WO2019003503A1 - 位相差フィルム、円偏光板、および位相差フィルムの製造方法 - Google Patents

位相差フィルム、円偏光板、および位相差フィルムの製造方法 Download PDF

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Publication number
WO2019003503A1
WO2019003503A1 PCT/JP2018/009158 JP2018009158W WO2019003503A1 WO 2019003503 A1 WO2019003503 A1 WO 2019003503A1 JP 2018009158 W JP2018009158 W JP 2018009158W WO 2019003503 A1 WO2019003503 A1 WO 2019003503A1
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Prior art keywords
retardation
film
heating
stretched film
polarizing plate
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PCT/JP2018/009158
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English (en)
French (fr)
Japanese (ja)
Inventor
暢 鈴木
浩 角村
秀行 高松
清水　享
寛教 柳沼
寛 友久
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日東電工株式会社
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Application filed by 日東電工株式会社 filed Critical 日東電工株式会社
Priority to KR1020197038058A priority Critical patent/KR102518911B1/ko
Priority to CN201880043387.5A priority patent/CN110799869B/zh
Publication of WO2019003503A1 publication Critical patent/WO2019003503A1/ja

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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
    • 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
    • B29C55/04—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets uniaxial, e.g. oblique
    • B29C55/06—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets uniaxial, e.g. oblique parallel with the direction of feed
    • 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
    • B29C55/04—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets uniaxial, e.g. oblique
    • B29C55/08—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets uniaxial, e.g. oblique transverse to the direction of feed
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/30—Polarising elements
    • 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

Definitions

  • the present invention relates to a retardation film, a circularly polarizing plate, and a method for producing a retardation film.
  • the organic EL panel has a highly reflective metal layer, and easily causes problems such as reflection of external light and reflection of a background. Therefore, it is known to prevent these problems by providing a circularly polarizing plate having a ⁇ / 4 plate on the viewing side.
  • the retardation film used for the said circularly-polarizing plate usually differs in retardation value with wavelengths, and a sufficient antireflection effect is not obtained with a wavelength, but color loss becomes a problem. Therefore, a so-called reverse dispersion retardation film has been proposed, in which the retardation value increases as the wavelength increases (for example, Patent Document 1).
  • the above-mentioned conventional reverse dispersive retardation film may change in retardation value when used in a high temperature environment and / or a high humidity environment, resulting in retardation unevenness. There is a case.
  • the present invention has been made to solve the above-mentioned conventional problems, and the main object thereof is a retardation film in which a change in retardation value in a high temperature and high humidity environment is suppressed, such a retardation film It is providing a circularly-polarizing plate which it has, and the manufacturing method of such retardation film.
  • the method for producing a retardation film of the present invention is a method for producing a retardation film in which the in-plane retardation satisfies the relationship Re (450) ⁇ Re (550), and the temperature is raised from 30 ° C. to Tg-25 ° C.
  • the shrinkage in the slow axis direction is 0.4% or less in the heating TMA test repeating 3 cycles of cooling again to 30 ° C., or 25 ° C./25% RH, 85 ° C./2% RH,
  • the above includes the heat treatment step of heating.
  • the heating temperature in the heat treatment step is T 1 (° C.), and the heating time in the heat treatment step is t 1 (minutes), and the above-mentioned stretched film before the heat treatment step is Assuming that the contraction rate in the heating TMA test is A 1 , 10 ⁇ t 1 / ⁇ (Tg ⁇ T 1 ) 2 ⁇ A 1 2 ⁇ > 2 is satisfied.
  • the heating temperature in the heat treatment step is T 1 (° C.), and the heating time in the heat treatment step is t 1 (minutes), and the above-mentioned stretched film before the heat treatment step is Assuming that the contraction rate in the humidified TMA test is A 2 , 10 ⁇ t 1 / ⁇ (Tg ⁇ T 1 ) 2 ⁇ A 2 2 ⁇ > 0.9 is satisfied.
  • the method for producing a retardation film of the present invention is a method for producing a retardation film in which the in-plane retardation satisfies the relationship of Re (450) ⁇ Re (550), wherein 25 ° C./25% RH, 85 ° C.
  • a stretched film having a shrinkage in the slow axis direction of 0.7% or less It includes a warm water treatment step of immersing in warm water for 3 minutes or more.
  • the immersion time in the hot water treatment step t 2 and (minutes), when the shrinkage ratio in the humidifying TMA test the hot water treatment step prior to the stretched film was A 3, t 2 / A 3 2 > 20 is satisfied.
  • a retardation film is provided.
  • This retardation film satisfies the relationship of in-plane retardation Re (450) ⁇ Re (550), and is heated up from 30 ° C to Tg-25 ° C and cooled again to 30 ° C.
  • the shrinkage ratio in the slow axis direction is 0.1% or less, and the environment is in the order of 25 ° C / 25% RH, 85 ° C / 2% RH, 85 ° C / 85% RH, 85 ° C / 2% RH.
  • the shrinkage factor in the slow axis direction is 0.2% or less in the humidified TMA test in which In one embodiment, the retardation film is formed of a resin selected from a polycarbonate resin and a polyester carbonate resin.
