage of the film is affected, the film forming property is deteriorated, and the film is torn. On the other hand, if the width shrinkage rate is greater than 20% / min, the effect of suppressing orientation relaxation due to the width shrinkage of the film is small, and the suppression of the bowing phenomenon is insufficient.
- the width reduction speed V1 (% / min) of the film in the cooling process shown here is the film width W1 (mm) immediately after entering the cooling process after passing through the transverse stretching process, and after passing through the cooling process.
- V1 (W1-W2) / W1 ⁇ 1 / T1 Formula (1)
- the passing time of the cooling step is preferably 10 seconds or more, and more preferably 15 seconds or more.
- the upper limit of the passage time of the cooling step is not particularly limited, it is preferably 60 seconds or less because productivity is improved.
- the polyester film of the present invention is preferably obtained by a method having the following steps in that order.
- Step 1 A step of stretching a non-stretched polyester film in the longitudinal direction at a stretch ratio of 2.5 to 5 to obtain a uniaxially stretched polyester film.
- Step 2 The uniaxially stretched polyester film is stretched at a stretch ratio of 3 to 6 in the width direction and a stretch ratio in the width direction larger than the stretch ratio in the longitudinal direction.
- Step 3) A step of cooling the biaxially stretched polyester film at a film temperature of 25 to 45 ° C. and a film width shrinkage rate of 0.1 to 20% / min to obtain a cooled polyester film.
- Step 4) A step of heat-treating the cooled polyester film at a heat treatment temperature of 180 to 230 ° C. to obtain a biaxially oriented polyester film.
- the polyester obtained by the well-known method is dried as needed, supplied to an extruder, and filtered with a filter. Since a small foreign substance also becomes a film defect, it is effective to use a high-accuracy filter that collects 95% or more of a foreign substance of 5 ⁇ m or more, for example. Subsequently, it is melt-extruded into a sheet using a T-type die and the like, and cooled and solidified on a casting roll to obtain an unstretched film.
- a uniaxially stretched polyester film is obtained by stretching the unstretched film in the longitudinal direction at a stretch ratio of 2.5 to 5 times.
- the stretching in the longitudinal direction is preferably performed at a stretching temperature of 90 to 130 ° C. in one step or in multiple steps.
- the stretching temperature is preferably 100 to 120 ° C. and the stretching ratio is preferably 3 to 4 times from the viewpoint of suppressing the bowing phenomenon and thickness unevenness in the film longitudinal direction, and the stretching is performed in two or more stages from the viewpoint of preventing stretching unevenness and scratches. It is preferable.
- a biaxially stretched polyester film is obtained by stretching the uniaxially stretched polyester film at a stretch ratio of 3 to 6 times in the width direction and a stretch ratio in the width direction larger than the stretch ratio in the longitudinal direction.
- the stretching in the width direction is preferably performed at a stretching temperature of 90 to 130 ° C. When the stretching temperature is lower than 90 ° C. and the stretching ratio is larger than 6 times, the film is easily broken. More preferably, the stretching temperature is 100 to 120 ° C., and the stretching ratio is 4 to 5 times.
- the stretching ratio in the width direction is larger than the stretching ratio in the longitudinal direction. If the stretching ratio in the width direction is larger than the stretching ratio in the longitudinal direction, the molecular orientation in the film tends to be inclined in the longitudinal direction, and it may be difficult to suppress the orientation angle variation.
- the biaxially oriented polyester film for polarizing plate release film of the present invention is produced, it is subjected to lateral stretching after longitudinal stretching.
- longitudinal stretching is performed after transverse stretching, the molecules are mainly oriented strongly in the TD direction after transverse stretching, but when longitudinal stretching is performed thereafter, the molecules are also oriented in the MD direction, resulting in a large variation in orientation angle. is there.
- the film temperature in the cooling step is 25 to 45 ° C., because lateral orientation relaxation due to width shrinkage can be suppressed and the bowing phenomenon can be suppressed. More preferably, it is 30 to 40 ° C.
- the film temperature in the cooling step is higher than 45 ° C., the tension due to the film width shrinkage affects the film forming property, and the effect of suppressing the lateral orientation relaxation may not be sufficiently obtained. It is not preferable that the film temperature in the cooling step is cooled to less than 20 ° C., because the productivity deteriorates.
- Examples of the method for cooling the polyester film include an air cooling method using a tenter that performs heat treatment, an air cooling method in which hot air is blocked by a shielding plate such as an aluminum plate above and below the heat treatment region, and a cooling method using a roll.
- the air-cooling method with a heat-treating tenter all zones are connected in the longitudinal direction, so there is a case where the film temperature cannot be sufficiently cooled due to temperature differences in the vertical and width directions of the film due to the free flow of high-temperature air such as an accompanying air flow. is there. In that case, it is possible to cope with this by sending compressed air or the like and actively cooling it.
