WO2006101251A1 - Film optique - Google Patents

Film optique Download PDF

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Publication number
WO2006101251A1
WO2006101251A1 PCT/JP2006/306391 JP2006306391W WO2006101251A1 WO 2006101251 A1 WO2006101251 A1 WO 2006101251A1 JP 2006306391 W JP2006306391 W JP 2006306391W WO 2006101251 A1 WO2006101251 A1 WO 2006101251A1
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WIPO (PCT)
Prior art keywords
layer
film
polymer
thickness
optical film
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Application number
PCT/JP2006/306391
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English (en)
Inventor
Tsutomu Sugou
Original Assignee
Fujifilm Corporation
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Publication of WO2006101251A1 publication Critical patent/WO2006101251A1/fr

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B23/00Layered products comprising a layer of cellulosic plastic substances, i.e. substances obtained by chemical modification of cellulose, e.g. cellulose ethers, cellulose esters, viscose
    • B32B23/04Layered products comprising a layer of cellulosic plastic substances, i.e. substances obtained by chemical modification of cellulose, e.g. cellulose ethers, cellulose esters, viscose comprising such cellulosic plastic substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B23/06Layered products comprising a layer of cellulosic plastic substances, i.e. substances obtained by chemical modification of cellulose, e.g. cellulose ethers, cellulose esters, viscose comprising such cellulosic plastic substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material of paper or cardboard
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C41/00Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
    • B29C41/24Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor for making articles of indefinite length
    • B29C41/28Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor for making articles of indefinite length by depositing flowable material on an endless belt
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C55/00Shaping by stretching, e.g. drawing through a die; Apparatus therefor
    • B29C55/02Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets
    • B29C55/04Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets uniaxial, e.g. oblique
    • B29C55/08Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets uniaxial, e.g. oblique transverse to the direction of feed
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04Coating
    • C08J7/043Improving the adhesiveness of the coatings per se, e.g. forming primers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04Coating
    • C08J7/044Forming conductive coatings; Forming coatings having anti-static properties
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04Coating
    • C08J7/046Forming abrasion-resistant coatings; Forming surface-hardening coatings
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04Coating
    • C08J7/056Forming hydrophilic coatings
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29KINDEXING 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
    • B29K2001/00Use of cellulose, modified cellulose or cellulose derivatives, e.g. viscose, as moulding material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29KINDEXING 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
    • B29K2105/00Condition, form or state of moulded material or of the material to be shaped
    • B29K2105/0005Condition, form or state of moulded material or of the material to be shaped containing compounding ingredients
    • B29K2105/0038Plasticisers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2301/00Characterised by the use of cellulose, modified cellulose or cellulose derivatives
    • C08J2301/08Cellulose derivatives
    • C08J2301/10Esters of organic acids
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/11Anti-reflection coatings
    • G02B1/111Anti-reflection coatings using layers comprising organic materials
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/14Protective coatings, e.g. hard coatings
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/16Optical coatings produced by application to, or surface treatment of, optical elements having an anti-static effect, e.g. electrically conducting coatings

Definitions

  • the present invention relates to an optical film.
  • a transparent polymer is used for several sorts of film products.
  • cellulose acylate film is formed from cellulose acylate.
  • a cellulose triacetate (hereinafter TAC) film is formed from the TAC in which averaged acetylation degree is 57.5% to 62.5%, and excellent in the optical isotropy.
  • the TAC film has been used as a film.support for optical sensitive materials because of the strength and inflammability.
  • the TAC film is used for a optical film, such as a protective film for a polarizing filter, or an optical compensation film (for example, a wide view film) and the like in a liquid crystal display while a market of these sorts of the optical films is extended recently.
  • the TAC film is usually produced by a solution casting method, in which the produced film is more excellent in physical properties such as optical properties and the like than other film production method such as a melt extrusion method and the like.
  • a solution casting method polymer is dissolved in a mixture solvent in which dichloromethane or methyl acylate is the main solvent component , so as to prepare a polymer solution (hereinafter, dope) .
  • the dope is cast onto a support by a casting die so as to form a casting film.
  • the casting film has a self-supporting property
  • the casting film is peeled as a wet film from the support and dried to be a film. Thereafter the film is wound up to a film roll, (cf: Japan Institute of Invention and Innovation (JIII) Journal of Technical Disclosure No. 2001-1745)
  • the TAC film on which several sorts of predetermined optical functional layers are formed, is used as optical film.
  • optical film there are an antiglare film (AG) in which an antiglare layer is formed, an low reflective film (LR) which is used for preventing the reflection, an antistatic film (AS) which is used for preventing the dust adhesion, a hard coat film (HC) for preventing the polarizing filter.
  • AG antiglare film
  • LR low reflective film
  • AS antistatic film
  • HC hard coat film
  • An object of the present invention is to provide an optical film having predetermined optical properties , which can be used in an optical field, while the optical functional layers are formed on the polymer film under the predetermined producing conditions .
  • an optical film includes a polymer layer containing polymer, an optical functional layer formed on the polymer layer from a solution containing an optical functional material and a solvent , and a mixture layer formed by dissolving a part of the polymer layer to the solution.
  • the solution is dried on the polymer layer.
  • the polymer and the optical functional material are mixed.
  • a thickness fluctuation of the mixture layer is in ⁇ 10% of an averaged thickness of the mixture layer even in each widthwise and lengthwise direction of the polymer layer.
  • an optical film includes a polymer layer containing polymer, an optical functional layer formed on the polymer layer from a solution containing an optical functional material and a solvent , and a mixture layer formed by dissolving a part of the polymer layer to the solution .
  • the solution is dried on the polymer layer. By dissolving the part of the polymer layer to the solution, the polymer and the optical functional material are mixed. If a thickness of the polymer layer is Ll ( ⁇ m) , the mixture layer is in the range of 0.00IxLl ( ⁇ m) to 0.IxLl ⁇ m).
  • the optical functional layer is one of an antiglare layer, an antireflection layer, an antistatic layer and a hard coat layer.
  • the solvent dissolves the polymer.
  • the polymer layer is transparent .
  • the polymer contains cellulose acylate.
  • the cellulose acylate is cellulose triacetate, and the polymer layer contains triphenyl phosphate as plasticizer.
  • a ratio (P2/P1) is in the range of 0.1 to 0.5 when Pl is a height of peak in the range of 1360 cm “1 to 1380 cm '1 that is caused by the cellulose triacetate in measuring the thickness of the mixture layer by an infrared spectrometer, and P2 is a height of peak in the range of 1480 cm “1 to 1500 cm “1 that is caused by the triphenyl phosphate in measuring the thickness of the mixture layer by the infrared spectrometer.
  • a thickness of the mixture layer is detected from a difference of coloring density between the polymer layer and the optical functional layer by performing an osmium coloring.
  • the polymer layer contains at least one of plasticizer and UV absorbing agent, and a content distribution of the plasticizer or said UV absorbing agent until a predetermined depth from a surface of the polymer layer is in ⁇ 10% from an averaged value of the content in each widthwise and lengthwise direction of the polymer layer.
  • a content distribution of remaining solvent until said predetermined depth is ⁇ 10% from the averaged value in a situation before the optical functional layer is formed.
  • the predetermined depth is 10 ⁇ m.
  • the predetermined depth is in the range of 0.00IxLl to 0.IxLl.
  • the polymer layer is produced by a solution casting method in which a dope is cast onto a support from a casting die, and the optical functional layer is formed on a surface of the polymer layer that is formed on the support .
  • a mixture layer is formed by dissolving compound of the polymer layer and the optical functional layer to a solution which is used for forming the optical functional layer.
  • a thickness fluctuation of the mixture layer is in ⁇ 10% of an averaged thickness of the mixture layer even in each widthwise and lengthwise direction of the polymer layer. Therefore, the optical functions appear almost uniformly on the film surface of the optical film. Further, since the averaged thickness is in the range of 0.1 ⁇ m to 10.0 ⁇ m, the optical functions appear almost uniformly on the film surface of the optical film.
  • the polymer layer of the present invention contains cellulose triacetate as the cellulose acylate and triphenyl phosphate as plasticizer.
  • a ratio (P2/P1) is in the range of 0.1 to 0.5 when Pl is a height of peak in the range of 1360 cm '1 to 1380 cm '1 that is caused by the cellulose triacetate in measuring the thickness of the mixture layer by an infrared spectrometer, and P2 is a height of peak in the range of 1480 cm '1 to 1500 cm "1 that is caused by the triphenyl phosphate in measuring the thickness of the mixture layer by the infrared spectrometer. Therefore, the optical functions appear almost uniformly on the film surface of the optical film.
  • a thickness of the mixture layer is detected from a difference of coloring density between the polymer layer and the optical functional layer by performing an osmium coloring. Therefore, the optical functions appear almost uniformly on the film surface of the optical film.
  • optical film of the present invention there are characteristics as follows:
  • the polymer layer contains at least one of plasticizer and UV absorbing agent, and a content distribution of the plasticizer or said UV absorbing agent until a predetermined depth from a surface of the polymer layer is in ⁇ 10% in each widthwise and lengthwise direction of the polymer layer " ;
  • the polymer layer has a content distribution of remaining solvent is until said predetermined depth is ⁇ 10% in a situation before the optical functional layer is formed;
  • the optical functions appear almost uniformly on the film surface of the optical film. Further, when the above con.ditions are satisfied, the optical functions are almost the same between the different optical films.
  • the predetermined depth is 10 ⁇ m, and thus the above effects can be easily obtained.
  • Figure 1 is a flow chart of processes of producing a polymer film of the present invention
  • Figure 2 is a schematic diagram of a dope production line for producing a dope which is used for producing a polymer film of the present invention
  • Figure 3 is a schematic diagram of a film production line for producing a polymer film of the present invention.
  • Figure 4 is a cross-sectional view of a first embodiment of an optical film which is produced from the polymer film of the present invention
  • Figure 5 is a cross-sectional view of a second embodiment of an optical film which is produced from the polymer film of the present invention.
  • cellulose acylate is used and especially preferably triacetyl cellulose.
  • cellulose acylate it is preferable that the degree of substitution of acyl groups for hydrogen atoms on hydroxyl groups of cellulose preferably satisfies all of following formulae (I)-(III).
  • A is the degree of substitution of the acetyl groups for the hydrogen atoms on the hydroxyl groups of cellulose
  • B is the degree of substitution of the acyl groups for the hydrogen atoms while each acyl group has carbon atoms whose number is from 3 to 22.
  • at least 90 wt.% of TAC is particles having diameters from 0.1 mm to 4 mm.
  • the polymer to be used in the present invention is not restricted in cellulose acylate.
  • a glucose unit constructing cellulose with ⁇ -1 , 4 bond has the free hydroxyl groups on 2 nd , 3 rd and 6 th positions.
  • Cellulose acylate is polymer in which, by esterification, the hydrogen atoms on the part or all of the hydroxyl groups are substituted by the acyl groups having at least two carbon atoms.
  • the degree of acylation is the degree of the esterification of the hydroxyl groups on the 2 nd , 3 rd , 6 th positions. In each hydroxyl group, if the esterification is made at 100%, the degree of acylation is 1.
  • the degree of the acylation is described as DS2- (the degree of substitution by acylation on the 2 nd position)
  • the degree of the acylation is described as DS3 (the degree of substitution by acylation on the 3 rd position)
  • the degree of the acylation is described as DS6 (the degree of substitution by acylation on the 6 th position) .
  • the total of the degree of acylation, DS2+DS3+DS6, is preferably 2.00 to 3.00, particylarly 2.22 to 2.90 , and especially 2.40 to 2.86. Further, DS6/(DS2+DS3+DS6) is preferably at least 0.28, particularly at least 0.30, and especially 0.31 to 0.34.
  • the number and sort of the acyl groups in cellulose acylate may be only one or at least two. If there are at least two sorts of acyl groups, one of .them is preferable the acetyl group. If the hydrogen atoms on the 2 nd , 3 rd and 6 th hydroxyl groups are substituted by the acetyl groups, the total degree of substitution is described as DSA, and if the hydrogen atoms on the 2 nd , 3 rd and 6 th hydroxyl groups are substituted by the acyl groups other than acetyl groups, the total degree of substitution is described as DSB.
  • the value of DSA+DSB is preferably 2.22 to 2.90, especially 2.40 to 2.86.