  • the retardation film has a Re (450) / Re (550) of 0.8 to 0.9. In one embodiment, the retardation film has a photoelastic coefficient of 1 ⁇ 10 ⁇ 12 (m 2 / N) to 40 ⁇ 10 ⁇ 12 (m 2 / N).
  • a circularly polarizing plate is provided. This circularly polarizing plate has a retardation layer composed of the above retardation film and a polarizer, and the angle between the slow axis of the retardation layer and the absorption axis of the polarizer is 35 ° to 55 °.
  • the circularly polarizing plate is sheet-like, and the in-plane retardation value of the central portion of the retardation layer is R A0, and the in-plane retardation value of the apex portion is R B0. after holding by bonding glass 240 hours at 85 ° C., the in-plane retardation value of the center portion of the retardation layer as R A1, an in-plane retardation value of the apex portion and R B1, glass on both sides And the in-plane retardation value of the central portion of the retardation layer as R A2 and the in-plane retardation value of the apex portion as R B2 after bonding them together and holding them at 65 ° C./90% RH for 240 hours.
  • the shrinkage rate in the slow axis direction is 0.4% or less in the heating TMA test, or the shrinkage rate in the slow phase direction is 0.7% or less in the humidified TMA test
  • a heat treatment step of heating a certain stretched film at a temperature of 105 ° C. or more for 2 minutes or more a retardation film in which a change in retardation value in a high temperature and high humidity environment is suppressed may be obtained.
  • Refractive index (nx, ny, nz) “Nx” is the refractive index in the direction in which the in-plane refractive index is maximum (ie, the slow axis direction), and “ny” is the direction orthogonal to the slow axis in the plane (ie, the fast axis direction) And “nz” is the refractive index in the thickness direction.
  • Refractive index (nx, ny, nz) “Nx” is the refractive index in the direction in which the in-plane refractive index is maximum (ie, the slow axis direction), and “ny” is the direction orthogonal to the slow axis in the plane (ie, the fast axis direction) And “nz” is the refractive index in the thickness direction.
  • In-plane retardation (Re) “Re ( ⁇ )” is an in-plane retardation measured at 23 ° C. with light of wavelength ⁇ nm.
  • Re (550) is an in-plane retardation measured with light of wavelength 550 nm at 23 ° C.
  • Retardation in the thickness direction (Rth) is a retardation in the thickness direction measured with light of wavelength ⁇ nm at 23 ° C.
  • the production method of the present invention is a production used for production of a retardation film showing so-called reverse dispersion wavelength dependency in which in-plane retardation satisfies the relationship of Re (450) ⁇ Re (550). It is a method.
  • the method for producing a retardation film according to one embodiment of the present invention includes a heat treatment step of heating the stretched film at a temperature of 105 ° C. or more for 2 minutes or more.
  • the stretched film has a shrinkage in the slow axis direction of 0.4% or less in a heated TMA test which repeats heating and cooling from 30 ° C. to Tg-25 ° C.
  • the shrinkage in the slow axis direction is 0.7% It is below.
  • the heating temperature in the heat treatment step is T 1 (° C.)
  • the heating time in the heat treatment step is t 1 (minutes)
  • the contraction rate in the heating TMA test of the stretched film before the heat treatment step is A 1
  • 10 ⁇ t 1 / ⁇ (Tg ⁇ T 1 ) 2 ⁇ A 1 2 ⁇ > 2 is satisfied.
  • the shrinkage ratio in humidified TMA test of the stretched film before the heat treatment step was set to A 2, preferably, meet the 10 ⁇ t 1 / ⁇ (Tg -T 1) 2 ⁇ A 2 2 ⁇ > 0.9.
  • the method for producing a retardation film according to another embodiment of the present invention includes a warm water treatment step of immersing the stretched film in warm water of 60 ° C. or more for 3 minutes or more.
  • the stretched film has a shrinkage rate in the slow axis direction in a humidified TMA test in which the environment is changed in the order of 25 ° C./25% RH, 85 ° C./2% RH, 85 ° C./85% RH, 85 ° C./2% RH It is 0.7% or less.
  • the immersion time in the warm water treatment process is t 2 (minutes)
  • the contraction ratio in the moistened TMA test of the drawn film before the warm water treatment process is A 3 , preferably t 2 / A 3 2 > 20 is satisfied.
  • the shrinkage ratio in the slow axis direction is 0.4% or less in the heated TMA test which repeats the cycle of raising the temperature from 30 ° C to Tg-25 ° C and cooling again to 30 ° C as described above.
  • a stretched film is typically produced by stretching a resin film in at least one direction.
  • the resin film is formed of any appropriate resin as long as a stretched film (retardation film) exhibiting so-called reverse dispersion wavelength dependency can be obtained by subjecting the resin film to a stretching treatment.
  • resin which forms a resin film polycarbonate resin, polyvinyl acetal resin, cellulose ester-type resin, polyester-type resin, polyester carbonate-type resin is mentioned, for example. These resins may be used alone or in combination depending on the desired properties.
  • any appropriate polycarbonate resin may be used as the polycarbonate resin.
  • a polycarbonate resin containing a structural unit derived from a dihydroxy compound is preferable.