- the number of rolls to be used and the set temperature are not limited, but it is preferable to cool by using a plurality of rolls.
- the roll temperature is preferably 20 to 45 ° C, more preferably 30 to 40 ° C.
- the width reduction rate of the film is 0.1 to 20% / min. If the width shrinkage rate is less than 0.1% / min, the film tension due to the suppression of the width shrinkage of the film is affected, the film forming property is deteriorated, and the film is torn. On the other hand, when the width shrinkage rate is greater than 20% / min, the effect of suppressing orientation relaxation due to the width shrinkage of the film is small, and the suppression of the bowing phenomenon may be insufficient.
- the width shrinkage rate of the film is more preferably 0.2 to 18% / min.
- the passing time of the cooling step is preferably 10 seconds or longer, more preferably 15 seconds or longer.
- the upper limit of the passage time of the cooling step is not particularly limited, it is preferably 60 seconds or less because productivity is improved.
- the width shrinking speed can be set from the cooling process length and the film forming speed, and can be realized by various methods. Specifically, in the air-cooling method in the tenter, the width reduction speed can be set to a desired value by gripping both ends with clips and adjusting the rail width.
- the cooled polyester film is heat-treated at a heat treatment temperature of 180 to 230 ° C. to obtain a biaxially oriented polyester film.
- a heat treatment temperature 180 to 230 ° C.
- the heat treatment becomes insufficient, and the heat shrinkage rate in the film longitudinal direction and film width direction after heat treatment at 150 ° C for 30 minutes is 5 to 7% and 7 to 9%, respectively. It may be difficult to fit within the range.
- the heat treatment temperature is higher than 230 ° C., the orientation by thermal crystallization advances, and it may be difficult to keep the variation of the tilt angle (orientation angle) of the orientation main axis with respect to the film width direction within 3.7 degrees. is there.
- the temperature difference between the top and bottom of the film is preferably 1 to 20 ° C., more preferably 1 to 10 ° C., and further preferably 1 to 5 ° C.
- the physical properties in the width direction of the film particularly the mechanical properties or the heat shrinkage rate, may be nonuniform.
- the relaxation treatment may be performed in either the lateral direction or the longitudinal direction, or may be performed in the lateral direction and the longitudinal direction simultaneously or separately.
- the relaxation rate is preferably 1 to 20%, more preferably 1 to 10% with respect to the entire width of the film, it is effective for obtaining a film having excellent thermal dimensional stability.
- the polyester film of the present invention is suitably used as a release film for a large-size polarizing plate. Specifically, it is preferably used in the following manner.
- the polyester film of the present invention is provided on at least one side of a polarizer having a width of 1700 mm or more to form a laminate.
- the laminate is preferably a laminate in which “the polyester film of the present invention / adhesive layer A / polarizer / adhesive layer B / protective sheet” is provided in that order, and more preferably, “the present invention”.
- polyester film / silicone layer / adhesive layer A / polarizer / adhesive layer B / protective sheet in that order.
- a well-known material can be used as a silicone layer, an adhesion layer, a polarizer, and a protective sheet.
- the laminate is inspected. Since the polyester film of the present invention is used for the laminate, good testability is obtained. Thereafter, the polyester film of the present invention is peeled from the laminate to obtain a polarizing plate.
- the polarizing plate refers to a member having at least a polarizer.
- polyester film of the present invention When the polyester film of the present invention is peeled (removed) from “layer / adhesive layer A / polarizer / adhesive layer B / protective sheet” (laminate), “adhesive layer A / polarizer / adhesive layer B / protective sheet” becomes A polarizing plate provided in order is obtained.
- a silicone layer is peeled with the polyester film of this invention.
- the measurement method of characteristic values in the examples and comparative examples is as follows.
- the film to be measured for film width was spread on a table, and the width was measured with a metal scale (JIS grade 1).
- Film temperature was measured using a handy type radiation thermometer (IR-TA manufactured by Chino Corporation). Three points were measured uniformly in the film width direction, and the average value was taken as the measurement result. Height (Z direction) magnification: 50,000 times.
- ⁇ Light in the field of view (background part) entering the field of view is slightly strong or slightly weak, and there is unevenness in the amount of light at each position. I missed some of the shortcomings.
- X The light entering the field of view (background part) is strong or weak, and there is a clear unevenness in the amount of light for each position. I missed many shortcomings.
- the light from the illumination means 4 enters and transmits the film 1 to be inspected through the first polarizing plate, and is imaged by the light receiving means 5 through the second polarizing plate, It is output to the signal processing means 6.