  • DSB is preferably at least 1.50, and especially at least 1.7.
  • the percentage of the substitution on the 6 th position to that on the 2 nd , 3 rd and 6 th positions is at least 20%. However, the percentage is preferably at least 25%, particularly at least 30%, and especially at least 33%.
  • DSA+DSB of the 6 th position of the cellulose acylate is preferably at least 0.75, particularly at least 0.80, and especially at least 0.85.
  • cellulose acylate the acyl group having at least 2 carbon atoms may be aliphatic group or aryl group, and is not restricted especially.
  • cellulose acylate is, for example, alkylcarbonyl ester and alkenylcarbonyl ester of cellulose.
  • aromatic carbonyl ester, aromatic alkyl carbonyl ester, or the like there are aromatic carbonyl ester, aromatic alkyl carbonyl ester, or the like, and these compounds may have other substituents .
  • the compounds there are propionyl group, butanoyl group, pentanoly group, hexanoyl group, octanoyl group, decanoyl group, dodecanoyl group, tridecanoyl group, tetradecanyol group, hexadecanoyl group, octadecanoyl group, iso-butanoyl group, t-butanoyl group, cyclohexanecarbonyl group, oleoyl group, benzoyl . group, naphthylcarbonyl group, cinamoyl group and the like.
  • the particularly preferable groups are propionyl group, butanoyl group, dodecanoyl group, octadecanoyl group, t-butanoyl group, oleoyl group, benzoyl group, naphthylcarbonyl group, cinamoyl group and the like, and the especially preferable groups are propionyl group and butanoyl group .
  • solvents for preparing the dope there are aromatic hydrocarbons (for example, benzene, toluene and the like), hydrocarbon halides (for example, dichloromethane, ⁇ hlorobenzene and the like), alcohols (for example, methanol, ethanol, n-propanol, n-butanol, diethyleneglycol and the like) , ketones (for example, acetone, methylethyl ketone and the like) , esters (for example, methyl acetate, ethyl acetate, propyl acetate and the like), ethers (for example, tetrahydrofuran , methylcellosolve and the like) and the like.
  • aromatic hydrocarbons for example, benzene, toluene and the like
  • hydrocarbon halides for example, dichloromethane, ⁇ hlorobenzene and the like
  • alcohols for example, methanol, ethanol, n-propan
  • the solvents are preferably hydrocarbon halides having 1 to 7 carbon atoms , and especially dichloromethane .
  • one or several sorts of alcohols having 1 to 5 carbon atoms is mixed with dichloromethane.
  • the content of the alcohols to the entire solvent is preferably in the range of 2 mass% to 25 mass%, and particularly in the range of 5 mass% to 20 mass%.
  • the preferable examples for the alcohols are methanol, e.thanol, n-butanol, or a mixture thereof.
  • ethers having 4 to 12 carbon atoms, ketones having 3 to 12 carbon atoms , esters having 3 to 12 esters , and alcohols having 1 to 12 carbons are preferable, and a mixture thereof can be used.
  • These ethers, ketones and esters may have the ring structure.
  • the compounds having at least two of functional groups (namely, -O- , -CO-, -COO- and -OH) in ethers, ketones and esters can be used for the solvent.
  • the additives (such as the solvent, plasticizer, deterioration inhibitor, UV absorbing agent, optically anisotropic controller, retardation controller, dyne, matting agent, release agent, releasing accelerator and the like) are described in detail from [0196] to [0516] of Japanese Patent Laid-Open Publication No. 2005-104148.
  • a dope 15 is obtained in a dope production process 14 from TAC 11, solvent 12 and additive 13.
  • the dope 15 is used in a casting process 16, and then a dry-stretching process 17, an aftertreatment process 18 follow.
  • a polymer film 19 is obtained and continuously wound to a film roll 21 in a winding process 20.
  • the polymer film 19 is unwound from the film roll 21 and coated with predetermined coating liquids in a coating process 22 such that several sorts of optical functional layers .
  • a production film 23 is obtained.
  • the dope production process 14 is performed in a dope production line 30, as shown in FIG.l.
  • the dope production line 30 is constructed of a solvent tank 31 for storing a solvent , a mixing tank 32 for mixing the TAC 11 and the solvent 12 therein, a hopper 33 for supplying the TAC 11 and an additive tank 34 for storing an additive.
  • a heating device for heating a swelling liquid (described below in detail)
  • a temperature controlling device 36 for controlling the temperature of prepared polymer solution
  • a filtration device 37 for controlling the temperature of prepared polymer solution
  • there are a flushing device 50 for concentrating the polymer solution and a filtration device 51.
  • the dope production line 30 is connected through the stock tank to a film production line 60.
  • the dope 15 is produced in the following order.
  • a valve 38 is opened, the solvent 12 is sent from the solvent tank 31 to the mixing tank 32. Amount of the solvent is controlled by adjusting the valve 38. Then the TAC 11 in the hopper 33 is sent to the mixing tank 32. Thereafter, a valve 39 is opened such that the additive is sent from the additive tank 34 to the mixing tank 32.
  • the method of feeding the additive to the mixing tank is not restricted in the above description. If the additive is in the liquid state in the room temperature, it may be fed in the liquid state to the mixing tank 32 without preparing for the additive solution. Otherwise, if the additive is in the solid state in the room temperature, it may be fed in the solid state to the mixing tank 32 with use of a hopper. If plural sorts of additive compounds are used, the additive containing the plural additive compounds may be accumulated in the additive tank 34 altogether. Otherwise plural additive tanks may be used so as to contain the respective additive compounds, which are sent through independent pipes to the mixing tank 32.
  • the solvent 12, the TAC 11, and the additive 13 are sequentially sent to the mixing tank 32.
  • the sending order is not restricted in it.
  • the feeding of the predetermined amount of the solvent and the additive may be performed to obtain a TAC solution.
  • the additive 13 may be added to a mixture of TAC and solvent in following processes.
  • the mixing tank 32 is provided with a jacket 40 covering over an outer surface of the mixing tank 32, a first stirrer 42 to be rotated by a motor 41, and a second stirrer 44 to be rotated by a motor 43.
  • the first stirrer 42 preferably has an anchor blade, and the second stirrer 44 is preferably an eccentric stirrer of a dissolver type.
  • the jacket is provided with a temperature controlling device for controlling the temperature of a heat transfer medium flowing in the jacket. Thus the inner temperature in the mixing tank 32 is controlled.
  • the preferable inner temperature is in the range of -10 0 C to
  • At least one of the first and second stirrers 42, 44 is adequately chosen for performing the rotation. Thus a swelling liquid 45 in which TAC is swollen in the solvent is obtained.
  • a pump 46 is driven such that the swelling liquid 45 in the mixing tank 32 may be sent to the heating device 35 which is preferably a pipe with a jacket. Further, the heating device
  • the swelling liquid 45 may be a polymer solution.
  • the polymer solution may be a solution in which the polymer is entirely dissolved and a swelling liquid in which the polymer is swollen.
  • the temperature of the swelling liquid 45 is preferably in the range of 50 0 C to 12O 0 C .
  • the swelling liquid 45 may be cooled in the range of -100 0 C to -3O 0 C so as to perform the dissolution, which is already known as the cool-dissolution method.
  • one of the heat-dissolution and cool-dissolution methods can be chosen in accordance with the properties of the materials, so as to control the solubility.
  • the dissolution of TAC to the solvent can be made enough.
  • the polymer solution is fed to the temperature controlling device 36, so as to control the temperature nearly to the room temperature.
  • the filter material of the filtration device 51 preferably has an averaged nominal diameter of at most 100 ⁇ m.
  • the flow rate of the filtration in the filtration device 51 is preferably at least 50 liter/hr.
  • the polymer solution after the filtration is fed through a valve 48 to a stock tank 61.
  • the polymer solution can be used as dope 15 for a film production, which will be explained.
  • the time for production of such dope becomes longer. Consequently, the production cost becomes higher. Therefore, it is preferable that a polymer solution of the lower concentration than the predetermined value is prepared at first and then the concentrating of the polymer solution is made.
  • the polymer solution after the filtration is sent to the flushing device 50 through the valve 48. In the flushing device 50, the solvent of the polymer solution is partially evaporated.
  • the solvent vapor generated in the evaporation is condensed by a condenser (not shown) to a liquid state, and recovered by the recovering device 52.
  • the recovered solvent is recycled by a recycling device 53 and reused. According to this method, the decrease of cost can be designated, since the production efficiency becomes higher and the solvent is reused.
  • the polymer solution after the concentrating as the above description is extracted from the flushing device 50 through a pump 54. Further, in order to remove bubbles generated in the polymer solution, it is preferable to perform the bubble removing treatment. As a method for removing the bubble, there are many methods which are already known, for example, an ultrasonic irradiation method and the like. Then the polymer solution is fed to the filtration device 37, in which the undissolved materials are removed. Note that the temperature of the polymer solution in the filtration device 37 is preferably in the range of O 0 C- to 200 0 C .
  • the polymer solution after the filtration is stored in the stock tank 61, which is provided with a stirrer 81 rotated by a motor 80. The stirrer 81 is rotated so as to continuously stir the dope 15.
  • a dope produced the produced dope preferably has the TAC concentration in the range of 5 mass% to 40 mass%, particularly 15 mass% to 30 mass%, and especially 17 mass% to 25 raass%. Further, the concentration of the additive (mainly plasticizer) is preferably in the range of 1 mass% to 20 mass%, if the solid content in the dope 15 is 100 mass%.
  • the film production line 60 includes the stock tank 61, a filtration device 62, a casting die 63, back-up rollers 64, 65, a belt supported by the back-up rollers 64, 65, and a tenter device 67. Further, there are an edge slitting device 70, a drying chamber 71, a cooling chamber 72 and a winding chamber 73. In the stock tank 61, there is the stirrer 81 rotated by the motor 80.
  • the stock tank 61 connects the dope production line 30 to the film production line 60, while being connected to the casting die 63 through a pump 82 and the filtration device 62.
  • the materials of the casting die 63 are preferably precipitation hardening stainless steel.
  • the preferable material has coefficient of thermal expansion of at most 2 x 10 "5 ( 0 C "1 J .
  • the material to be used has an anti-corrosion property, which is almost the same as SUS316, in the examination of forcible corrosion in the electrolyte solution.
  • the materials to be used for the casting die 63 has such resistance of corrosion that the pitting doesn't occur on the gas-liquid interface even if the material is dipped in a mixture of dichloromethane , methanol and water for three months.
  • the casting die 63 is preferably manufactured by performing the polishing after a month from the material casting.
  • the finish precision of a contact face of the casting die to dope 15 is at most 1 ⁇ m in surface roughness and at most 1 ⁇ m/m in straightness.
  • the clearance of a slit of the casting die 63 is automatically adjustable in the range of 0.5 mm to 3.5 mm.
  • R is at most 50 ⁇ m in all of a width.
  • the shearing rate in the casting die 63 is controlled in the range of 1 to 5000 per second.
  • a width of the casting die 63 is not restricted especially. However, the width is preferably at least 1.01 times and at most 1.3 times as large as a film width.
  • the casting die 63 is preferably a coat hanger type die. Further, in order to adjust a film thickness, the casting die 63 is preferably provided with an automatic thickness adjusting device.
  • thickness adjusting bolts are disposed at a predetermined distance in a widthwise direction of the casting die 63.
  • the profile is set on the basis of a predetermined program, depending on feed rate of pumps (preferably, high accuracy gear pumps), while the film production is performed.
  • the film production line 60 may be provided with a thickness meter (not shown) , such as infrared ray thickness meter and the like.
  • the feed back control of the adjustment value of the heat bolts may be made by the adjusting program on the base of the profile of the thickness meter.
  • the thickness difference between any two points in the widthwise direction except the side edge portions in the casting film is controlled preferably to at most 1 //m.
  • the difference between the maximum and the minimum of the thickness in the widthwise direction is at most 3 ⁇ m, and especially at most 2 ⁇ m.
  • the accuracy to the designated object value of the thickness is preferably in ⁇ 1.5 ⁇ m.
  • a hardened layer is preferably formed on a top of a lip end of the casting die 63.