  • the dihydroxy compound 9,9-bis (4-hydroxyphenyl) fluorene, 9,9-bis (4-hydroxy-3-methylphenyl) fluorene, 9,9-bis (4-hydroxy-3-3) Ethylphenyl) fluorene, 9,9-bis (4-hydroxy-3-n-propylphenyl) fluorene, 9,9-bis (4-hydroxy-3-isopropylphenyl) fluorene, 9,9-bis (4-hydroxy) -3-n-butylphenyl) fluorene, 9,9-bis (4-hydroxy-3-sec-butylphenyl) fluorene, 9,9-bis (4-hydroxy-3-tert-butylphenyl) fluorene, 9, 9-Bis (4-hydroxy-3-cyclohexylphenyl) fluorene, 9,9-Bis
  • the polycarbonate resin contains a structural unit derived from a dihydroxy compound such as isosorbide, isomannide, isoidet, spiro glycol, dioxane glycol, diethylene glycol, triethylene glycol, polyethylene glycol, and bisphenols in addition to the structural unit derived from the dihydroxy compound. It may be.
  • a dihydroxy compound such as isosorbide, isomannide, isoidet, spiro glycol, dioxane glycol, diethylene glycol, triethylene glycol, polyethylene glycol, and bisphenols in addition to the structural unit derived from the dihydroxy compound. It may be.
  • the glass transition temperature (Tg) of the polycarbonate resin is preferably 110 ° C. or more and 250 ° C. or less, more preferably 120 ° C. or more and 230 ° C. or less. If the glass transition temperature is excessively low, the heat resistance tends to deteriorate, and dimensional change may occur after film formation. When the glass transition temperature is excessively high, the molding stability at the time of film molding may be deteriorated, and the transparency of the film may be impaired.
  • the glass transition temperature is determined in accordance with JIS K 7121 (1987).
  • melt extrusion for example, T-die molding
  • cast coating for example, casting
  • calendar molding heat pressing
  • coextrusion co-melting
  • multilayer extrusion inflation molding
  • T-die molding casting and inflation molding are used.
  • the thickness of the thickness (unstretched film) of the resin film may be set to any appropriate value depending on the desired optical properties, the stretching conditions described later, and the like.
  • the thickness is preferably 50 to 300 ⁇ m, and more preferably 80 to 250 ⁇ m.
  • any appropriate stretching direction and stretching conditions eg, stretching temperature, stretching ratio, stretching direction
  • various stretching methods such as free end stretching, fixed end stretching / free end shrinkage, fixed end shrinkage can be used alone or simultaneously or sequentially.
  • the stretching direction can also be performed in various directions and dimensions, such as the horizontal direction, the vertical direction, the thickness direction, and the diagonal direction.
  • the stretching temperature is preferably in the range of the glass transition temperature (Tg) of the resin film ⁇ 20 ° C.
  • a stretched film is produced by uniaxially stretching or uniaxially stretching a resin film.
  • uniaxial stretching there is a method of stretching in the longitudinal direction (longitudinal direction) while traveling the resin film in the longitudinal direction.
  • the stretch ratio is preferably 10% to 500%.
  • a stretched film is produced by continuously stretching a long resin film obliquely in the direction of the angle ⁇ with respect to the long direction.
  • a long stretched film having an orientation angle of angle ⁇ with respect to the longitudinal direction of the film can be obtained, and, for example, roll-to-roll becomes possible upon lamination with a polarizer, and the manufacturing process Can be simplified.
  • a tenter type drawing machine capable of applying a feed force or a drawing force or a take-up force at different speeds in the lateral and / or longitudinal directions
  • a tenter type stretching machine includes a transverse uniaxial stretching machine, a simultaneous biaxial stretching machine, etc., any appropriate stretching machine may be used as long as it can continuously stretch a long resin film obliquely.
  • the thickness of the stretched film is preferably 20 ⁇ m to 100 ⁇ m, more preferably 30 ⁇ m to 80 ⁇ m.
  • a commercially available film may be used as it is, or the commercially available film may be subjected to secondary processing (for example, stretching treatment, surface treatment) according to the purpose.
  • secondary processing for example, stretching treatment, surface treatment
  • a trade name "Pure Ace RM” manufactured by Teijin Limited can be mentioned.
  • the stretched film is subjected to a relaxation treatment.
  • a relaxation treatment Thereby, the stress generated by stretching can be relaxed, and the contraction rate in the slow axis direction in the heating TMA test is 0.4% or less, or the contraction rate in the slow axis direction in the humidification TMA test is 0. It may be 7% or less.
  • Any appropriate condition may be adopted as the relaxation treatment condition.
  • the stretched film is shrunk along the stretching direction at a predetermined relaxation temperature and a predetermined relaxation rate (shrinkage ratio).
  • the relaxation temperature is preferably 60.degree. C. to 150.degree.
  • the relaxation rate is preferably 3% to 6%.
  • the stretched film is heated at a temperature of 105 ° C. or more for 2 minutes or more.
  • the heating temperature in the heat treatment step is T 1 (° C.), and the heating time in the heat treatment step is t 1 (minutes), and the shrinkage in the heated TMA test of the stretched film before the heat treatment step
  • the ratio is A 1 , preferably, the value represented by 10 ⁇ t 1 / ⁇ (Tg ⁇ T 1 ) 2 ⁇ A 1 2 ⁇ is larger than 2.