- the evaluation of the variation in the amount of light received in the background portion without the base defect is based on the angle of the second polarizing plate on the light receiving means side as a uniform fixed, and the first polarizing plate angle installed on the illumination side is adjusted,
- the film sampled with the measurement width is used as the inspection object, and the amount of light received in the background portion with no defect in the entire inspection width is evaluated in 256 gradations.
- the difference between the maximum value and the minimum value of the amount of received light was confirmed, and this difference was evaluated as the variation in the amount of received light in the background without any defects.
- the present invention will be described in detail with reference to examples.
- Example 1 To 100 parts by weight of dimethyl terephthalate (DMT), 61 parts by weight (1.9 moles per 1 mole of DMT) of ethylene glycol and magnesium acetate tetrahydrate 0.05 parts by weight and 0.015 parts by weight of phosphoric acid are added and heated. Transesterification was conducted, 0.025 parts by mass of antimony trioxide was subsequently added, the temperature was raised by heating, and a polycondensation reaction was carried out by evacuation to obtain polyester pellets having an intrinsic viscosity of 0.63, substantially containing no particles.
- DMT dimethyl terephthalate
- calcium carbonate having a true specific gravity of 2.71 g / cm 3 and an average particle diameter of 1.0 ⁇ m was prepared to obtain a 10 wt% ethylene glycol slurry.
- This slurry was dispersed for 1 hour with a jet agitator and filtered with high accuracy through a filter having a collection efficiency of 95% of 5 ⁇ m or more.
- This slurry was added after transesterification, and subsequently a polycondensation reaction was performed in the same manner as described above to obtain a calcium carbonate-containing master pellet having an intrinsic viscosity of 0.63 and containing 1% of calcium carbonate having an average particle diameter of 1.0 ⁇ m. .
- polyester A containing 0.5% by weight of calcium carbonate
- polyester B containing 0.054% by weight of calcium carbonate
- polyesters A and B were each dried under reduced pressure at 160 ° C. for 8 hours, then supplied to separate extruders, melt-extruded at 275 ° C., filtered through a high-precision filter with a collection efficiency of 95% of 5 ⁇ m or more, The layers were merged and laminated in a rectangular three-layer merge block to form a three-layer laminate comprising polyester A / polyester B / polyester A. Thereafter, the film was cooled and solidified on a casting roll having a surface temperature of 25 ° C. by using an electrostatic application casting method through a slit die maintained at 285 ° C. to obtain an unstretched film.
- This unstretched film was first stretched 3.4 times in the longitudinal direction with a roll heated to 103 ° C. and a radiation heater. Subsequently, the film was stretched 4.4 times at 105 ° C. in the width direction by a tenter. Then, it cooled so that the film temperature might be 35 degreeC with the width shrinkage speed
- Examples 2-12, Comparative Examples 1-4 A biaxially oriented polyester film consisting of three layers was obtained in the same manner as in Example 1 except that the film forming conditions such as the stretching conditions, the cooling conditions, the heat treatment temperature, the width shrinkage rate of the cooling process, and the sampling width were changed. The obtained results are shown in Table 1-1 and Table 1-2.
- the variation of the inclination angle (orientation angle) of the orientation main axis with respect to the film width direction is within 3.7 degrees, and in addition, the haze value of the film is 7 to 13%.
- the variation in the amount of light received in the background area where there are no defects in the crossed Nicols tester can be reduced, so even if inspection is performed using an automatic inspection device, defects are not missed or erroneous detection is reduced. It was.
- the light of the background (background part) is no longer too strong or too weak, so it is possible to confirm that inspections are improved and fewer defects are missed. It was.
- the film of the present invention has excellent crossed Nicols inspection properties, it can be suitably used for releasing a polarizing plate.