  • a method of forming the hardened layer is not restricted. But it is, for example, ceramics hard coating, hard chrome plating, neutralization processing, and the like. If ceramics is used as the hardened layer, it is preferable that the used ceramics is grindable but not friable, with a lower porosity, high resistance of corrosion, and poor adhesiveness to the casting die 63. Concretely, there are tungsten carbide (WC), Al 2 O 3 , TiN, Cr 2 O 3 , and the like. Especially preferable ceramics is tungsten carbide. Tungsten carbide coating can be made by a spraying method.
  • a solvent supplying device (not shown) at the slit ends, on which a gas-liquid interfaces are formed between both edges of the slit and between both bead edges and the outer gas.
  • these gas-liquid interfaces are supplied with the solvent which can dissolve the dope, (for example a mixture solvent of dichloromethane 86.5 pts.mass, acetone 13 pts.mass, n-butanol 0.5 pts.mass).
  • the supply rate to each slit end is preferably in the range of 0.1 mL/min to 1.0 mL/min, in order to prevent the foreign materials from mixing into the casting film.
  • the pump for supplying the solvent has a pulse rate (or ripple factor) at most 5%.
  • a belt 66 is positioned below the casting die 63, and lapped on back-up rollers 64, 65. When the back-up rollers 64,
  • the belt 66 are rotated by the driving device (not shown) , and thus the belt 66 runs endlessly in accordance with the rotation of the back-up rollers 64, 65. Then the casting speed is preferably in the range of 10 m/min to 200 m/min. Further, the temperatures of the back-up rollers 64, 65 are controlled by a heat transfer medium circulator 83 for cycling a heat transfer medium. It is preferable that the surface temperature of the belt 66 is adjusted in the range of -20 0 C to 40 0 C by heat transmission from the back-up rollers 64, 65.
  • the back-up rollers 64 , 65 paths (not shown) of the heat transfer mediums are formed in the back-up rollers 64 , 65 , and the heat transfer mediums whose temperatures are controlled by the heat transfer medium circulator 83 pass through the paths.
  • the temperature of the back-up rollers 64, 65 are kept to the predetermined values.
  • the width, the length and the material of the belt 66 are not restricted especially. However, it is preferably 1.05 to 1.5 times as large as the casting width.
  • the length is from 20m to 100m, and the thickness is from 1 mm to 2 mm.
  • the surface is preferably polished so as to have a surface roughness at most 0.05 ⁇ m.
  • the belt 66 is preferably made of stainless steel, and especially of SUS 316 so as to have enough resistance of corrosion and strength.
  • the thickness unevenness of the entire belt 66 is preferably at most 0.5%.
  • the back-up roller used as support is preferably rotated at high accuracy such that a rotation flutter may be at most 0.2 mm. Therefore the surface roughness is preferably at most 0.01 ⁇ m.
  • the chrome plating is preferably performed to the drum such that the drum may have enough hardness and endurance.
  • the surface defect must be reduced to be minimal. Concretely there are no pin hole of at least 30 ⁇ m, at most one pin hole in the range of 10 ⁇ m to 30 ⁇ m, and at most two pin holes of less than 10 /(m per 1 m 2 .
  • a temperature controlling device 85 is provided for controlling the inner temperature of a casting chamber 84 to the predetermined value and a condenser 86 for condensing organic solvent evaporated in the casting chamber 84. Further a recovering device 87 for recovering the condensed organic solvent outside the casting chamber 84. Further, the cast dope forms a bead between the casting die 63 and the belt 66. In order control the pressure in a rear side of the bead, it is preferable to dispose a decompression chamber 88, as in this embodiment.
  • Air ducts 90, 91, 92 are disposed around the belt 66, so as to feed out through outlets drying airs for drying the casting film 89 formed on the belt 66. Further, an air shielding plate 93 is preferably disposed at the outlet of the air duct 90 near the casting die 63, so as to control the surface condition variation of the casting film 89 that is caused by applying the drying air to the casting film 89 just after the formation thereof .
  • a transfer area 100 there is an air blower 101. Then the wet film 94 is stretched and dried in the tenter device 67 and fed out as polymer film 19. Thereafter, the edge slitting device 70 slits off both side edge portions of the polymer film 19 into tips, and the tips of both side edge portions are crushed by a crusher 110 connected to the edge slitting device 70.
  • the polymer film 19 is transported with lapping on rollers 111.
  • the solvent vapor evaporated from the polymer film 19 by the drying chamber 71 is adsorbed by an adsorbing device 112.
  • the polymer film 19 is transported into the cooling chamber 72, and cooled therein to around the room temperature.
  • a humidity control chamber (not shown) may be provided for conditioning the humidity between the drying chamber 71 and the cooling chamber 72.
  • a compulsory neutralization device (or a neutralization bar) 113 eliminates the charged electrostatic potential of the polymer film 19 to the predetermined value (for example, in the range of -3kV to +3kV) .
  • the position of the neutralization process is not restricted in this embodiment.
  • the position may be a predetermined position in the drying section or in the downstream side from a knurling roller 114, and otherwise, the neutralization may be made at plural positions .
  • the polymer film 19 is wound by the winding shaft 115. At this moment, a tension is applied at the predetermined value to a press roller 116.
  • the dope 15 is always made uniform by rotating the stirrer 81. Also in the stirring, the additive (for example, plasticizer and the UV-absorbing agent and the like) can be mixed.
  • the pump 82 is driven to feed the dope 15 to the filtration device 62, and then filtration is made. Thereafter the dope 15 is cast from the casting die 63 onto the belt 66 to form the casting film 89.
  • the drive of the back-up rollers 64, 65 is controlled such that the tension generating in the belt 66 may be in the range of 10 4 N/m to 10 6 N/m.
  • the relative speed between the belt and the back-up rollers 64, 65 adjusted to at most 0.01 m/min.
  • the control was made such that the variation of the speed of the belt 66 was at most 0.5% to the predetermined value.
  • the position of the belt in the widthwise direction was controlled with detection of the position of the side end, such that meandering in one circle of the moving belt 66 was reduced in 1.5 mm.
  • the variation of the position in the vertical direction between the lip end of the casting die and the belt 66 was in 200 ⁇ m.
  • the belt 66 is preferably incorporated in the casting chamber 84 which has air pressure controller (not shown) .
  • the temperature in the casting chamber 84 is controlled in the range Of -IO 0 C to 57 0 C . Note that the solvent vapor is recovered by the recovering device 87, and used as a solvent for preparing the dope after the refinement .
  • the dope 15 is cast from the casting die 63 onto the belt 66, so as to form the casting film 89.
  • the temperature of the dope 15 is preferably controlled in the range of -10 0 C to 57 0 C .
  • the decompression is made such that the pressure of the back side may be 2000 Pa to 10 Pa lower than that of the front side. It is preferable to provide the decompression chamber 88 with a jacket (not shown) for controlling the inner temperature.
  • the temperature of the decompression chamber 88 is not restricted especially.
  • the temperature is preferably at least the boiling point of the used organic solvent.
  • aspirators (not shown) may be provided with the decompression chamber 88 so as to be near both side edges of a dope outlet of the casting die 63.
  • the aspiration in both side edges of the bead is made to stabilize the shape of the bead.
  • the force velocity of the aspiration is preferably in the range of one to one hundred Litter/min.
  • the drying airs are applied from the air ducts 90, 91, 92 to the casting film 89 conveyed in accordance with running the belt 66 , such that the evaporation of the solvent may proceed.
  • the air shielding plate 93 reduces the change of the surface condition.
  • the surface temperature of the belt 66 is preferably in the range of -20 0 C to 40 0 C .
  • the casting film 89 is continuously peeled as wet film 94 with support of the peeling roller 95.
  • the solvent content at the peeling is preferably in the range of 20 mass% to 250 mass% to the solid content. Then the wet film 94 is transported in the transfer area 100 in which many rollers are provided, and thus transported into the tenter device 67.
  • a drying air is fed from the air blower to dry the wet film 94, such that the drying may proceed.
  • the temperature of the drying air is in the range of 20 0 C to 25O 0 C .
  • the rotating speed of the pass roller may be set to be higher in the downstream side, so as to draw the wet film 94.
  • the wet film 94 is held by clipping both side edge portions, and at the same time the drying is made to evaporate the solvent.
  • the tenter device 67 is preferably partitioned into several temperature areas of different temperatures, such that the drying is made under different drying conditions of the respective temperature areas.
  • the stretching of the wet film 94 in the widthwise direction may be made.
  • the stretching in the widthwise direction and the drawing in the lengthwise direction are made such that the width and the length may be in the range of 0.5% to 300% larger than the original size.
  • the wet film 94 is dried until the content of the remaining solvent become the predetermined value, and fed out as polymer film 19 from the tenter device 67 toward the edge slitting device 70 for slitting off both side edge portions.
  • the slit side edge portions are sent to the crusher 110 by a cutter blower (not shown), and crushed to tips by the crusher 110.
  • the tips are reused for preparing the dope, which is effective in view of the decrease of the production cost. Note that the slitting process of both side edge portions may be omitted. However, it is preferable to perform the slitting between the casting process and the winding process.
  • the polymer film 19 whose side edge portions are slit off is sent to a drying chamber 71 and dried furthermore.
  • the drying chamber 71 the polymer film 19 is transported with lapping on the rollers 111.
  • the inner temperature of the drying chamber 71 is not restricted especially. However, it is preferable in the range of 50 0 C to 160 0 C .
  • the solvent vapor evaporated from the polymer film 19 by the drying chamber 71 is adsorbed by the adsorbing device 112.
  • the air from which the solvent components are removed is reused for the drying air in the drying chamber 71.
  • the drying chamber 71 preferably has plural partitions for variation of the drying temperature.
  • a pre-drying chamber (not shown) is provided between the edge slitting device 70 and the drying chamber 71, so as to perform the pre-drying of the polymer film 19.
  • the polymer film 19 is transported into the cooling chamber 72, and cooled therein to around the room temperature.
  • a humidity control chamber (not shown) may be provided for conditioning the humidity between the drying chamber 71 and the cooling chamber 72.
  • an air whose temperature and humidity are controlled is applied to the polymer film 19.
  • a compulsory neutralization device (or a neutralization bar) 113 eliminates the charged electrostatic potential of the polymer film 19 to the predetermined value (for example, in the range of -3kV to +3kV) .
  • the position of the neutralization process is not restricted in this emb ⁇ diment .
  • the position may be a predetermined position in the drying section or in the downstream side from the knurling roller 114, and otherwise, the neutralization may be made at plural positions.
  • the embossing of both side portions of the polymer film 19 is made by the embossing rollers to provide the knurling.
  • the emboss height from the bottom to the top of the embossment is in the range of 1 ⁇ m to 200 ⁇ m.
  • the polymer film 19 is wound by a winding shaft 115 in the winding chamber 73.
  • a tension is applied at the predetermined value to a press roller 116.
  • the tension is gradually changed from the start to the end of the winding.
  • the length of the polymer film 19 is preferably at least 100m.
  • the width of the film is preferably at least 600 mm, and particularly in the range of 1400 mm to 1800 mm. Further, even if the width is more than 1800 mm, the present invention is effective. When it is designated to produce the film which is 15 ⁇ m to 100 ⁇ i in thickness, the present invention is also applied.
  • a feed block may be attached to the casting die as in this embodiment, or a multi-manifold type casting die (not shown) may be used.
  • the plural dopes are cast onto a support to form a casting film having a first layer (uppermost layer) and a second layer (lowermost layer) . Then in the produced film, at least one of the thickness of the first layer and that of the lowermost layer opposite thereto is preferably in the range of 0.5% to 30% of the total film thickness.
  • a dope of. higher viscosity is sandwiched by lower-viscosity dopes.
  • the dopes for forming the surface layers have lower viscosity than the dope for forming a layer sandwiched by the surface layers.
  • the co-casting it is preferable in the bead between a die slit (or die lip) and the support that the composition of alcohol is higher in the two outer dopes than the inner dope.
  • Japanese Patent Laid-Open Publication No. 2005-104148 describes from [0617] to [0889] in detail about the structures of the casting die, the decompression chamber, the support and the like, and further about the co-casting, the peeling, the stretching, the drying conditions in each process, the handling method, the curling, the winding method after the correction of planarity, the solvent recovering method, the film recovering method. The descriptions thereof can be applied to the present invention.
  • Japanese Patent Laid-Open Publication No. 2005-104148 describes from [0112] to [0139] about the properties of the wound cellulose acylate film and the measuring method thereof.