  • the above value is preferably more than 2 and less than 150, more preferably 3 to 50, and particularly preferably 3 to 10.
  • (Tg ⁇ T 1 ) is preferably 5 or more.
  • the shrinkage ratio in humidified TMA test of the stretched film before the heat treatment step when the A 2 preferably, 10 ⁇ t 1 / ⁇ ( Tg-T 1) 2 ⁇ A 2 2 ⁇
  • the represented value is greater than 0.9.
  • the above value is preferably 1 to 60, more preferably 1 to 20, and particularly preferably 1 to 10.
  • the heating temperature is preferably 105 ° C. to 140 ° C., more preferably 110 ° C. to 130 ° C., particularly preferably 115 ° C. to 125 ° C.
  • the heating time is preferably 2 minutes to 150 minutes, more preferably 3 minutes to 120 minutes, and particularly preferably 5 minutes to 60 minutes.
  • any appropriate heating means can be used as long as the stretched film can be heated under the above heating conditions.
  • the heating means is typically an oven.
  • a stretched film is obtained by stretching a long resin film while traveling in the long direction, the obtained stretched film may be subjected to heat treatment while traveling as it is.
  • Hot Water Treatment Step In the warm water treatment step, as described above, the stretched film is immersed in warm water of 60 ° C. or more for 3 minutes or more.
  • the above value is preferably more than 20 and 1,000 or less, more preferably 25 to 500, and particularly preferably 30 to 150.
  • the temperature of the hot water is preferably 60 ° C. to 90 ° C., more preferably 65 ° C. to 85 ° C., particularly preferably 68 ° C. to 82 ° C.
  • the immersion time is preferably 3 minutes to 60 minutes, more preferably 3 minutes to 30 minutes, and particularly preferably 5 minutes to 20 minutes.
  • any suitable warm water treatment means can be used as long as the stretched film can be heated under the above heating conditions.
  • the hot water treatment means is typically a hot water bath adjusted to an appropriate temperature.
  • the hot water treatment may be performed while running the obtained stretched film as it is.
  • the retardation film of the present invention is a retardation film exhibiting in-plane retardation satisfying the relationship of Re (450) ⁇ Re (550), that is, a retardation film showing so-called reverse dispersion wavelength dependency.
  • the retardation film has a shrinkage ratio in the slow axis direction of 0.1% or less in a heated TMA test which repeats heating and cooling from 30 ° C. to Tg-25 ° C. three cycles again.
  • the shrinkage in the slow axis direction is 0.2% It is below.
  • the shrinkage factor in the slow axis direction in the above-mentioned heated TMA test is preferably 0% to 0.08%, and more preferably 0% to 0.05%.
  • the shrinkage factor in the slow axis direction in the humidified TMA test is preferably 0% to 0.15%, and more preferably 0% to 0.10%.
  • the retardation film as described above can suppress the change in retardation value in a high temperature and high humidity environment.
  • the value of Re (450) / Re (550) of the retardation film is preferably 0.8 to 0.9, and more preferably 0.83 to 0.87.
  • the in-plane retardation Re (550) of the retardation film is preferably 100 nm to 180 nm, more preferably 135 nm to 155 nm.
  • the photoelastic coefficient of the retardation film is preferably 1 ⁇ 10 ⁇ 12 (m 2 / N) to 40 ⁇ 10 ⁇ 12 (m 2 / N), more preferably 1 ⁇ 10 ⁇ 12 (m 2 / N) And 30 ⁇ 10 ⁇ 12 (m 2 / N), particularly preferably 1 ⁇ 10 ⁇ 12 (m 2 / N) to 20 ⁇ 10 ⁇ 12 (m 2 / N).
  • the retardation film as described above can be obtained, for example, by the manufacturing method described in Section A.
  • the retardation film may be used for a circularly polarizing plate.
  • the circularly polarizing plate of the present invention has a retardation layer composed of the above retardation film, and a polarizer.
  • the angle between the slow axis of the retardation layer and the absorption axis of the polarizer is 35 ° to 55 °, preferably 40 ° to 50 °, particularly preferably 43 to 47 °, and most preferably It is about 45 °.
  • FIG. 1 is a schematic cross-sectional view of a circularly polarizing plate according to one embodiment of the present invention.
  • the circularly polarizing plate 100 is sheet-like.
  • the retardation unevenness (heating retardation unevenness) of the retardation layer 30 when the circularly polarizing plate 100 is heated is 3 nm or less.
  • the retardation unevenness (humidified retardation unevenness) of the retardation layer 30 when the circularly polarizing plate 100 is humidified is 3 nm or less.
  • the heating retardation unevenness and the humidification retardation unevenness are preferably 0 nm to 2 nm, more preferably 0 nm to 1 nm.
  • the heating phase difference unevenness can be determined, for example, as an absolute value of a value calculated from the following equation when glass is attached to both sides of the circularly polarizing plate 100 and heated (held at 85 ° C. for 240 hours) .