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Abstract
Description
(工程1)未延伸ポリエステルフィルムを、長手方向に延伸倍率が2.5~5倍で延伸して、一軸延伸ポリエステルフィルムを得る工程。
(工程2)前記一軸延伸ポリエステルフィルムを、幅方向に延伸倍率が3~6倍、かつ、幅方向の延伸倍率が長手方向の延伸倍率よりも大きい延伸倍率で延伸して、二軸延伸ポリエステルフィルムを得る工程。
(工程3)前記二軸延伸ポリエステルフィルムを、フィルム温度を25~45℃、フィルムの幅縮み速度が0.1~20%/minにて冷却して、冷却されたポリエステルフィルムを得る工程。
(工程4)前記冷却されたポリエステルフィルムを、熱処理温度が180~230℃にて熱処理して、二軸配向ポリエステルフィルムを得る工程。
(工程1)未延伸ポリエステルフィルムを、長手方向に延伸倍率が2.5~5倍で延伸して、一軸延伸ポリエステルフィルムを得る工程。
(工程2)前記一軸延伸ポリエステルフィルムを、幅方向に延伸倍率が3~6倍、かつ、幅方向の延伸倍率が長手方向の延伸倍率よりも大きい延伸倍率で延伸して、二軸延伸ポリエステルフィルムを得る工程。
(工程3)前記二軸延伸ポリエステルフィルムを、フィルム温度を25~45℃、フィルムの幅縮み速度が0.1~20%/minにて冷却して、冷却されたポリエステルフィルムを得る工程。
(工程4)前記冷却されたポリエステルフィルムを、熱処理温度が180~230℃にて熱処理して、二軸配向ポリエステルフィルムを得る工程。
(工程1)未延伸ポリエステルフィルムを、長手方向に延伸倍率が2.5~5倍で延伸して、一軸延伸ポリエステルフィルムを得る工程。
(工程2)前記一軸延伸ポリエステルフィルムを、幅方向に延伸倍率が3~6倍、かつ、幅方向の延伸倍率が長手方向の延伸倍率よりも大きい延伸倍率で延伸して、二軸延伸ポリエステルフィルムを得る工程。
(工程3)前記二軸延伸ポリエステルフィルムを、フィルム温度を25~45℃、フィルムの幅縮み速度が0.1~20%/minにて冷却して、冷却されたポリエステルフィルムを得る工程。
(工程4)前記冷却されたポリエステルフィルムを、熱処理温度が180~230℃にて熱処理して、二軸配向ポリエステルフィルムを得る工程。
[1]検出テスト1
・サンプル:常温にてポリエステルフィルムを加工した際に発生した表面欠点を有するポリエステルフィルム。ただし、このポリエステルフィルムは小片であり、フィルム面内において配向角のバラツキはほとんど無いものである。
・測定装置:後に述べる「(9)クロスニコル検査器による評価」にて示したクロスニコル検査器。
・ベースライン:クロスニコル検査器では、検査に際して、欠点がない背景部分での受光量のベースラインを定める必要がある。そこで、欠点がない背景部分での受光量のベースライン(欠点の無い正常部分の光漏れ量)を256階調で10~30の範囲としたテストをテスト1Aとし、欠点がない背景部分での受光量のベースラインを256階調で30~50の範囲としたテストをテスト1Bとした。なお、ベースラインの調整は、受光手段側の第2の偏光フィルターの角度、照明側に設置されている第1の偏光フィルター角度の両方を調整することによって行った。
・テスト結果:テスト1Aの条件で、サンプルを検査したところ、フィルムの表面欠点部では、ベースラインから40ほど高い欠点がない背景部分での受光量を示した。一方、テスト1Bの条件で、同一のサンプルを検査したところ、フィルムの表面欠点部では、ベースラインから17ほど高い欠点がない背景部分での受光量を示した。なお、欠点がない背景部分での受光量のベースラインから高い欠点がない背景部分での受光量を示すほど、検査性は高い(鋭敏である)。テスト結果を図1に示す。図1において、黒い部分は欠点がない背景部分での受光量が小さいことを示し、白い部分は欠点がない背景部分での受光量が大きいことを示す。
・結論:上記のテスト結果より、欠点がない背景部分での受光量のベースラインによって、検査性が変化することが示された。そして、ポリエステルフィルムの面内において配向角のバラツキが存在すると、フィルムの位置によって配向角にバラツキがあるため、欠点がない背景部分での受光量のベースラインが変化する。具体的には、配向角が0度の位置において、欠点がない背景部分での受光量のベースラインを20となるように設定せしめても、配向角が0度以外の位置では、欠点がない背景部分での受光量のベースラインが20から変化する。そして、欠点がない背景部分での受光量のベースラインが変化すると、検査性が変化することになる。
・サンプル:ポリエステルフィルム製造時(特に加熱延伸時)発生した表面欠点を有するポリエステルフィルム。ただし、このポリエステルフィルムは小片であり、フィルム面内において配向角のバラツキはほとんど無いものである。