  • the properties and the measuring methods can be applied to the present invention.
  • the cellulose acylate film is preferably used in several ways after the surface treatment of at least one surface.
  • the preferable surface treatments are vacuum glow discharge, plasma discharge under the atmospheric pressure, UV-light irradiation, corona discharge , flame treatment , acid treatment and alkali treatment. Further it is preferable to make one of these sorts of the surface treatments .
  • the polymer film 19 may be provided with an undercoating layer on at least one of the surfaces, and used in the several ways.
  • the polymer film 19 as base film to which at least one of functional layers may be provided in the coating process 22 so as to obtain the production film 23.
  • the production film 23 as optical film in which the optical functional layers are formed on the polymer film 19 is obtained easily.
  • the preferable functional layers are an antiglare layer, an antireflection layer, an antistatic layer, a cured resin layer (hard coat layer) , an easily adhesive layer and an optical compensation layer.
  • materials for forming the antiglare layer there are inorganic or organic particles which can provide unevenness on the film surface, active curable resins as binder, and the like.
  • silicon dioxide and active cursive resin are combined in use.
  • materials for forming the antireflection layer there are high refractive index metal alcoxide, low refractive index material containing fluorine or silicon, SiO 2 sol of low refractivity, gel sheet of reactive organic compounds , and the like, and it is preferable to combine some of them in use.
  • materials for forming the antistatic layer there are ionic conductive material, conductive particles, cationic conductive resin and the like, and it is preferable to use electronic conductive material.
  • materials for forming the hard coat layer there are UV curable resin, electron beam curable resin and the like , and it is preferable to use UV curable resin.
  • hydrophilic polymer containing -COOM group vinyl maleic acid polymer containing -COOM group, vinyl maleic acid - maleic acid anhydride containing -COOM group, and it is preferable to use vinyl acetate - maleic acid co-polymer containing -COOM group .
  • coating method there is a already known coating device (coater) , for example, die coater (extrusion coater, slide coater) , roll coater (coater having normal rotation roller, coater having reverse rotation roller, gravure coater) , rod coater, blade coater and the like.
  • coating speed is not especially restricted, it is preferably in the range of 5 m/min to 180 m/min, particularly in the range of 10 m/min to 150 m/min. Further, the temperature of the coating solution is not especially restricted.
  • the temperature is preferably in the range of 5 0 C to 5O 0 C , and particularly in the range of 10 0 C to 40 0 C , so as to easily make the dissolution and the swelling of the polymer and the evaporation of the solvent.
  • the drying chamber has the inner temperature, preferably in the range of 2O 0 C to 16O 0 C and especially in the range of 30 0 C to 140 0 C, such that the TAC may be dissolved to or swelled in the coating solution.
  • the transportation time in the drying chamber is preferably in the range of 0.1 min to 30 min, and especially to 0.5 min to 10 min.
  • the production film 23 is constructed of the polymer film 19 and an optical functional layer 120 which is formed on a coating surface 19a of the polymer film 19.
  • the coating surface 19a is preferably a surface in a support side (hereinafter support side surface) in the film production.
  • another surface is named an air side surface 19b, since being disposed to air in the film production.
  • a thickness Ll ( ⁇ m) of the polymer film 19 is preferably in the range of 10 ⁇ m to 150 ⁇ m, particularly in the range of 30 ⁇ m to 120 ⁇ m, and especially in the range of 40 ⁇ m to 100 ⁇ m.
  • a thickness L2 ( ⁇ m) of the optical functional layer 120 is preferably in the range of 0.1 ⁇ m to 20 ⁇ m, particularly in the range of 0.5 ⁇ m to 15 ⁇ m, and especially in the range of 1 ⁇ m to 10 ⁇ m.
  • the optical functional layer 120 contains the solvent.
  • the dissolvable material elements in the polymer film 19 to the solvent of the coating solution and the optical functional material elements are mixed to form a mixture layer 121.
  • a thickness of the mixture layer 121 is controlled in the widthwise and lengthwise directions of the production film 23.
  • the difference between the thickness and an average thickness L3 ( ⁇ m) of the mixture layer 121 is preferably in ⁇ 10%, particularly in ⁇ 7%, and especially ⁇ 3%.
  • the average thickness L3 ( ⁇ m) of the mixture layer 121 is preferably in the range of 0.1 ⁇ m to 10.0 ⁇ m, particularly in the range of 0.1 ⁇ m to 7 ⁇ m, and especially in the range of 0.1 ⁇ m to 0.3 ⁇ m. Further, the average thickness L3 is preferably in the range of 0.00IxLl to 0.IxLl, particularly in the range of 0.002xLl to 0.IxLl, and especially in the range of 0.0IxLl to 0.IxLl. Further, the difference of the actual thickness between any points of the mixture layer from the start to the end position of the winding to the film roll is preferably in the range of ⁇ 10% of the average thickness L3, particularly ⁇ 5%, and especially ⁇ 3%. Furthermore, the difference of the actual thickness at any point between the different film rolls is preferably in the range of ⁇ 10% of the average thickness L3, particularly ⁇ 5%, and especially ⁇ 3%.
  • the measurement of the thickness of the mixture layer 121 is made as follows .2Og of a mixture of cyclohexanone and toluene (mixture ratio is 7:3 in weight ratio) is coated on 1 m 2 of the polymer film 19. Then the drying is made at 100 0 C for 50 minutes . Thereafter, the coated film is cut into fragments of 10 mm x 50 nm by a microtome. Thereafter, the dying method in gas phase exposure of the fragments is made in a tightly closed chamber with use 1% osmium tetroxide aqueous solution, so as to dye the fragments. The difference of the dye concentration of the dyed fragments is observed with use of a scanning electron microscope (SEM) . The difference of the die concentration is estimated with eyes . In followings , this measuring method is called a measuring method of mixture layer thickness.
  • SEM scanning electron microscope
  • the thickness of the mixture layer 121 can be also calculated by measuring a quantity of additive contained in the polymer film 19.
  • the additive is not restricted especially, but preferably TPP which is usually used as plasticizer of the polymer film.
  • the measurement is made in ATR method (IR method of reflective type) .
  • the device therefor is FT-IR (Fourier Transform Infrared Spectrometer) .
  • As prism NaCl or KBr is used.
  • the prism is contacted to the fragment to perform the measurement.
  • a ratio of the peaks (P2/P1) is calculated and used for the estimation.
  • the ratio (P2/P1) is preferably in the range of 0.1 to 0.5, particularly in the range of 0.1 to 0.4, and especially in the range of 0.1 to 0.3.
  • the polymer film 19 of the present invention preferably contains at least plasticizer or UV absorbing agent.
  • the content distribution until 10 ⁇ m in depth in thickness direction of the polymer film 19 is preferably in ⁇ 10% in each of the width- and lengthwise directions, particularly in ⁇ 7%, and especially in ⁇ 3%.
  • the standardized depth ( ⁇ m) of the content distribution area in the thickness direction of the polymer film 19 is preferably in the range of 0.00IxLl to 0.IxLl, particularly in the range of 0.002xLl to 0.IxLl, and especially in the range of 0.0IxLl to 0.IxLl.
  • the measurement of the content of the plasticizer and the UV absorbing agent is made by the already known methods , such as ATR method, TOF-SIMS method, ESCA method and the like.
  • the crystallinity of the polymer until 10 //in in depth in thickness direction of the polymer film 19 is preferably in ⁇ 10% in each of the width- and lengthwise directions, particularly in ⁇ 7%, and especially in ⁇ 3%.
  • the standardized depth ( ⁇ m) of the crystallization distribution area in the thickness direction of the polymer film 19 is preferably in the range of 0.00IxLl to 0.IxLl, particularly in the range of 0.002xLl to 0.IxLl, and especially in the range of 0.01 x Ll to 0.1 x Ll.
  • the measurement of the crystallization distribution of the polymer is made by the already known methods, such as IR method, X ray diffraction method and the like.
  • the content distribution of the remaining solvent until 10 /im in depth in thickness direction of the polymer film 19 is preferably in ⁇ 10%.in each of the width- and lengthwise directions, particularly in ⁇ 7%, and especially in ⁇ 3%.
  • the standardized depth ( ⁇ m) of the content distribution area of the remaining solvent in the thickness direction of the polymer film 19 is preferably in the range of 0.00IxLl to 0.IxLl, particularly in the range of 0.002xLl to 0.IxLl, and especially in the range of 0.0IxLl to 0. IxLl .
  • the measurement of the content distribution of the remaining solvent is made by the already known methods , such as thickness measurement, evaporation by dryness, gas chromatography and the like.
  • the degree distribution of in-plane orientation until 10 ⁇ m in depth in thickness direction of the polymer film 19 is preferably in ⁇ 10% in each of the width- and lengthwise directions, particularly in ⁇ 7%, and especially in ⁇ 3%.
  • the standardized depth ( ⁇ m) of the degree distribution area of in-plane orientation in the thickness direction of the polymer film 19 is preferably in the range of 0.00IxLl to 0.IxLl, particularly in the range of 0.002xLl to O.lxLl, and especially in the range of 0.0IxLl to O.lxLl.
  • the measurement of the degree distribution of in-plane orientation is made by the already known methods, such as birefringence method, X ray diffraction method and the like .
  • These functional layers preferably contain at least one sort of surfactants in the range of 0.1 mg/m 2 to 1000 mg/m 2 . Further, the functional layers preferably contain at least one sort of plasticizers in the range of 0.1 mg/m 2 to 1000 mg/m 2 . The functional layers preferably contain at least one sort of matting agents in the range of 0.1 mg/m 2 to 1000 mg/m 2 . The functional layers preferably contain at least one sort of antistatic agents in the range of 1 mg/m 2 to 1000 mg/m 2 .
  • the produced cellulose acylate film can be effectively used as a protection film for a polarizing filter.
  • the cellulose acylate film is adhered to a polarizer.
  • two polarizing filters are adhered to a liquid crystal layer such that the liquid crystal display may be produced.
  • the arrangement of the liquid crystal layer and the polarizing filters are not restricted in it, and several arrangements already known are possible.
  • Japanese Patent Laid-Open Publication No. 2005-104148 discloses the liquid crystal displays of TN type, STN type, VA type, OCB type, reflective type, and other types in detail. The description may be applied to the present invention.
  • the produced film can be used as an optical compensation film since being double axial cellulose acylate film provided with adequate optical properties.
  • the optical compensation film can be used as a protective film for a polarizing filter. The detail description thereof is made from [1088] to [1265] in the publication No. 2005-104148.
  • the formed cellulose acylate film is excellent in optical properties .
  • the TAC film can be used as the protective film for the polarizing filter, a base film of the photosensitive material, and the like.
  • the produced film can be also used for the optical compensation film.
  • the produced film is effectively used when it doubles as protective film for the polarizing filter. Therefore, the film is not only used in the TN-mode as prior mode, but also IPS-mode, OCB-mode, VA-mode and the like.
  • the polarizing filter may be constructed so as to have the protective film as construction element.
  • composition of the dope (or polymer solution) used for the film production will be shown.
  • Example 1 Composition of Cellulose Triacetate 100 pts.mass
  • Plasticizer A (triphenylphosphate) 7.6 pts.mass
  • Plasticizer B (diphenylphosphate) 3.8 pts.mass
  • UV-agent A 0.7 pts.mass (2(2' -hydroxy-3' , 5 ' -di-tert-butylphenyl)benzotriazol)
  • citric acid esters 0.006 pts.mass (Mixture of citric acid, citric acid monoethyl ester, citric acid dimethyl ester, citric acid triethyl ester) Particles 0.05 pts.mass
  • the remaining content of acetic acid was at most 0.1 mass%
  • the Ca content was 58 ppm
  • the Mg content was 42 ppm
  • the Fe content was 0.5 ppm
  • the free acetic acid was 40 ppm
  • the sulfuric ion content was 15 ppm.
  • the degree of acetylation at 6 th position was 0.91
  • the percentage of acetyl groups at 6 th position to the total acetyl groups was 32.5 %.
  • the acetone extract was 8 mass%, and a ratio of weight-average molecular weight to number-average molecular weight was 2.5. Further, yellow index was 1.7, haze was 0.08, and transparency was 93.5%.
  • Tg (measured by DSC) was 160 °C , and calorific value in crystallization was 6.4 J/g.