  • R A1 -R B1 is the in-plane retardation value of the central portion of the retardation layer 30
  • R B0 is the in-plane retardation value of the top portion of the retardation layer 30
  • R A1 is the retardation after the heating.
  • the in-plane retardation value of the central portion of the layer 30, R.sub.B1 is the in-plane retardation value of the peak portion after the heating.
  • the above-mentioned humidification phase difference unevenness is, for example, as an absolute value of a value calculated from the following equation when glass is attached to both sides of the circularly polarizing plate 100 and humidified (holding for 240 hours at 65 ° C./90% RH) It can be determined.
  • R A2 -R B2 is an in-plane retardation value of the central portion of the retardation layer 30 after the humidification
  • R B2 is an in-plane retardation value of the apex portion after the humidification.
  • the retardation layer is composed of the retardation film
  • the change of the in-plane retardation at the end of the retardation layer can be suppressed, and the retardation unevenness is Can be suppressed.
  • the resin film forming the polarizer may be a single layer resin film, or may be a laminate of two or more layers.
  • the polarizer composed of a single-layer resin film include hydrophilic polymer films such as polyvinyl alcohol (PVA) -based films, partially formalized PVA-based films, ethylene / vinyl acetate copolymer-based partially saponified films, etc.
  • PVA polyvinyl alcohol
  • those which have been subjected to a dyeing process and a drawing process with a dichroic substance such as iodine and a dichroic dye and a polyene-based oriented film such as a dewatered product of PVA or a dehydrochlorinated product of polyvinyl chloride.
  • a polarizer obtained by dyeing a PVA-based film with iodine and uniaxially stretching it is used because of excellent optical properties.
  • the staining with iodine is performed, for example, by immersing a PVA-based film in an aqueous iodine solution.
  • the stretching ratio of the uniaxial stretching is preferably 3 to 7 times. Stretching may be carried out after the dyeing process or may be carried out while dyeing. Moreover, it may be dyed after being drawn.
  • the PVA-based film is subjected to swelling treatment, crosslinking treatment, washing treatment, drying treatment, and the like. For example, by immersing and washing the PVA-based film in water prior to dyeing, it is possible not only to wash the stains and anti-blocking agent on the surface of the PVA-based film, but also to swell the PVA-based film to make uneven dyeing It can be prevented.
  • the polarizer obtained by using a laminate a laminate of a resin substrate and a PVA-based resin layer (PVA-based resin film) laminated on the resin substrate, or a resin substrate and the resin
  • coated-formed to the base material is mentioned.
  • coated and formed by the said resin base material applies a PVA-type resin solution to a resin base material, for example, it is made to dry, and a resin base material Forming a PVA-based resin layer thereon to obtain a laminate of the resin base and the PVA-based resin layer; stretching and dyeing the laminate to make the PVA-based resin layer as a polarizer; obtain.
  • stretching typically includes dipping the laminate in a boric acid aqueous solution and stretching.
  • stretching may optionally further comprise air-stretching the laminate at a high temperature (eg, 95 ° C. or higher) prior to stretching in an aqueous boric acid solution.
  • the resulting laminate of resin substrate / polarizer may be used as it is (that is, the resin substrate may be used as a protective layer of polarizer), and the resin substrate is peeled off from the laminate of resin substrate / polarizer.
  • any appropriate protective layer depending on the purpose may be laminated on the peeled surface.
  • the details of the method for producing such a polarizer are described, for example, in JP-A-2012-73580. The publication is incorporated herein by reference in its entirety.
  • the thickness of the polarizer is, for example, 1 ⁇ m to 80 ⁇ m. In one embodiment, the thickness of the polarizer is preferably 1 ⁇ m to 15 ⁇ m, more preferably 3 ⁇ m to 10 ⁇ m, and particularly preferably 3 ⁇ m to 8 ⁇ m. If the thickness of the polarizer is in such a range, curling at the time of heating can be favorably suppressed, and good appearance durability at the time of heating can be obtained.
  • the circularly polarizing plate having such a second retardation layer can suppress changes in reflectance and reflection hue when used in an organic EL panel.
  • the thickness direction retardation Rth (550) of the second retardation layer is preferably -50 nm to -300 nm, more preferably -70 nm to -250 nm, still more preferably -90 nm to -200 nm, particularly preferably -100 nm to -180 nm.
  • the second retardation layer may preferably include a liquid crystal material fixed in homeotropic alignment.
  • the liquid crystal material (liquid crystal compound) which can be homeotropically aligned may be a liquid crystal monomer or a liquid crystal polymer.
  • Specific examples of the method of forming the liquid crystal compound and the second retardation layer include the method of forming a liquid crystal compound and a retardation film described in [0020] to [0028] of JP-A-2002-333642.
  • the thickness of the second retardation layer is preferably 0.5 ⁇ m to 10 ⁇ m, more preferably 0.5 ⁇ m to 8 ⁇ m, and still more preferably 0.5 ⁇ m to 5 ⁇ m.
  • the second retardation layer may be formed of a retardation film formed of fumaric acid diester resin described in JP-A-2012-32784.
  • the thickness is preferably 5 ⁇ m to 80 ⁇ m, more preferably 10 ⁇ m to 50 ⁇ m.