・測定装置:後に述べる「(9)クロスニコル検査器による評価」にて示したクロスニコル検査器。
・ベースライン:クロスニコル検査器では、検査に際して、欠点がない背景部分での受光量のベースラインを定める必要がある。そこで、欠点がない背景部分での受光量のベースラインを256階調で10~30の範囲としたテストをテスト2Aとし、欠点がない背景部分での受光量のベースラインを256階調で30~50の範囲としたテストをテスト2Bとした。なお、ベースラインの調整は、受光手段側の第2の偏光フィルターの角度、照明側に設置されている第1の偏光フィルター角度の両方を調整することによって行った。
・テスト結果:テスト2Aの条件で、サンプルを検査したところ、フィルムの表面欠点部では、ベースラインから80ほど高い欠点がない背景部分での受光量を示した。一方、テスト2Bの条件で、同一のサンプルを検査したところ、フィルムの表面欠点部では、ベースラインから70ほど高い欠点がない背景部分での受光量を示した。また、表面欠点の大きさを測定したところ、テスト2Aの条件下では0.475mm2ほどの大きさとして観察され、テスト2Aの条件下では0.588mm2ほどの大きさとして観察された。テスト結果を図1に示す。
・結論:上記のテスト結果より、欠点がない背景部分での受光量のベースラインによって、検査性(特に測定値として示される欠点の大きさ)が変化することが示された。そして、ポリエステルフィルムの面内において配向角のバラツキが存在すると、フィルムの位置によって、欠点がない背景部分での受光量のベースラインが変化する。そして、欠点がない背景部分での受光量のベースラインが変化すると、検査性が変化することになる。
V1=(W1-W2)/W1 × 1/T1 式(1)
また、本発明の偏光板離型フィルム用二軸配向ポリエステルフィルムを製造するに際し、冷却工程においてフィルムは温度が低下した状態である程度の時間を経ることが重要である。この理由としては、以下のように推測している。前述したように冷却工程では幅縮みをする際に配向緩和が起こっていると考えられるが、フィルムを冷却することによって配向緩和を止めるには一定の時間が必要であると推測される。そのため、冷却工程の通過時間が不十分であると配向緩和を抑制できないため、ボーイング現象を抑制する効果が少ないと推測している。本発明の偏光板離型フィルム用二軸配向ポリエステルフィルムを製造するに際して、冷却工程の通過時間は、10秒間以上が好ましく、更に好ましくは15秒間以上である。冷却工程の通過時間の上限は特に限定されないが、60秒間以下であると生産性が良好となるため好ましい。
(工程1)未延伸ポリエステルフィルムを、長手方向に延伸倍率が2.5~5倍で延伸して、一軸延伸ポリエステルフィルムを得る工程。
(工程2)前記一軸延伸ポリエステルフィルムを、幅方向に延伸倍率が3~6倍、かつ、幅方向の延伸倍率が長手方向の延伸倍率よりも大きい延伸倍率で延伸して、二軸延伸ポリエステルフィルムを得る工程。
(工程3)前記二軸延伸ポリエステルフィルムを、フィルム温度を25~45℃、フィルムの幅縮み速度が0.1~20%/minにて冷却して、冷却されたポリエステルフィルムを得る工程。
(工程4)前記冷却されたポリエステルフィルムを、熱処理温度が180~230℃にて熱処理して、二軸配向ポリエステルフィルムを得る工程。
公知の方法で得られたポリエステルを、必要に応じて乾燥し、押出機に供給して、フィルターにより濾過する。小さな異物もフィルム欠点となるため、このフィルターには例えば5μm以上の異物を95%以上捕集する高精度のものを用いることが有効である。続いてT型口金等を用いてシート状に溶融押出し、キャスティングロール上で冷却固化せしめて未延伸フィルムを得る。
前記未延伸フィルムを、長手方向に延伸倍率が2.5~5倍で延伸することによって、一軸延伸ポリエステルフィルムを得る。長手方向への延伸は、90~130℃の延伸温度で1段階的に、もしくは多段階的に分けて延伸することが好ましい。ボーイング現象およびフィルム長手方向の厚みムラを抑える観点から、延伸温度は100~120℃、延伸倍率は3~4倍が好ましく、延伸ムラおよびキズを防止する観点から延伸は2段階以上に分けて行うことが好ましい。
前記一軸延伸ポリエステルフィルムを、幅方向に延伸倍率が3~6倍、かつ、幅方向の延伸倍率が長手方向の延伸倍率よりも大きい延伸倍率で延伸することによって、二軸延伸ポリエステルフィルムを得る。幅方向の延伸は、90~130℃の延伸温度で延伸することが好ましい。延伸温度が90℃よりも低く、延伸倍率が6倍よりも大きくなるとフィルムが破断しやすくなる。延伸温度は100~120℃、延伸倍率は4~5倍であるとより好ましい。
前記二軸延伸ポリエステルフィルムを、フィルム温度を25~45℃、フィルムの幅縮み速度が0.1~20%/minにて冷却することによって、冷却されたポリエステルフィルムを得る。