  • This cellulose triacetate is synthesized from cellulose as material obtained from cotton, and called cotton TAC in the following explanation.
  • (1-1) Preparation of Dope The dope 15 was prepared in the dope production line 30 of FIG.2.
  • the mixing tank had first and second stirrers 42, 44 and was made of stainless and 4000L in volume. Into the mixing tank, plural solvent compounds were mixed such that a mixture solvent was obtained. Note that the water content in each solvent compound is at most 0.5 mass%.
  • the stirring was made with use of the first stirrer 42 having the anchor blade and the second stirrer 44 which was eccentric stirrer of dissolver type.
  • the first stirrer 42 performed the stirring at one m/sec as circumferential velocity
  • the second stirrer 44 performed the stirring at shear rate at first 5 m/sec.
  • the dispersion was made for 30 minutes during the stirring.
  • the dissolving started at 25 0 C , and the temperature of the dispersion became 48 0 C at last.
  • the stirring of the mixture solvent was made, the cellulose triacetate flakes were added from the hopper 14 to the mixture solvent gradually, such that the total mass of the mixture solution and the cellulose triacetate flakes might be 2000kg.
  • the high speed stirring (of the second stirrer 44) was stopped, and the stirring was performed by the first stirrer 42 at 0.5 m/sec as circumferential velocity for 100 minutes.
  • the swelling liquid was fed to the heating device which is the tube with the jacket, and heated to 50 0 C , and thereafter heated under the application of pressure at 2MPa to 90 0 C . Thus the dissolving was made completely.
  • the heating time was 15 minutes .
  • the temperature of the swelling liquid is decreased to 36 0 C by the temperature controlling device 36, and then filtrated through the filtration device having filtration material whose nominal diameter was 8 ⁇ m.
  • the upstream side filtration pressure was 1.5 MPa
  • the downstream side filtration pressure was 1.2 MPa. Since the filter, the housing and the pipes were made of hastelloy alloy and had jacket for using at high temperature, they were made from materials excellent in corrosion resistance.
  • the temperature of the polymer solution in the flush tank was 25 0 C , the retaining period of the polymer solution in the flush tank was 50 minutes. Part of the polymer solution was sampled, and the measurement of the shearing viscosity was made at 25 0 C .
  • the shearing viscosity was 450Pa -s at 10 (1/s) of shearing rate.
  • the defoaming was further made by irradiating very weak ultrasonic waves .
  • the polymer solution was fed to the filtration device by the pump under the application of pressure at 1.5 MPa.
  • the polymer solution was fed at first through a sintered fiber metal filter whose nominal diameter was 10 ⁇ m, and then through the same filter of 10 ⁇ m nominal diameter.
  • the upstream pressures were respectively 1.5 MPa and 1.2 MPa, and the downstream pressures were respectively 1.0 MPa and 0.8 MPa.
  • the temperature of the polymer solution after the filtration was controlled to 36 0 C , and stored as the dope 15 in the stainless stock tank 61 whose volume was 2000L.
  • the anchor blade is provided to a center shaft of the stock tank 61, and the dope 15 was always stirred by the anchor blade at 0.3 m/se ⁇ as circumferential velocity. Note that when the concentrating of the polymer solution is made, corrosions of parts or portions contacting to the polymer solution in the devices didn't occur at all.
  • the mixture solvent A for preparing the additive liquid contained dichloromethane of 86.5 pts.mass, methanol 13 pts.mass, and 1-butanol 0.5 pts.mass.
  • the film is formed in the film production line 60 shown in FIG.l.
  • the pump 82 for increasing the upstream pressures was high accuracy gear pumps and driven to feed the dope 15 while the feed back control was made by an inverter motor .
  • the upstream pressure of high accuracy gear pump was controlled to 0.8 MPa.
  • volumetric efficiency was 99.2%, and the variation rate of the discharging was at most 0.5%.
  • the discharging pressure was 1.5MPa.
  • the width of the casting die 63 was 1.8 m, The flow rate of the dope 15 near a die lip of the casting die 63 is controlled such that the dried film may be 80 ⁇ m in thickness.
  • the casting width of the dope 15 from the die lip was 1700 mm. T Further, in order to control the temperature of the dope 15 to 36 0 C , the temperature of the heat transfer medium at an entrance of the jacket was 36 0 C.
  • the temperature of the casting die 63 and pipes was kept to 36 0 C in the film production.
  • the casting die 63 was the coat hunger type, in which heat bolts for adjusting the film thickness were disposed at the pitch of 20 mm.
  • the film thickness (or the thickness of the dopes) is automatically controlled by the heat bolt.
  • a profile of the heat volt can be set corresponding to the flow rate of the high accuracy gear pump, on the basis of the preset program.
  • the feed back control can be made by the control program on the basis of the profile of an infrared ray thickness meter (not shown) disposed in the film production line 60.
  • the control was made such that, with exception of both side edge portions (20 mm each in the widthwise direction of the produced film) , the difference of the film thickness between two positions which were 50 mm far from each other might be at most 1 ⁇ m, and the largest difference between the minimal values of the film thickness in the widthwise direction might be at most 3 ⁇ m/m. Further, the average film thickness might was controlled in ⁇ 1.5%.
  • the upstream side of the casting die 63 is provided with the decompression chamber 88.
  • the decompression rate of the decompression chamber 88 was controlled in accordance with the casting speed, such that the pressure difference might occur in the range of one Pa to 5000Pa between the upstream and downstream sides of the bead of the cast dope above the casting die.
  • the pressure difference between both side of a bead of the cast dope was determined such that the length of the bead might be from 20 mm to 50 mm.
  • an instrument was provided such that the temperature of the decompression chamber 88 might be set to be higher than the condensation temperature of the gas around the casting section.
  • labyrinth packings (not shown) in the upstream and downstream sides of the beads.
  • an opening was provided in both edges of the die lip of the casting die 63.
  • an edge suctioning device (not shown) for reducing the disturbance of the bead was provided for the casting die 63.
  • the material of the casting die 63 was the precipitation hardening stainless steel, whose coefficient of thermal expansion was at most 2 x 10 '5 ( 0 C '1 J .
  • the corrosion resistance was almost the same as that of SUS316.
  • the material to be used for the casting die 63 had enough corrosion resistance, such that the pitting (or pitting corrosion) might not occur on the gas-liquid interface even if this material were dipped in a mixture liquid of dichloromethane , methanol and water for three months.
  • the finish accuracy of the contact surface of each casting die to the dope 15 was at most 1 ⁇ m in surface roughness , straighthness in any direction was at most 1 /jm in surface roughness, and the slit clearance of the die lip was adjusted to 1.5 mm.
  • R is at most 50 ⁇ m in all of a width.
  • the shearing rate in the casting die 63 controlled in the range of one to 5000 per second.
  • the WC coating was made on the lip end from the casting die 63 by a melt extrusion method, so as to provide the hardened layer.
  • the mixture solvent A dissolvable of the solidified dope was supplied to each edge portion of the gas-liquid interface of the slit at 0.5 ml/min.
  • the pulse rate of a pump for supplying the mixture solvent was at most 5%.
  • the decompression chamber 88 was provided for decreasing the pressure in the rear side by 150 Pa.
  • a jacket (not shown) was provided, and a heat transfer medium whose temperature was controlled at 35 0 C was supplied into the jacket.
  • the edge suction rate could be controlled in the range of 1 L/min to 100 L/min, and was adequately controlled in this experiment so as to be in the range of 30 L/min to 40 L/min.
  • the belt 66 was an endless stainless belt which was 2.1m in width and 70m in length.
  • the thickness of the belt 66 was 1.5 mm, and the surface of the belt 66 was polished, such that the surface roughness might be at most 0.05 ⁇ m.
  • the material was SUS316, which had enough corrosion resistance and strength.
  • the thickness unevenness of the entire belt 66 was at most 0.5% of the predetermined value.
  • the belt 66 was moved by rotating the back-up rollers 64, 65. At this moment, the tension of the belt 66 was controlled to 1.5xlO 5 N/m 2 . Further, the relative speed to each roller to the belt 66 changed.
  • the control was made such that the difference of the relative speed between the back-up rollers 64, 65 was at most 0.01 m/min. Further the control was made such that the variation of the speed of the belt 66 was at most 0.5% to the predetermined value.
  • the position of the belt in the widthwise direction was controlled with detection of the position of the side end, such that meandering in one circle of the moving belt 66 was reduced in 1.5 mm. Further, below the casting die 63, the variation of the position in the vertical direction between the lip end of the casting die 63 and the belt 66 was in 200 ⁇ m.
  • the belt 66 is preferably incorporated in the casting chamber 84 which has air pressure controller (not shown). The three dopes (for forming the uppermost, intermittent and lower most layers) were cast onto the belt 66 from the casting die 63.
  • the back-up rollers 64, 65 were supplied therein with a heat transfer medium, such that the temperature of the belt 66 might be controlled.
  • the back-up roller 65 disposed in a side of the casting die 63 was supplied with the heat transfer medium (water) at 5°C
  • the back-up roller 64 was supplied with the heat transfer medium (water) at 4O 0 C .
  • the surface temperature of the middle portion of the belt 66 at a position just before the casting was 15 0 C
  • the temperature difference between both sides of the halt was at most 6 0 C . Note that a number of pinhole (diameter, at least
  • the temperature of the casting chamber 84 was kept to 35 0 C .
  • the drying air was fed out in parallel to the casting film 89 so as to make the drying.
  • the overall heat transfer coefficient from the drying air to the casting film 89 was 24 kcal/(m 2 - ⁇ r-°C ) .
  • the drying air at 135 0 C was fed out from the upstream air duct 90 to dry the casting film 89
  • the drying air at 14O 0 C was fed out from the downstream air duct 91 to dry the casting film 89
  • the drying air at 65°C was fed out from the lower air duct 92 to dry the casting film 89.
  • the saturation temperature of each drying air was about -8°C .
  • the oxygen concentration in the drying atmosphere on the belt 66 was kept to 5 vol% by substituting the air for nitrogen gas .
  • the inner air of the drying atmosphere was substituted by nitrogen gas.
  • the solvent vapor in the casting chamber 84 was recovered by setting the temperature of exit of the condenser 86 to -1O 0 C .
  • the air shielding plate 93 was disposed such that the drying air might not be applied to the casting film 89 and the bead directly for 5 seconds after the casting.
  • the stationary fluctuation near the casting die 63 was reduced to at most ⁇ 1 Pa.
  • the casting film 89 was peeled as polymer film 19 from the belt 66 with support of the peeling roller 95. If the sample weight of the casting film 89 was x and the sample weight after the drying was y, the solvent content on the dry basis (%) was calculated in the formula, ⁇ (x-y) /y ⁇ x 100. Note that in the content of the remaining solvent on dry basis, the weight of the solid obtained by completely drying the dope corresponds to 100%. Further, the peeling tension was IxIO 2 N/m 2 .
  • the percentage of the peeling speed (the draw of the peeling roller) to the speed of the belt 66 was controlled from 100.1% to 110% .
  • the surface temperature of the polymer film 19 was 15 0 C .
  • the drying speed on the belt 66 was 60 mass%/min in average on dry basis.
  • the solvent vapor generated in the evaporation is condensed by the condenser 86 at -10 0 C to a liquid state, and recovered by the recovering device 87.
  • the water content of the recovered solvent was adjusted to at most 0.5%.
  • the air from which the solvent components were removed was heated again and reused for the drying air.
  • the polymer film 19 was transported with the rollers in the transfer area 100 toward the tenter device 67. Note that the tension about 3ON was applied to the polymer film 19 in the lengthwise direction of the rollers in the transfer area 100. (1-8) Tenter Transportation, Drying. Edge Slitting
  • the stretch of the polymer film 19 in the widthwise direction was made with the transportation.
  • the transportation is made with chain, and the speed change of sprocket was at most 0.5% from a predetermined speed.
  • the clips for the clipping in the tenter device 67 was cooled to 20 0 C with use of a heat transfer medium.
  • the drying chamber 71 was partitioned into three zones. The temperature of the drying air in each zone was 90 0 C , 110 0 C , 120 0 C from the upstream side. The gas concentration in the drying air at -1O 0 C was the saturated gas concentration.
  • the averaged drying speed (or solvent evaporation speed) in the tenter device 67 was 120 mass% on dry basis.