  • the protective layer is formed of any suitable protective film that can be used as a film to protect a polarizer.
  • suitable protective film include cellulose-based resins such as triacetyl cellulose (TAC), polyester-based, polyvinyl alcohol-based, polycarbonate-based, polyamide-based, polyimide-based, polyether sulfone-based, and polysulfone.
  • transparent resins such as polystyrene, polynorbornene, polyolefin, (meth) acrylic and acetate.
  • thermosetting resins such as (meth) acrylic resins, urethane resins, (meth) acrylic urethane resins, epoxy resins, and silicone resins, ultraviolet curable resins, and the like can also be mentioned.
  • glassy polymers such as siloxane polymers can also be mentioned.
  • a polymer film described in JP-A-2001-343529 (WO 01/37007) can also be used.
  • a resin composition containing a thermoplastic resin having a substituted or unsubstituted imide group in a side chain, and a thermoplastic resin having a substituted or unsubstituted phenyl group and a nitrile group in a side chain for example, a resin composition having an alternating copolymer of isobutene and N-methyl maleimide and an acrylonitrile / styrene copolymer can be mentioned.
  • the polymer film may be, for example, an extrusion of the resin composition.
  • the thickness of the protective film is preferably 10 ⁇ m to 100 ⁇ m.
  • the protective film may be laminated to the polarizer through an adhesive layer (specifically, an adhesive layer, an adhesive layer), or may be laminated to the polarizer in close contact (without the adhesive layer). Good.
  • the adhesive layer is formed of any suitable adhesive.
  • the water-soluble adhesive which has polyvinyl alcohol-type resin as a main component is mentioned, for example.
  • the water-soluble adhesive containing a polyvinyl alcohol-based resin as a main component can preferably further contain a metal compound colloid.
  • the metal compound colloid may be one in which metal compound fine particles are dispersed in a dispersion medium, may be electrostatically stabilized due to mutual repulsion of the same kind of charge of the fine particles, and may be permanently stable. .
  • the average particle size of the fine particles forming the metal compound colloid may be any appropriate value as long as the optical properties such as polarization properties are not adversely affected.
  • the thickness is preferably 1 nm to 100 nm, more preferably 1 nm to 50 nm. This is because fine particles can be uniformly dispersed in the adhesive layer, adhesion can be secured, and knicks can be suppressed. In addition, a "knick" means the thing of the local uneven defect which arises at the interface of a polarizer and a protective film.
  • the pressure-sensitive adhesive layer is composed of any suitable pressure-sensitive adhesive.
  • the surface of the protective film opposite to the polarizer may be subjected to surface treatment such as hard coating treatment, anti-reflection treatment, anti-sticking treatment, anti-glare treatment, etc., as necessary.
  • the thickness of the protective film is typically 5 mm or less, preferably 1 mm or less, more preferably 1 ⁇ m to 500 ⁇ m, and still more preferably 5 ⁇ m to 150 ⁇ m.
  • thermomechanical analyzer (Hitachi High-Tech Science Co., Ltd., model number “TMA7100”), increase the temperature of the measurement sample from 30 ° C. to Tg-25 ° C. and cool it again to 30 ° C. for three cycles and measure The dimensional change rate (shrinkage rate) in the longitudinal direction (late axis direction) of the sample was measured. The temperature rising rate was 5 ° C./min, and the holding time at each temperature was 10 minutes.
  • (4) Dimensional change due to humidification Huidified TMA test
  • the stretched film or retardation film obtained in Examples and Comparative Examples was cut into a size of 20 mm (in slow axis direction) ⁇ 5 mm (in fast axis direction) to obtain a measurement sample.
  • the length direction of the measurement sample was measured.
  • the holding time at 25 ° C./25% RH was 60 minutes
  • the holding time at 85 ° C./2% RH was 60 minutes
  • the holding time at 85 ° C./85% RH was 300 minutes.
  • phase difference value RB11 and the in-plane phase difference value RB12 of the peak portion located in the fast axis direction from the center portion were measured.
  • the larger one of the absolute values of the values A and B obtained from the following equation was regarded as heating phase difference unevenness.
  • A (R A1 -R B11 )-(R A0 -R B01 )
  • B (R A1- R B12 )-(R A0- R B02 ) (6)
  • Humidification phase difference unevenness A measurement sample of a circularly polarizing plate is produced in the same manner as in (5) above, and the in-plane retardation value R A0 of the central portion and the apex portion located in the slow axis direction from the central portion the in-plane retardation value R B01, an in-plane retardation value R B02 vertex portion positioned from the center to the fast axis was measured.
  • the measurement sample is humidified in an oven at 65 ° C./90% for 240 hours, and the in-plane retardation value R A2 of the central portion and the apex portion located in the slow axis direction from the central portion
  • the in-plane retardation value RB21 and the in-plane retardation value RB22 of the vertex located in the fast axis direction from the central portion were measured.
  • the larger one of the absolute values of the values C and D obtained from the following equation was taken as the humidification phase difference unevenness.