前記冷却されたポリエステルフィルムを、熱処理温度が180~230℃にて熱処理することによって、二軸配向ポリエステルフィルムを得る。熱処理温度が180℃未満では熱処理が不十分となり、熱収縮率を150℃30分間の条件で熱処理したのちのフィルム長手方向およびフィルム幅方向の熱収縮率がそれぞれ5~7%、7~9%の範囲に収めることが困難となる場合がある。熱処理温度が230℃より高いと、熱結晶化による配向が進むことにより、フィルム幅方向に対する配向主軸の傾きの角度(配向角)のバラツキが3.7度以内に収めることが困難となる場合がある。
測定対象のフィルムを台に広げ、幅を金尺(JIS1級)で測定した。
野村商事製配向性測定機(SST-4000)を用いて測定をする。試料となるフィルムの幅に対して両端部からA4サイズに切り出したサンプルの中点(105mm)を測定し、配向主軸がフィルム幅方向と平行である時を配向角0度であり、フィルム幅方向に対して時計回りの傾きを+、反時計回りを-とし、その絶対値を測定結果とした。
配向角バラツキは対象となる採取幅取りにおいて、最大値と最小値の差分の絶対値を測定結果とした。
JIS K7105(1981)に準じ、フィルム長手方向4cm×フィルム幅方向3.5cmの寸法に切り出したものをサンプルとし、ヘイズメータ(スガ試験機製HGM-2DP(C光用))を用いて測定する。フィルム幅方向に対して均等に3点測定し、その平均値を測定結果とした。
フィルム表面に、幅10mm、測定長約100mmとなるように2本のラインを引き、この2本のライン間の距離を23℃で測定しこれをL0とする。このフィルムサンプルを150℃のオーブン中に30分間、1.5gの荷重下で放置した後、再び2本のライン間の距離を23℃で測定しこれをL1とし、下式により熱収縮率を求めた。
熱収縮率(%)={(L0-L1)/L0}×100
フィルムの長手方法および幅方向についてそれぞれ3カ所の測定を行い、平均値を求めた。
安立電気製フィルム厚み連続測定器を用いて、長手方向に15m測定し、記録されたフィルム厚さチャートから、最大厚みと最小厚みの差を厚みむら(μm)として測定した。測定条件は下記の通り。
構成:K-306C広範囲電子マイクロメータ、K-310Cレコーダー、フィルム送り装置
検出器:3Rルビー端子、測定力:15g±5g
フィルム幅:45mm、測定長:15m、フィルム送り速度:3m/分。
JIS C2151(1990)に準じ、マイクロメーター(ミツトヨOMM-25)を用いてフィルム幅方向に対して均等に30点測定し、その平均値を測定結果とした。
ハンディ形放射温度計(株式会社チノー製IR-TA)を用いて、フィルム温度を測定した。フィルム幅方向に対して均等に3点測定し、その平均値を測定結果とした。
高さ(Z方向)拡大倍率:5万倍。
光源(ライトボックス)上に偏光板2枚を載せ、その間にポリエステルフィルムを置き、2枚の偏光板をフィルム全体がクロスニコル状態になるように合わせた状態とし、目視検査を行い、フィルム表面の欠点をマーキングした。検査は2名で行いクロスチェックをして欠点の見逃しの有無を確認し、以下の判断基準で評価した。
◎:目視検査に良好な地合(背景部分)であったため、欠点をほとんど見逃すことなく、検査することができた。
○:視界に入る地合(背景部分)の光がやや強かったり、やや弱かったり、位置ごとに軽微な光量ムラが存在したので、2時間程度続けて検査をしていると疲労感を感じるようになり、いくつかの欠点を見逃してしまった。
△:視界に入る地合(背景部分)の光がやや強かったり、やや弱かったり、位置ごとに光量ムラが存在したので、1時間程度でも続けて検査をしていると疲労感を感じるようになり、いくつかの欠点を見逃してしまった。
×:視界に入る地合(背景部分)の光が強かったり、弱かったり、位置ごとに明確な光量ムラが存在したので、1時間程度でも続けて検査をしていると疲労感を強く感じるようになり、多くの欠点を見逃してしまった。
本発明におけるクロスニコル検査性を評価する機器として、照明手段として250Wのメタルハライド(目白プレシジョン製 BMH-250A)及び角度調整が可能な第1の偏光板が設けられ、受光手段として分解能25μmのCCDカメラ(DALSA製 P3-80-8K-40)と角度調整が可能な第2の偏光板を組み合わせて複数配置されているクロスニコル検査器を使用した。装置の概要を図2に示す。
(9)クロスニコル検査器による評価にて用いた検査装置を用いて、カメラの検出感度は一定値として、フィルム10mを検査した。この際の検査性を確認し、以下の判断基準で評価した。
○:誤検知の多発による検査停止が発生することなく検査できた。検査後のフィルムを
目視にてクロスニコル検査したが、検査器での見逃しは殆ど確認できなった。
□:誤検知の多発による検査停止が発生することなく検査できた。検査後のフィルムを