  • the condition of each zone was controlled such that the content of the remaining solvent in the polymer film 19 might be 7 mass% at the exit of the tenter device 67. If the percentage of the film width before the tenter device 67 was determined to 100%, the stretching ratio of the film width after the tenter device 67 was 103%. Further, the polymer film 19 was drawn in the lengthwise direction between the peeling roller 95 and the tenter device 67. The drawing ratio in percentage was 102%.
  • the difference of the actual stretching ratio was at most 10% between positions which were at least 10 mm apart from the holding positions of the clips, and at most 5% between positions which were 20 mm apart from the holding portions.
  • the ratio of the length variation between the clip starting position and the clip releasing position was made was 90% .
  • the solvent vapor generated in the tenter device 67 was condensed at -10 0 C to a liquid state and recovered.
  • a condenser (not shown) was provided, and a temperature at an exit thereof was -8 0 C .
  • the water content in the recovered solvent was regulated to at most 0.5 mass%, and then the recovered solvent was reused.
  • the polymer film 19 was fed out as the polymer film 19 from the tenter device 67.
  • both side edge portions were slit off in the edge slitting device 70.
  • each side portion of 50 mm in the widthwise direction of the polymer film 19 was determined as the side edge portion, which were slit off by an NT type slitter of the edge slitting device 70.
  • the slit side edge portions were sent to the crusher 110 by applying air blow from a blower (not shown) , and crushed to tips about 80 mm 2 .
  • the tips were reused as raw material with the TAC frame for the dope production .
  • the oxygen concentration in the drying atmosphere in the tenter device 67 was kept to 5 vol . % .
  • the polymer film 19 was dried at high temperature in the drying chamber 71, which was partitioned into four partitions. Air blows whose temperatures were 120 0 C, 13O 0 C, 130 0 C and 130 0 C from the upstream side were fed from air blowers (not shown) to the partitions.
  • the transporting tension of each roller 111 to the polymer film 19 was 100 N/width.
  • the drying was made for ten minutes such that the content of the remaining solvent might be 0.3 mass%.
  • the lapping angle (center angle of contacting arc) of the roller 4 was 90° and 180°.
  • the rollers 111 were made of aluminum or carbon steel. On the surface, the hard chrome coating was made. The surfaces of the rollers 111 were flat or processed by blast of matting process.
  • the swing of the roller in the rotation was in 50 ⁇ m. Further, the bending of the roller 111 at the tension of 100N/width was reduced to at most 0.5 mm.
  • the solvent vapor contained in the drying air is removed with use of the adsorbing device 112 in which an adsorbing agent was used.
  • the adsorbing agent was active carbon, and the desorption was performed with use of dried nitrogen.
  • the recovered solvent was reuse as the solvent for the dope preparation after the water content might be at most 0.3 mass%.
  • the drying air contains not only the solvent vapor but also gasses of the plasticizer, UV-absorbing agent, and materials of high boiling points. Therefore, a cooler for removing by cooling and a preadsorber were used to remove them. Thus the drying air was reused.
  • the ad- and desorption condition was set such that a content of VOC (volatile organic compound) in exhaust gas might be at most 10 ppm. Furthermore, in the entire solvent vapor, the solvent content to be recovered by condensation method was 90 mass%, and almost of the remaining solvent vapor was recovered by the adsorption recovering.
  • VOC volatile organic compound
  • the polymer film 19 was transported to a first moisture controlling chamber (not shown) .
  • the drying air at 110 0 C was fed.
  • the air whose temperature was 50 0 C and dewing point was 20 0 C was fed.
  • the polymer film 19 was fed into a second moisture chamber (not shown) in which the curling of the polymer film 19 was reduced.
  • An air whose temperature was 90 0 C and humidity was 70% was applied to the polymer film 19 in the second moisture controlling chamber.
  • (1-9) Knurling, Winding- Conditions After the moisture adjustment, the polymer film 19 was cooled to 30 0 C in the cooling chamber 107, and then the edge slitting was performed.
  • the compulsory neutralization device (or a neutralization bar) 113 was provided, such that in the transportation, the charged electrostatic potential of the film might be in the range of -3kV to +3kV. Further, the film knurling was made on a surface of each side of the polymer film 19 by the knurling roller 114. The width of the knurling was 10 mm, and the knurling pressure was set such that the maximal thickness might be at most 12 ⁇ m larger in average than the averaged thickness.
  • the polymer film 19 was transported to the winding chamber 73, whose inside temperature and humidity were respectively kept to 28 0 C and 70%. Further, a compulsory neutralization device (not shown) was provided, such that the charged electrostatic potential of the film might be in the range of -1.5 kV to +1.5 kV.
  • the obtained polymer film 19 was 80 mm in thick and 1475 mm in width. The diameter of the winding shaft 115 was 169 mm.
  • the tension pattern was set such that the winding tension was 300 N/width at first, and 200 N/width at last.
  • the polymer film 19 was entirely 3940m in length.
  • the winding cycle was 400m, and the oscillation width was in ⁇ 5 mm.
  • the pressure of the press roller 116 to the winding shaft 115 was set to 50 N/width.
  • the temperature of the film at the winding was 25 0 C, the water content was 1.4 mass%, and the content of the remaining solvent was 0.3 mass%.
  • the film production was continuously made for 8760 hours. Through all processes, according to the drying speed, 20 mass% of the solvent in dry weight standard was evaporated per minute in average. Further, the loose winding and wrinkles didn ' t occur, and the film didn ' t transit in the film roll even in 1OG impact test. Further, the roll appearance was good.
  • the film roll 21 was stored under the condition at 25 0 C and 55%RH for one month. Furthermore, as result of inspecting in the same manner as above, the change having influence of the film quantity was not recognized. Furthermore there was any adhesion in the film roll 21. Further, after the polymer film 19 was produced, part of the casting film 89 didn't remain on the belt 66 after the peeling.
  • the dope 15 was sampled and stationary disposed at 30 °C . During the disposure the observation was made, and estimations thereof are four grades, A-D.
  • A Transparency and uniformity were kept even after 20 days; B: Transparency and uniformity were kept after 10 days, but white turbidity was recognized after 20 days; C : The sample was transparent and uniform at the completion of the dope production, but the gelatization and nonuniformity were recognized after one day; D: neither swelling nor dissolution was not observed, and the sample was opaque and nonuniform.
  • the surface condition of the polymer film 19 was observed with eyes, and the estimation was made as follows.
  • A The film surface was smooth; B: The film surface was smooth but some foreign materials were observed; C: Slight unevenness was observed on the film surface, and the foreign materials were clearly observed; D: Unevenness was observed on the film surface, and there are many foreign materials .
  • the polymer film 19 was cut to 64 mm x 50 mm to obtain a sample film.
  • the sample film was disposed for two hours at 23 °C and
  • a low-load tearing tester (produced by Toyo Seiki Seisakusho KK) is used to measure the weight to tear the sample film in an MD direction
  • the polymer film 19 was cut to 120 mm width by 120 mm long to obtain a sample film.
  • the sample film was disposed for two hours at 23 0 C and 65 %RH. According to the standard of ISO8776-1988, the sample was folded plural times until the sample film was broken.
  • Ig of the polymer film 19 was cut as sample film, which was folded and stored at 9O 0 C and 100% of relative humidity in a glass bottle.
  • the glass bottle was tightly closed, and the temperature was kept at 9O 0 C . After 10 days the sample was picked up, and the sensory examination of the sample film was made.
  • the polymer film 19 was cut to 35 mm width by 35 mm long to obtain sample films.
  • the sample films were disposed at 85
  • Thickness Fluctuation Measurement The thickness was measured at 600mm/min by an electric micrometer produced by Anritsu Company. The result was recorded on a chart paper at contraction scale 1/20 and chart speed 30 mm/min . Then the measurement of the chart was made with a ruler, and the half adjust of the read data was made at first decimal place .
  • Size Stabilization was represented as degree of heat shrinkage.
  • the polymer film 19 was cut to 30 mm wide by 120 mm long to obtain three sample films . In both edge portions of each sample film, holes of 6 mm ⁇ were punched at 100 mm distance. Then the sample films were disposed at 23 ⁇ 3 0 C and 65 ⁇ 5 %RH of relative humidity for 3 hours (the period may be more than 3 hour).
  • the original length of the punch distance (LIl) was measured by an automatic pin gauge (produced by Shinto Kagaku
  • the film samples were hanged in a constant-temperature oven for three hours, while the inner condition was 80 ⁇ l°C .
  • the heating treatment was made.
  • the moisture control of the sample film was made at 23 ⁇ 3 0 C and 65 ⁇ 5 %RH in a chamber for more than 3 hours , and then the length of the punch distance after the heat treatment (L12) was measured with the automatic pin gauge.
  • the degree of heat shrinkage (DHS) was calculated in the following formula:
  • the polymer film 19 was cut to 40 mm by 80 mm to obtain sample films. Then the sample films were disposed at 25 0 C and
  • HGM-2DP produced by Suga Test Instrument
  • the polymer film 19 was cut to 20 mm by 70 mm to obtain sample films. Then the sample films were disposed at 25 0 C and
  • the polymer film 19 was cut to 13 mm by 40 mm to obtain sample films. Then the sample films were disposed at 25 0 C and 60 %RH of humidity, and the permeability was measured with use of ray (wavelength, 300 nm to 400 nm) by a spectroscopic meter (U3210, produced by Hitachi, Ltd.). A wavelength inclination variation was obtained according to a formula, ⁇ (wavelength of 72% permeability) - (wavelength of 5% permeability) ⁇ . The limit wavelength was represented after the formula [ ⁇ (wavelength inclination variation) /2 ⁇ +5 ]. The absorption end was wavelength of 0.4% permeability. Further, the estimation was made at the permeability of 380 nm wavelength.
  • the polymer film 19 was cut to 70 mm by 100 mm to obtain sample films. Then the sample films were disposed at 25 0 C and 60 %RH of humidity for two hours, and the extrapolation values of the refractive index were measured according to the perpendicular direction to the sample film with use of 632.5 nm visible ray by an automatic birefringence meter (KOBRA21DH, produced by Oji Scientific Instruments). On the base of the result, the in-plane retardation was calculated from the following formula:
  • nMD and nTD were refractive indexes in the lengthwise and widthwise directions of the polymer film 19 respectively, "d” was an average thickness (nm) of the sample film.
  • the ray to be used for the measurement may have another wavelength than 632.8 nm.
  • the polymer film 19 was cut to 30 mm by 40 mm to obtain sample films. Then the sample films were disposed at 25 0 C and
  • the values of the refractive index was measured according to the perpendicular direction to the sample film, and the extrapolation values of the refractive index were measured with inclining the sample films.
  • the wavelength of the ray used for the measurement was
  • nMD refractive indexes in the lengthwise (casting), widthwise, and thickness directions of the sample film respectively
  • d was an average thickness (nm) of the sample film.
  • the polymer film 19 was cut to 70 mm by 100 mm to obtain sample films. Then the sample films were disposed at 25 0 C and 60 %RH of humidity for two hours, and the phase difference was measured according to changing an incident angle at perpendicular incident by an automatic birefringence meter (KOBRA21DH, produced by Oji Scientific Instruments).
  • KOBRA21DH automatic birefringence meter
  • the discrepancy of optical axis was measured by an automatic birefringence meter (KOBRA21DH, produced by Oji Scientific Instruments) .
  • the discrepancy angles of the optical axis were measured at 20 points positioned at a predetermined distance in a widthwise direction of the polymer film 19. Then the average of absolute values of the discrepancy angles was calculated. Note that the range of the discrepancy angles was calculated in the following manner. At first. The discrepancy angles of the optical axis were measured at 20 points positioned at a predetermined distance in a widthwise direction of the polymer film 19.
  • the polymer film 19 was cut to 15 mm by 250 mm to obtain sample films, according to ISO 1184-1983. Then the sample films were disposed at 23 0 C and 65 %RH of humidity for two hours, and the stress at beginning the stretch and an elongation value were measured by tensilon (tension tester, RTA-100, produced by Orientec Co. , LTD. ) . The data was obtained as value, supposed that the original length of the sample film would be 100 mm.