  • C (R A2- R B21 )-(R A0- R B01 )
  • D (R A2- R B22 )-(R A0- R B02 )
  • Example 1 Preparation of retardation film (polycarbonate resin) The polymerization was carried out using a batch polymerization apparatus consisting of two vertical reactors equipped with stirring blades and a reflux condenser controlled at 100 ° C. 29.60 parts by mass (0.046 mol) of bis [9- (2-phenoxycarbonylethyl) fluoren-9-yl] methane, 29.21 parts by mass (0.200 mol) of ISB, 42.28 parts by mass of SPG (0. 139 mol), 63.77 parts by mass (0.298 mol) of DPC and 1.19 ⁇ 10 -2 parts by mass (6.78 ⁇ 10 -5 mol) of calcium acetate monohydrate were loaded as a catalyst.
  • a batch polymerization apparatus consisting of two vertical reactors equipped with stirring blades and a reflux condenser controlled at 100 ° C. 29.60 parts by mass (0.046 mol) of bis [9- (2-phenoxycarbonylethyl) fluoren-9-yl]
  • a resin film having a thickness of 135 ⁇ m was produced using a film production apparatus equipped with a set temperature of 120 to 130 ° C. and a winder.
  • a stretched film is obtained by stretching the obtained long resin film in the width direction at a stretching temperature of 134 ° C. and a stretching ratio of 2.8 times and subsequently subjecting the stretched film in the width direction to a relaxation treatment.
  • the relaxation treatment conditions were a relaxation temperature of 130 ° C. and a relaxation rate of 4.5%.
  • the stretched film was subjected to the humidified TMA test of (4) above, and the dimensional change was 0.30%. Moreover, when this stretched film was subjected to the heating TMA test of the above (3), the dimensional change was 0.05%. Next, the stretched film was heated (heat treatment) at 125 ° C. for 2 minutes to obtain a retardation film with a thickness of 48 ⁇ m.
  • a long amorphous polyethylene terephthalate (A-PET) film (Mitsubishi Resins Co., Ltd., trade name "Novaclear", thickness: 100 ⁇ m) is prepared as a substrate, and polyvinyl alcohol (PVA) resin is formed on one side of the substrate.
  • PVA polyvinyl alcohol
  • An aqueous solution of (Gosenol (registered trademark) NH-26, trade name, manufactured by Japan Synthetic Chemical Industry Co., Ltd.) was applied and dried at 60 ° C. to form a 7 ⁇ m-thick PVA-based resin layer.
  • the laminate thus obtained was immersed in an insolubilization bath at a liquid temperature of 30 ° C.
  • a side chain type liquid crystal polymer represented by the following chemical formula (I)
  • 80 parts by weight of a polymerizable liquid crystal manufactured by BASF: trade name Paliocolor LC 242
  • a photopolymerization initiator manufactured by BASF: trade name Irgacure 907
  • 5 parts by weight was dissolved in 400 parts by weight of cyclopentanone to prepare a liquid crystal coating liquid.
  • the coating solution is applied to a base film (a norbornene resin film: manufactured by Nippon Zeon Co., Ltd., trade name "Zeonor") by a bar coater, and then the liquid crystal is dried by heating and drying at 70 ° C for 4 minutes. It was oriented.
  • the liquid crystal layer was irradiated with ultraviolet light to cure the liquid crystal layer, whereby a liquid crystal solidified layer (thickness: 1 ⁇ m) to be a retardation film was formed on the substrate.
  • the Re (550) of this layer was 0 nm, and the Rth (550) was -71 nm (nx: 1.5326, ny: 1.5326, nz: 1.6550).
  • the retardation film was bonded to the polarizer side of the polarizing plate via an adhesive such that the angle between the absorption axis of the polarizer and the slow axis of the retardation film was 45 °. Subsequently, the said liquid-crystal solidified layer is transcribe
  • the circularly-polarizing plate which has the structure of a protective layer / polarizer / retardation layer / 2nd retardation layer Made.
  • Example 2 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 1 except that the stretched film was heated at 125 ° C. for 10 minutes.
  • Example 3 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 1 except that the stretched film was heated at 125 ° C. for 30 minutes.
  • Example 4 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 1 except that the stretched film was heated at 125 ° C. for 60 minutes.
  • Example 5 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 1 except that the stretched film was heated at 125 ° C. for 120 minutes.
  • Example 6 A stretched film was produced in the same manner as in Example 1 except that the relaxation temperature was 110 ° C. The stretched film was subjected to the humidified TMA test in (4) above, and the dimensional change was 0.50%. Moreover, when this stretched film was subjected to the heating TMA test of the above (3), the dimensional change was 0.08%. A retardation film and a circularly polarizing plate were produced in the same manner as in Example 2 except that the above-mentioned stretched film was used.
  • Example 7 A stretched film was produced in the same manner as in Example 1 except that the relaxation temperature was 80 ° C. The stretched film was subjected to the humidified TMA test in (4) above, and the dimensional change was 0.70%. Moreover, when this stretched film was subjected to the heating TMA test of the above (3), the dimensional change was 0.13%. A retardation film and a circularly polarizing plate were produced in the same manner as in Example 2 except that the above-mentioned stretched film was used.
  • Example 8 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 1 except that the stretched film was heated at 105 ° C. for 10 minutes.
  • Example 9 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 1 except that the stretched film was heated at 110 ° C. for 10 minutes.