目視にてクロスニコル検査したところ、検査器で検出出来ていない幾つかの欠点が確認された。
△:誤検知の多発による検査停止が検査開始から10m以内に発生した。
×:誤検知の多発による検査停止が検査開始から1m未満で発生した。
(2)配向主軸の傾き(配向角)と同様の手法に測定を行う。フィルム両端部位置で長手方向に1000mm毎に配向角を10点測定する。フィルム端部毎に測定値の最大値と最小値の差の絶対値を求め、絶対値が大きかった方の値をMD配向角ムラの測定結果とした。
以下、実施例で本発明を詳細に説明する。
ジメチルテレフタレート(DMT)100質量部に61重量部(DMT1モルに対して1.9モル)のエチレングリコールおよび酢酸マグネシウム・4水塩を0.05質量部、リン酸を0.015質量部加え加熱エステル交換を行い、引き続き三酸化アンチモン0.025質量部を加え、加熱昇温し真空化で重縮合反応を行い、粒子を実質的に含有しない、固有粘度0.63のポリエステルペレットを得た。
得られた結果を表1に示した。
延伸条件、冷却条件、熱処理温度、冷却工程の幅縮み速度、採取幅などの製膜条件を変えるほかは実施例1と同様に実施し、3層からなる二軸配向ポリエステルフィルムを得た。得られた結果を表1-1、表1-2に示した。
すなわち、本発明の態様とすることにより(特に、フィルム幅方向に対する配向主軸の傾きの角度(配向角)のバラツキを3.7度以内としたり、それに加えてフィルムのヘイズ値を7~13%とすることにより)、クロスニコル検査器における欠点がない背景部分での受光量バラツキを低減できたので、自動検査装置を用いて検査しても、欠点を見逃したり、誤検知することが少なくなった。また、目視で検査する場合においても、地合(背景部分)の光が強すぎたり、弱すぎたりすることがなくなったので、欠点を見逃すことが少なくなり、検査性が向上することが確認できた。
2 第1の偏光フィルター
3 第2の偏光フィルター
4 照明手段
5 受光手段
6 信号処理手段
Claims (12)
- フィルム幅方向に対する配向主軸の傾きの角度(配向角)のバラツキが3.7度以内であり、フィルム幅が1700mm以上である偏光板離型用二軸配向ポリエステルフィルム。
- フィルムのヘイズ値が7~13%である請求項1に記載の偏光板離型用二軸配向ポリエステルフィルム。
- 150℃、30分間の条件で熱処理したのちのフィルム長手方向の熱収縮率が5~7%であり、フィルム幅方向の熱収縮率が7~9%であることを特徴とする請求項1又は2に記載の偏光板離型用二軸配向ポリエステルフィルム。
- フィルム幅方向に対する配向主軸の傾きが同一方向であることを特徴とする請求項1~3のいずれかに記載の偏光板離型用二軸配向ポリエステルフィルム。
- フィルム長手方向の厚みムラが2.0μm未満である請求項1~4に記載の偏光板離型用二軸配向ポリエステルフィルム。
- 長手方向での配向角バラツキ(MD配向角ムラ)が1.5度未満である請求項1~5に記載の偏光板離型用二軸配向ポリエステルフィルム。
- フィルム幅方向に対する配向主軸の傾きの角度(配向角)が少なくとも5m幅にわたって3.7度以下であるフィルムから採取されることを特徴とする請求項1~6のいずれかに記載の偏光板離型用二軸配向ポリエステルフィルム。
- 以下の工程をその順に有する方法によって得られる請求項1~7のいずれかに記載の偏光板離型用二軸配向ポリエステルフィルム。
(工程1)未延伸ポリエステルフィルムを、長手方向に延伸倍率が2.5~5倍で延伸して、一軸延伸ポリエステルフィルムを得る工程。
(工程2)前記一軸延伸ポリエステルフィルムを、幅方向に延伸倍率が3~6倍、かつ、幅方向の延伸倍率が長手方向の延伸倍率よりも大きい延伸倍率で延伸して、二軸延伸ポリエステルフィルムを得る工程。
(工程3)前記二軸延伸ポリエステルフィルムを、フィルム温度を25~45℃、フィルムの幅縮み速度が0.1~20%/minにて冷却して、冷却されたポリエステルフィルムを得る工程。
(工程4)前記冷却されたポリエステルフィルムを、熱処理温度が180~230℃にて熱処理して、二軸配向ポリエステルフィルムを得る工程。 - 幅が1700mm以上の偏光子の少なくとも片側に、請求項1~8のいずれかに記載の偏光板離型用二軸配向ポリエステルフィルムを設けてなる積層体。
- 請求項9に記載の積層体から前記偏光板離型用二軸配向ポリエステルフィルムを剥離する、偏光板の製造方法。
- 請求項1~8のいずれかに記載の偏光板離型フィルム用二軸配向ポリエステルフィルムの製造方法であって、以下の工程をその順に有する二軸配向ポリエステルフィルムの製造方法。
(工程1)未延伸ポリエステルフィルムを、長手方向に延伸倍率が2.5~5倍で延伸して、一軸延伸ポリエステルフィルムを得る工程。
(工程2)前記一軸延伸ポリエステルフィルムを、幅方向に延伸倍率が3~6倍、かつ、幅方向の延伸倍率が長手方向の延伸倍率よりも大きい延伸倍率で延伸して、二軸延伸ポリエステルフィルムを得る工程。