  • the polymer film 19 was cut to 100 mm by 200 mm and to 75 mm by 100 mm, to obtain sample films. Then the sample films were disposed at 23 0 C and 65 %RH of humidity for two hours, and the friction coefficient was measured by tensilon (tension tester, RTA-100, produced by Orientec Co., LTD.). For the measurement, the larger sample film was fixed on a stage, and thereafter the smaller sample film with 20Og clog was disposed on the larger sample film. The clog was drawn in a horizontal direction, during which the force at and during the moving the sample films was measured. Then coefficients of dynamic and static frictions were calculated in the following formula:
  • F was a measured value of the force
  • W was a weight of the clog.
  • the polymer film 19 was cut to 100 mm by 100 mm to obtain sample films , which was dipped in 2N-NaOH aqueous solution at 60 °C for 2 minutes to make saponification. Then the water washing of the sample film was made for 4 minutes. Thereafter, the sample film was dipped into 0.01N-HNO 3 aqueous solution at 30 0 C for 4 minutes to make neutralization. Then the water washing of the sample film was made for 4 minutes. Thereafter, the drying was made at 100 0 C for 30 minutes, and air seasoning was made for one hour. The estimation was made according to the haze value and the grades of the observation with eyes . A: Whitening was not recognized B: Whitening was slightly recognized C: Whitening was recognized so much D: Whitening was recognized extremely
  • the polymer film 19 was cut to 35 mm by 3 mm to obtain sample films. Then the sample films were disposed for 24 hours in a moisture controlling bath (HEIDON NO.YG53-168, Shinto Scientific Co. , Ltd. ) for making the curling of the film, while an atmosphere in the bath was controlled to 25 %RH, 55 %RH, 85 %RH of humidity to respective sample films. Thus the curling was made, and curvature radius was measured by a curl measuring plate. Further, for measuring the curl rate of a wet curling, the sample film was disposed in water at 25 0 C for 30 minutes, and then picked out to measure the curl value . (22) Measurement of Water Content
  • the polymer film 19 was cut to 7 mm by 35 mm to obtain sample films, whose water content was measured with drying chambers (CA-03, VA-05, both are produced by Mitsubishi Chemical Corporation) by a Karl Fischer's method. The difference of the data to the mass of the sample filmwas obtained as the water content .
  • the polymer film 19 was cut to 7 mm by 35 mm to obtain sample films , whose base content of remaining solvent was measured by gas chromatography (GC-18A, produced by Shimadzu Corporation) .
  • the polymer film was disposed at 60 0 C and 95 %RH for one day (24 hours), and thereafter the measurement of coefficient of moisture permeation was made.
  • the estimation was made to following grades:
  • Size Stabilization was represented as degree of heat shrinkage.
  • the polymer film 19 was cut to 30 mm width by 120 mm long to obtain three sample films. In both edge portions of each sample film, holes of 6 mm ⁇ were punched at 100 mm distance. Then the sample films were disposed at 23 ⁇ 3 0 C and 65 ⁇ 5 %RH of relative humidity for 3 hours (the period may be more than 3 hour) .
  • the original length of the punch distance (L15) was measured by an automatic pin gauge (produced by Shinto Kagaku KK. ), and the data was read to the minimal unit of 1/1000 mm. Then the film samples were hanged in a constant-temperature oven for three hours, while the inner condition was 80 ⁇ l°C . Thus the heating treatment was made.
  • the polymer film 19 was cut to two sample films 30 mm width by 120 mm long to obtain sample film. Then one of the sample films was disposed at 40 0 C and 95 %RH, and another one is disposed at 60 0 C and 90 %RH of relative humidity for each 24 hour period. In both edge portions of the sample film, holes of 6 mm ⁇ were punched at 100 mm distance. The original length of the punch distance (L17) was measured by an automatic pin gauge (produced by Shinto Kagaku KK.), and the data was read to the minimal unit of 1/1000 mm. Thereafter the sample film was further disposed at 9O 0 C and 5 %RH of relative humidity for 24 hours. Then, the heat treatment was made for 120 hours. The length of the punch distance (L18) was measured in the same manner as above. The dimensional change rate was calculated from ⁇ (L17-L18)/L17 ⁇ xlOO (%) (27) Inspection of Foreign Material
  • a reflective light having a size of (film width) x (one meter) was applied to the polymer film 19, and the foreign materials in the film was observed with eyes. Thereafter, the foreign materials (lint) were inspected with use of a polarization microscope.
  • Two polarizing filters were disposed in the cross-nicol configuration, such that the permeable light might be interrupted. Then a sample film was disposed between the two polarizing filters. Note that the polarizing filter was a glass protective plate. A light was discharged to one side of the polarizing plate, and a number of the bright points having 0.01 mm per 1 cm 2 of the sample film was counted from another side by an optical microscope (multitude was 50).
  • the estimation of solution stability (1) was A.
  • the estimation of surface condition (2) of the obtained polymer film 19 was A.
  • the result of tear strength test (3) was 16g.
  • the result of folding strength test was 71 times.
  • the estimation of humidity resistance and heat resistance (5) was A. All of these results and estimation was excellent.
  • the content of remaining acetic acid (6) was less than 0.01 mass%.
  • the Ca content was less than 0.05 mass%, and the Mg content was less than 0.01 mass%.
  • thickness fluctuation measurement (8) the thickness of the polymer film 19 was 80 ⁇ m ⁇ 1.5 ⁇ m.
  • Average heat shrinkage (9) was -0.1% while the sample films were disposed at 80 0 C and 90 %RH of relative humidity for 48 hours, and therefore the heat shrinkage hardly occurs in the obtained film. Further, at an exit of a tenter device, the content of remaining solvent was 7 mass% and the edge silo LEL (LEL: Lower Explosion Limit) was less than 25%, which were adequate.
  • the haze (10) was 0.3% and the permeability (11) was 92.4%.
  • the inclination variation was 19.6 nm
  • the limit wavelength was 39.27 nm
  • absorption edge was 374.1 nm
  • the absorption of 380 nm ray was 2.0%.
  • the in-plane retardation Re (13) was 1.2 nm
  • the thickness retardation Rth (14) was 48 nm.
  • the molecular orientation (15) was 1.4°
  • the discrepancy of optical axis (16) was 1° .
  • the elasticity modules (17) was 3.54 GPa in the lengthwise direction and 3.45 GPa in the widthwise direction.
  • the tensile strength (18) was 43% in the lengthwise direction and 49% in the widthwise direction.
  • the coefficient of static friction was 0.65 and that of dynamic friction was 0.51.
  • the estimation of alkaline hydrolysis test (20) was A. According to the curl value (21) , the value under 25 %RH was -0.4 and that under the wet condition was 1.7.
  • the water content (22) was 1.4 mass%, the content of remaining solvent (23) was 0.3 mass% and the coefficient of moisture permeation (24) was 1000 g/m 2 xday.
  • the heat shrinkage (25) was -0.09% in the lengthwise direction and -0.08% in the widthwise direction. Furthermore, the dimension stabilization in high humidity (26) was 0.10%. There were 5 foreign material (27) per unit that were lint. A number of the bright point recognized in 3 meter was 10 (diameter was 0.02 mm to 0.05 mm) and 5 (diameter was 0.05 mm to 0.1 mm) , and there was no bright point whose diameter was at least 0.1 mm. These result shows that the produced polymer film was excellent for optical use.
  • the adhesion after the casting didn't occur and the moisture permeability was good. Furthermore, the Rth difference of film roll was 3 nm. In the film roll, the Rth difference of teh film roll was also obtained according to a front end, a back end and a middle area in the lengthwise direction and according to both edges and a center area in the widthwise direction. Thus the effort of the data was at most 0.2%.
  • the content of remaining solvent in the polymer film 19 was measured by the gas chromatography method.
  • the coating solution for forming a hard coat layer as optical functional layer was prepared.
  • the temperature of the coating solution was controlled to 25°C, and the coating was made at the coating speed of 25 m/min with use of the gravure coater, while it is designated that the thickness L2 ( ⁇ m) of the coating layer might be 3 ⁇ m.
  • the coated film was transported for one minute in a drying chamber whose inner temperature was 100 9 C . Thus the drying of the coating solution was made to obtain the production film 23.
  • the quantity of surface plasticizer was a relative quantity.
  • the quantity of surface plasticizer is determined to 100% when the content of TTP in the film (80mm in thickness) is 12 wt. %.
  • the quantity of surface plasticizer was measured with use of FT-IR by an ATR method.
  • the coated film is cut into fragments of 10 mm x 10 nm, and a prism was contacted to the coating surface 19a to perform the measurement.
  • a peak Pl of the transmittance about 1370 cm "1 caused by TAG and a peak P2 of the transmittance about 1490 cm “1 caused by TPP are observed.
  • a ratio of the peaks (P2/P1) was calculated and the value of the ratio (P2/P1) was 0.3.
  • the measurement of the average thickness L3 ( ⁇ m) of the mixture layer 121 was made in the same manner as above description for measuring the thickness of the mixture layer 121.
  • the coated film was cut into fragments of 10 mm x 50 nm by microtome. With use 1% osmium tetroxide solution, the fragments was dyed for 24 hours. The difference of the dying concentration of the fragment was inspected with use of the scanning electron microscope.
  • the average thickness L3 ( ⁇ c ⁇ ) of the mixture layer 121 was 1 ⁇ m, and the thickness distribution was 3%. Further, also for the air side surface 19b, the measurement of the mixture layer 121 was made in the same manner.
  • the average thickness L3 ( ⁇ m) of the mixture layer 121 was 1.2 ⁇ m, and the thickness distribution was 3%.
  • the coating uniformity was inspected with eyes, and the estimation thereof was good.
  • Experiment 2 the final dry was made for 5 minutes. Other conditions were the same as Experiment 1 in the Examination 1 (hereinafter, simply Experiment 1) , such that the film roll 21 was obtained. Then the content of remaining solvent in the sample obtained from the film roll 21 was measured. Further, the production film with the hard coat layer as optical functional layer was obtained from the polymer film 19. The thickness distribution of the mixture layer 121 and the plasti ⁇ izer ratio in the coating surface 19a was calculated. Furthermore, the coating uniformity was inspected with eyes, and the estimation thereof was good.
  • Experiment 3 the conditions were the same as Experiment 1, such that the film roll 21 was obtained. Then the content of remaining solvent in the sample obtained from the film roll 21 was measured. Further, the production film with the antireflection layer as optical functional layer was obtained from the polymer film 19. The thickness distribution of the mixture layer 121 and the plasticizer ratio in the coating surface 19a was calculated. Furthermore, the coating uniformity was inspected with eyes, and the estimation thereof was good. In Experiment 4, the conditions were the same as Experiment 1, such that the film roll 21 was obtained. Then the content of remaining solvent in the sample obtained from the film roll 21 was measured. Further, the production film with the antistatic layer as optical functional layer was obtained from the polymer film 19. The thickness distribution of the mixture layer 121 and the plasticizer ratio in the coating surface 19a was calculated. Furthermore, the coating uniformity was inspected with eyes, and the estimation thereof was good.
  • Experiment 5 the final dry was made for 3 minutes. Other conditions were the same as Experiment 1, such that the film roll 21 was obtained. Then the content of remaining solvent in the sample obtained from the film roll 21 was measured. Further, the production film with the hard coat layer as optical functional layer was obtained from the polymer film 19. The thickness distribution of the mixture layer 121 and the plasticizer ratio in the coating surface 19a was calculated. Furthermore, the coating uniformity was inspected with eyes, and the estimation thereof was bad.
  • Experiment 7 the conditions were the same as Experiment 5, such that the film roll 21 was obtained. Then the content of remaining solvent in the sample obtained from the film roll 21 was measured. Further, the production film with the antireflection layer as optical functional layer was obtained from the polymer film 19. The thickness distribution of the mixture layer 121 and the plasticizer ratio in the coating surface 19a was calculated. Furthermore, the coating uniformity was inspected with eyes, and the estimation thereof was bad.
  • PR plasicizer ratio (P2/P1) in coating surface 12a
  • the production film 23 as antireflection film was produced from the polymer film 19 obtained in Experiment 1 of examination 2.
  • 125g of a mixture (DPHA, Japan Chamical Co. , LTD) of dipentaelithlitolpetaacrylate and dipentaelithlitolhexa acrylate was dissolved to a mixture solvent of methylethylketone and cyclohexanone at 439g in ratio 50:50 in weight percent.
  • a mixture solution was obtained.