  • Example 10 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 1 except that the stretched film was heated at 115 ° C. for 10 minutes.
  • Example 11 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 1 except that the stretched film was heated at 120 ° C. for 10 minutes.
  • Example 12 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 1 except that the stretched film was heated at 130 ° C. for 10 minutes.
  • Example 13 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 1 except that the stretched film was immersed in warm water at 60 ° C. for 3 minutes (warm water treatment) instead of the above heat treatment.
  • Example 14 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 1 except that the stretched film was immersed in warm water at 60 ° C. for 10 minutes instead of the above heat treatment.
  • Example 15 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 1 except that the stretched film was immersed in warm water at 60 ° C. for 30 minutes instead of the above heat treatment.
  • Example 16 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 1 except that the stretched film was immersed in warm water at 60 ° C. for 60 minutes instead of the above heat treatment.
  • Example 17 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 6 except that the stretched film was immersed in warm water at 60 ° C. for 10 minutes instead of the above heat treatment.
  • Example 18 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 7 except that the stretched film was immersed in warm water at 60 ° C. for 10 minutes instead of the above heat treatment.
  • Example 19 A commercially available polycarbonate resin film (manufactured by Teijin Limited, product name “Pure Ace RM”, thickness 50 ⁇ m) was used as a stretched film.
  • the stretched film was subjected to the heating TMA test in (3) above, and the dimensional change was 0.22%. Moreover, when this stretched film was subjected to the humidified TMA test of (4) above, the dimensional change was 0.10%.
  • the retardation film was obtained by heating (heating process) the said stretched film for 2 minutes at 125 degreeC. Furthermore, a circularly polarizing plate was produced in the same manner as in Example 1 except that the above retardation film was used.
  • Example 20 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 19 except that the stretched film was heated at 125 ° C. for 10 minutes.
  • Example 21 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 19 except that the stretched film was heated at 125 ° C. for 30 minutes.
  • Example 22 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 19 except that the stretched film was heated at 125 ° C. for 60 minutes.
  • Example 23 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 19 except that the stretched film was heated at 125 ° C. for 120 minutes.
  • Example 24 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 19 except that the stretched film was heated at 105 ° C. for 10 minutes.
  • Example 25 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 19 except that the stretched film was heated at 110 ° C. for 10 minutes.
  • Example 26 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 19 except that the stretched film was heated at 115 ° C. for 10 minutes.
  • Example 27 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 19 except that the stretched film was heated at 120 ° C. for 10 minutes.
  • Comparative Example 1 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 1 except that the stretched film was heated at 125 ° C. for 1 minute.
  • Comparative Example 2 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 1 except that the stretched film was heated at 100 ° C. for 10 minutes.
  • Comparative Example 3 A stretched film was produced in the same manner as in Example 1 except that the relaxation temperature was 80 ° C. and the relaxation rate was 0%. The stretched film was subjected to the humidified TMA test in (4) above, and the dimensional change was 0.90%. Moreover, when this stretched film was subjected to the heating TMA test of the above (3), the dimensional change was 0.18%. A retardation film and a circularly polarizing plate were produced in the same manner as in Example 2 except that the above-mentioned stretched film was used. Comparative Example 4 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 1 except that the stretched film was immersed in warm water at 60 ° C. for 1 minute instead of the above heat treatment.
  • Comparative Example 5 A retardation film and a circularly polarizing plate were produced in the same manner as in Comparative Example 3 except that the stretched film was immersed in warm water at 60 ° C. for 10 minutes instead of the above heat treatment.
  • Comparative Example 6 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 1 except that the heat treatment was not performed.
  • Comparative Example 7 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 19 except that the stretched film was heated at 100 ° C. for 10 minutes.
  • Comparative Example 8 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 19 except that the stretched film was heated at 125 ° C. for 1 minute.
  • Comparative Example 9 A retardation film and a circularly polarizing plate were produced in the same manner as in Example 19 except that the heat treatment was not performed.
  • t 2 / A 3 2 was calculated.
  • t 2 is the immersion time in the hot water treatment step (min)
  • a 3 is a shrinkage ratio in humidified TMA test of the stretched film before the hot water treatment step (%).
  • the retardation films of Examples 1 to 27 and Comparative Examples 1 to 9 were subjected to the humidified TMA test and the heated TMA test, and the dimensional change rate in each test was measured. Furthermore, the humidification phase difference unevenness and the heating phase difference unevenness were measured for Examples 1 to 27 and Comparative Examples 1 to 9. The respective results are shown in Table 1.
  • the retardation film of the example has a smaller dimensional change rate in the TMA test after heat treatment or warm water treatment than the retardation film of the comparative example, and is used for a circularly polarizing plate Inconsistencies in phase difference were also small.
  • the retardation film of the present invention is suitably used for a circularly polarizing plate, and the circularly polarizing plate of the present invention is suitably used for an organic EL panel.

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  • Mechanical Engineering (AREA)
  • Optics & Photonics (AREA)
  • General Physics & Mathematics (AREA)
  • Polarising Elements (AREA)
  • Shaping By String And By Release Of Stress In Plastics And The Like (AREA)
  • Electroluminescent Light Sources (AREA)
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