(工程3)前記二軸延伸ポリエステルフィルムを、フィルム温度を25~45℃、フィルムの幅縮み速度が0.1~20%/minにて冷却して、冷却されたポリエステルフィルムを得る工程。
(工程4)前記冷却されたポリエステルフィルムを、熱処理温度が180~230℃にて熱処理して、二軸配向ポリエステルフィルムを得る工程。 - フィルム幅方向に対する配向主軸の傾きの角度(配向角)のバラツキが3.7度以内であり、フィルム幅が1700mm以上である二軸配向ポリエステルフィルムの製造方法であって、以下の工程をその順に有する二軸配向ポリエステルフィルムの製造方法。
(工程1)未延伸ポリエステルフィルムを、長手方向に延伸倍率が2.5~5倍で延伸して、一軸延伸ポリエステルフィルムを得る工程。
(工程2)前記一軸延伸ポリエステルフィルムを、幅方向に延伸倍率が3~6倍、かつ、幅方向の延伸倍率が長手方向の延伸倍率よりも大きい延伸倍率で延伸して、二軸延伸ポリエステルフィルムを得る工程。
(工程3)前記二軸延伸ポリエステルフィルムを、フィルム温度を25~45℃、フィルムの幅縮み速度が0.1~20%/minにて冷却して、冷却されたポリエステルフィルムを得る工程。
(工程4)前記冷却されたポリエステルフィルムを、熱処理温度が180~230℃にて熱処理して、二軸配向ポリエステルフィルムを得る工程。
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- 2012-08-09 JP JP2012552162A patent/JP6007792B2/ja active Active
- 2012-08-09 WO PCT/JP2012/070313 patent/WO2013031511A1/ja active Application Filing
- 2012-08-09 KR KR1020137030253A patent/KR101884252B1/ko active IP Right Grant
- 2012-08-30 TW TW101131456A patent/TWI565579B/zh active
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TWI632053B (zh) * | 2013-06-28 | 2018-08-11 | 東麗股份有限公司 | Biaxially oriented polyester film |
JP2015096928A (ja) * | 2013-11-16 | 2015-05-21 | 三菱樹脂株式会社 | 偏光板保護用ポリエステルフィルム |
JP2018162435A (ja) * | 2016-09-30 | 2018-10-18 | 東レ株式会社 | 二軸配向ポリエステルフィルムおよびその製造方法 |
JP7172025B2 (ja) | 2016-09-30 | 2022-11-16 | 東レ株式会社 | 二軸配向ポリエステルフィルムおよびその製造方法 |
JP2019211601A (ja) * | 2018-06-04 | 2019-12-12 | 三菱ケミカル株式会社 | 偏光子保護フィルム |
JP7259216B2 (ja) | 2018-06-04 | 2023-04-18 | 三菱ケミカル株式会社 | 偏光子保護フィルム |
JP2022517201A (ja) * | 2019-01-07 | 2022-03-07 | 東レ先端素材株式会社 | 偏光子保護用ポリエステルフィルムとその製造方法及びこれを備える偏光板 |
JP2020125405A (ja) * | 2019-02-05 | 2020-08-20 | 東レ株式会社 | 偏光板離型用ポリエステルフィルム |
JP7225863B2 (ja) | 2019-02-05 | 2023-02-21 | 東レ株式会社 | 偏光板離型用ポリエステルフィルム |
Also Published As
Publication number | Publication date |
---|---|
CN103649182B (zh) | 2016-11-02 |
KR20140053000A (ko) | 2014-05-07 |
CN103649182A (zh) | 2014-03-19 |
TWI565579B (zh) | 2017-01-11 |
JPWO2013031511A1 (ja) | 2015-03-23 |
TW201318821A (zh) | 2013-05-16 |
JP6007792B2 (ja) | 2016-10-12 |
KR101884252B1 (ko) | 2018-08-01 |
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