  • optical polymer initialyzer Irgacure 907, Chiba Gaigy Japan
  • photosensitizer (KAYACURE DETX, produced by NIPPON KAYAKU CO. , LTD. ) at 3.Og were dissolved to methylethylketone at 49g, which were added to the mixture solution.
  • the refractive index of the coating layer was 1.60.
  • To the solution was added 1Og of cross-liked polystyrene particles (averaged diameter, 2 ⁇ m; trade name, SX-200H, produced by Soken Chemical & Engineering Co., Ltd.), and the mixture was stirred at 5000 rpm by a high speed disperser for one hour, so as to make a dispersion. Thereafter, the filtration was made with a polypropylene filter whose porous diameter was 30 ⁇ m. Thus the coating solution A for forming the antiglare layer was obtained.
  • the refractive index of the coating layer was 1.60.
  • Dezolite Z-7526 Produced by JSR Co., LTD
  • a solution was obtained and coated to form a coating layer by UV curing.
  • the refractive index of the coating layer was 1.53.
  • the filtration of the solution was made with a polypropylene filter whose porous diameter was 30 ⁇ m.
  • the coating solution D for forming the hard coat layer was obtained.
  • the coating solution D was dried in 120 °C for five minutes, and hardened in illumination of air cooling metal halide lamp having power of 160 W/cm (Eyegraphics Co., LTD) to form a hard coat layer 131 (see, FIG.5) of 2.5 ⁇ m in thickness.
  • the coating solution A was coated by a bar coater.
  • the drying and the UV curing were made in the same manner as the hard coat layer so as to form an antiglare layer 132 (see, FIG.5) of 1.5 ⁇ m in thickness.
  • the coating solution F was coated by a bar coater. The drying was made at first at 80°C, and then at 120°C for 10 minutes so as to form a low reflective layer 133 (see, FIG.5) of 0.096 ⁇ m in thickness.
  • an antireflection film B (corresponding to an antireflection film 130 in FIG.5) was obtained.
  • the obtained antireflection film 130 includes the hard coat layer 131, the antiglare layer 132 and the low reflective index layer 133 which were sequentially superimposed on the polymer film 19.
  • the thickness L4 ( ⁇ m) of the polymer film 19 was 80 ⁇ m
  • the thickness L5 ( ⁇ m) of the hard coat layer 131 was 2.5 ⁇ m
  • the thickness L6 ( ⁇ m) of the antiglare layer 132 was 1.5 ⁇ m
  • the thickness L7 ( ⁇ m) of the low reflective layer was 0.096 ⁇ m.
  • the solvent compounds (methylethylketone and cyclohexanone (sometimes called anone) ) of the coating solution D for the hard coat layer penetrates toward the coating surface 19a of the polymer film 19, and the components (mainly TAC) of the polymer film 19 was swollen or dissolved to form a mixture layer 134.
  • the mixture layer 134 extends to part of the hard coat layer 131, and about 1 ⁇ m in thickness.
  • the thickness L4 of the polymer film 19 is in the range of 40 ⁇ m to 100 / ⁇ m, it is preferable that the thickness L5 of the hard coat layer 131 is in the range of 1 ⁇ m to 8 ⁇ m, the thickness L6 of the antiglare layer 132 is in the range of 1 ⁇ m to 5 ⁇ m, and the thickness L7 of the low reflective index layer 133 is in the range of 0.01 ⁇ m to 8 ⁇ m.
  • the averaged thickness L8 ( ⁇ m) of the mixture layer 134 is preferably in the range of 0.1 ⁇ m to 10.0 ⁇ m, particularly in the range of 0.1 ⁇ m to 7 ⁇ m, and especially in the range of 0.1 ⁇ m to 3 ⁇ m. Further, the thickness distribution of the mixture layer 134 is preferably in ⁇ 10% to the averaged thickness L8 , particularly in ⁇ 7%, and especially in ⁇ 3%. In this case, it is preferable that the thickness distribution of the mixture layer 134 is in the above range, also according to the front and back end of the polymer film 19 in each film roll 21. Further, it is preferable that thickness distribution of the mixture layer 134 is in the above range also among the different film roll 21.
  • the coating solution B was used to form the antiglare layer, and thus the antireflection film B was obtained.
  • the coating solution C was used to form the antiglare layer, and thus the antireflection film C was obtained.
  • the coating solutions A-C were coated on the films obtained in Experiment 2 of Examination 2 , so as to produce the antireflection films A' -C, respectively. (Estimation of Antireflection Film) The estimations of the antireflection films A-C, A' -C were made according to the follows. The results thereof will be shown in Table 2.
  • Specular Reflectance (SF) & Coloring A spectrophotometer V-550 (produced by JASCO Corporation) was provided with an adapter ARV-474 to measure the specular reflectance at an exiting angle of -5° according to the incident light of wavelength in the range of 380 nm to 780 nm at the incident angle of 5° . Then the average of the specular reflectance of the reflection whose wave length was in the range of 450 nm to 650 nm was calculated to evaluate antiglare property.
  • the L* value, the a*value and the b*value in CIE 1976 L*a*b* color space was calculated from the data of measured reflection spectrum while the CIE 1976 L*value, a*value, b*value color space represents color of direct reflection of an incident light at incident angle of 5° from a CIE standard light source D65. Thus the color of the reflection was estimated.
  • a spectrophotometer V-550 (produced by JASCO Corporation) was provided with an adapter ILV-471 to measure the integrated reflectance at the incident angle of 5° of the incident light of wavelength in the range of 380 nm to 780 nm. Then the average of the integrated reflectance of the reflection whose wavelength was in the range of 450 nm to 650 nm was calculated.
  • a haze meter model 100IDP (produced by Nippon Denshoku Industries Co., Ltd.) was used for measuring the haze of the obtained antireflection films .
  • the pencil hardness represents a grade of scratch resistance.
  • the estimations of pencil hardness were made as described in JIS-K-5400. After the antiglare and antireflection film was set in atmosphere with the temperature of 25 0 C and the humidity of 60%RH for two hours, the front surface of the antiglare and antireflection film was scratched with 3H test pencils determined in JIS-S-6006. Thereby a force of 1 kg was applied to the test pencil. This test was made five times. The evaluation of the pencil hardness was "A” (Excellent) , when no scratch remains on the front surface in the five tests. The evaluation of the pencil hardness was "B” (Good) , when one or two scratches remains on the front surface in the five tests. The evaluation was "R" (Reject) when more than three scratches remain on the front surface in the five tests.
  • the contact angle represents a grade of stainproofness, especially finger printing stainproofness. After the antiglare and antireflection film was set in the atmosphere with the temperature of 25 °C and the humidity of 60%RH for two hours, the contact angle to pure water on the antireflection film was measured.
  • the coefficient of dynamic friction represents the grade of the smoothness of the front surface, of the antiglare and antireflection film.
  • the estimation of antiglare property was "A” (Excellent) when no outline of the illumination lamp was observed.
  • the estimation was “B” (Good) when the outline was slightly recognized.
  • the estimation was “C” (Good) when the outline was not clear but recognized.
  • the estimation was "R” (Reject) when the outline was almost clear.
  • Table 2 shows that the antireflection film with a film base of the polymer film 19 of the present invention is excellent in the optical properties. Especially, the antireflection film is excellent in the antiglare properties and the antireflection properties and the coloring is weak, which causes the good results in the film properties (such as pensile hardness, properties for staining finger print, coefficient of dynamic friction and the like) according the polymer film of the present invention.
  • the polarizing filter with antiglare and antireflection properties was produced from the antireflection film having the antiglare layer A in Example 1 of experiment 3.
  • the polarizing filter was used for producing a liquid crystal display, in which the antireflection layer was disposed as a surface layer.
  • a contrast was excellent since no silhouette of light from the outside was not formed on the liquid crystal display, and the antiglare properties reduces the reflection image on the liquid crystal display.
  • the visibility was excellent and the staining of the finger print was reduced.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Moulding By Coating Moulds (AREA)

Abstract

La présente invention concerne un film optique faisant l’objet d’une dissolution de TAC et de TPP dans un mélange de solvant dont le solvant principal est le dichlorométhane, de sorte à préparer un additif. Un film polymère (19) est obtenu à partir de l’additif au moyen d’un procédé de coulée de solution. Une solution de revêtement contenant des matériaux à fonctions optiques est préparée. La solution de revêtement est appliquée au film polymère (19) pour former une couche à fonctions optiques (120). Un film optique (23) est ainsi obtenu. Le solvant de la solution de revêtement pénètre à travers une surface de revêtement (19a) dans le film polymère (19). Le TAC gonfle ou se dissout alors, de sorte qu’une couche de mélange (121) se forme en continu dans le film polymère et la couche à fonctions optiques (120). Une épaisseur moyenne L3 ( µm) de la couche de mélange (121) est comprise entre 0,1 µm et 10 µm, ce qui permet d’obtenir des fonctions optiques quasi uniformes.
PCT/JP2006/306391 2005-03-25 2006-03-22 Film optique WO2006101251A1 (fr)

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WO2014183145A1 (fr) * 2013-05-15 2014-11-20 Berndorf Band Gmbh Procédé de fabrication d'une feuille ou d'un film
US9989675B2 (en) 2013-09-30 2018-06-05 Fujifilm Corporation Polarizing plate and image display device
EP3421525A1 (fr) * 2017-06-26 2019-01-02 Essilor International Procédés de préparation de films optiques fonctionnels
US11414534B2 (en) 2015-02-27 2022-08-16 Island Polymer Industries Gmbh Multifunctional optically highly transparent films and method for their production

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TWI448372B (zh) * 2009-12-30 2014-08-11 Polarizing film protective film manufacturing device

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JP2002182004A (ja) * 2000-12-14 2002-06-26 Fuji Photo Film Co Ltd 反射防止フィルム、偏光板および液晶表示装置
JP2003227932A (ja) * 2002-02-04 2003-08-15 Fuji Photo Film Co Ltd 偏光板用保護フィルムの製造方法、偏光板、および画像表示装置
JP2005062594A (ja) * 2003-08-18 2005-03-10 Konica Minolta Opto Inc 光学フィルム、光学フィルムの製造方法、及びそれを用いた偏光板、表示装置

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CN100398584C (zh) * 2002-10-18 2008-07-02 富士胶片株式会社 过滤和生产聚合物溶液的方法和制备溶剂的方法
JP4390247B2 (ja) * 2003-04-25 2009-12-24 富士フイルム株式会社 溶液製膜方法

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JP2002182004A (ja) * 2000-12-14 2002-06-26 Fuji Photo Film Co Ltd 反射防止フィルム、偏光板および液晶表示装置
JP2003227932A (ja) * 2002-02-04 2003-08-15 Fuji Photo Film Co Ltd 偏光板用保護フィルムの製造方法、偏光板、および画像表示装置
JP2005062594A (ja) * 2003-08-18 2005-03-10 Konica Minolta Opto Inc 光学フィルム、光学フィルムの製造方法、及びそれを用いた偏光板、表示装置

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014183145A1 (fr) * 2013-05-15 2014-11-20 Berndorf Band Gmbh Procédé de fabrication d'une feuille ou d'un film
JP2016519314A (ja) * 2013-05-15 2016-06-30 ベルンドルフ バント ゲゼルシャフト ミット ベシュレンクテル ハフツング フォイル又はフィルムを製造するための方法
US10183422B2 (en) 2013-05-15 2019-01-22 Berndorf Band Gmbh Method for producing a foil or a film
US9989675B2 (en) 2013-09-30 2018-06-05 Fujifilm Corporation Polarizing plate and image display device
US11414534B2 (en) 2015-02-27 2022-08-16 Island Polymer Industries Gmbh Multifunctional optically highly transparent films and method for their production
EP3421525A1 (fr) * 2017-06-26 2019-01-02 Essilor International Procédés de préparation de films optiques fonctionnels
WO2019002220A1 (fr) * 2017-06-26 2019-01-03 Essilor International Procédés de préparation de films optiques fonctionnels
CN110770286A (zh) * 2017-06-26 2020-02-07 依视路国际公司 用于制备功能性光学膜的方法
CN110770286B (zh) * 2017-06-26 2023-01-03 依视路国际公司 用于制备功能性光学膜的方法
US11648742B2 (en) 2017-06-26 2023-05-16 Essilor International Methods for preparing functional optical films

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