WO2010100917A1 - 薄型高機能偏光膜およびその製造方法 - Google Patents
薄型高機能偏光膜およびその製造方法 Download PDFInfo
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- WO2010100917A1 WO2010100917A1 PCT/JP2010/001460 JP2010001460W WO2010100917A1 WO 2010100917 A1 WO2010100917 A1 WO 2010100917A1 JP 2010001460 W JP2010001460 W JP 2010001460W WO 2010100917 A1 WO2010100917 A1 WO 2010100917A1
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- film
- resin
- polyvinyl alcohol
- polarizing film
- resin layer
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
- G02B5/3025—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state
- G02B5/3033—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
- Y10T428/263—Coating layer not in excess of 5 mils thick or equivalent
- Y10T428/264—Up to 3 mils
- Y10T428/265—1 mil or less
Definitions
- the present invention relates to a thin high-performance polarizing film formed by dyeing and stretching a polyvinyl alcohol resin layer coated and dried on a resin substrate integrally with the resin substrate, and a method for producing the same.
- a manufacturing method of a so-called polarizer (hereinafter referred to as “polarizing film”) in which a dichroic substance is adsorbed and oriented by dyeing on a polyvinyl alcohol resin (hereinafter referred to as “PVA resin”) layer is well known. Yes.
- polarizing film a so-called polarizer (hereinafter referred to as “polarizing film”) in which a dichroic substance is adsorbed and oriented by dyeing on a polyvinyl alcohol resin (hereinafter referred to as “PVA resin”) layer
- PVA resin polyvinyl alcohol resin
- a method of producing a thin polarizing film in which a stretcher is used and stretched in a dry manner, and then a dichroic substance is adsorbed and oriented by dyeing, or a laminate including a thin PVA resin layer A method of manufacturing a thin polarizing film in which a dichroic material is oriented by adsorbing the dichroic material by dyeing and then stretching it by a dry method using a stretching machine in a heating apparatus is shown in the comparative example of FIG. As shown, it is already known.
- a polarizing film used for a liquid crystal display element bonded to the front and back of a liquid crystal cell is generally dyed by applying a single layer of a PVA resin of 60 to 80 ⁇ m to, for example, a roll transporter having a plurality of sets of rolls having different peripheral speeds.
- the polarizing film is sensitive to changes in temperature and humidity, and easily expands and contracts. Therefore, a polarizing film in which protective films are bonded to both sides is usually used so as to suppress expansion and contraction and to reduce the influence of temperature and humidity. Still, when a thick polarizing film is used, it is difficult to suppress the expansion and contraction of the polarizing film, causing stress on the member when bonded to a member such as a liquid crystal cell, and causing display unevenness on the liquid crystal display element. This is one of the technical problems of the thick polarizing film. Furthermore, it goes without saying that there are technical issues that should meet the demands of the times for thinning and low energy consumption.
- a thin polarizing film has been demanded instead of a thick polarizing film.
- a thin PVA-based resin monolayer for example, a PVA-based resin film having a thickness of 50 ⁇ m or less is applied to, for example, a roll transporter, from room temperature to around 60 ° C.
- a wet method such as an aqueous solution
- the thin PVA-based resin film dissolves or breaks without being able to withstand the tension applied to the film. That is, it is difficult to stably produce a thin polarizing film from a thin PVA resin film.
- optical characteristics of a polarizing film that can be used for a large display element can be simply represented by a degree of polarization P and a single transmittance T.
- the performance of the polarizing film is generally represented by a TP graph in which two optical characteristic values of a polarization degree P and a single transmittance T which are in a trade-off relationship are plotted.
- the transmittance decreases for the amount of reflection, so the maximum T value that can be practically achieved is about 45 to 46%.
- the degree of polarization P can represent the contrast ratio (CR) of the polarizing film or display.
- the polarization degree P of 99.95% corresponds to 2000: 1 in the CR of the polarizing film, and corresponds to 1050: 1 in the CR of the display when used in a commercially available liquid crystal television cell.
- the larger the CR the better the display contrast and the easier it is to see.
- the CR of the polarizing film is a value obtained by dividing the parallel transmittance by the orthogonal transmittance, as will be described later.
- the CR of the display is a value obtained by dividing the maximum luminance by the minimum luminance.
- the minimum luminance is the luminance at the time of black display, and is required to be 0.5 cd / m 2 or less in a liquid crystal television set assuming a general viewing environment. If the value exceeds this value, the color reproducibility deteriorates.
- the maximum luminance is the luminance at the time of white display, and is used in the range of 450 to 550 cd / m 2 in a liquid crystal television assuming a general viewing environment. Below this, the visibility decreases.
- a CR of 1000: 1 or more is generally required for a liquid crystal television.
- the polarizing film requires a CR of 2000: 1 or more. This corresponds to a polarization degree P of 99.95% or more.
- a polarizing film for a liquid crystal television generally has a single transmittance T of 42.0% or more.
- the single transmittance T of the polarizing film is less than 42.0%, the luminance L of the display is lowered.
- the display luminance L must be increased by increasing the luminance of the light source itself. .
- JP 2001-343521 A Japanese Patent No. 4279944 Japanese Patent Laid-Open No. 51-069644
- An object of the present invention is to provide a thin polarizing film having high optical characteristics, a so-called thin high-performance polarizing film, and a method for producing the same.
- the present inventors have found that all of the conventional production methods must be stretched dry using a stretching machine in a heating device such as an oven. Focused on. Since the crystallization of the resin base material and the PVA-based resin layer formed on the resin base material is stretched by a dry method, it is difficult to stretch the laminate itself to 5 times or more of the original length. This crystallization phenomenon is the same in the case of manufacturing a thick polarizing film obtained by stretching a single layer body by a dry method. Due to the crystallization of the PVA-based resin layer and the limit of the draw ratio, the dichroic material cannot be sufficiently oriented. This was the first technical problem.
- PVA-based resin is a hydrophilic polymer composition and is easily dissolved in water.
- the inventors of the present invention describe how to insolubilize a thin PVA-based resin layer in an aqueous solution, how to orient the dichroic material adsorbed by stretching at a high magnification, and, as a result, how to obtain optical characteristics. Sought to realize a thin and highly polarizing film.
- the inventors of the present invention applied a thin PVA resin layer formed on a resin substrate by applying and drying an aqueous solution of a PVA resin in a boric acid aqueous solution at a low temperature (65 ° C. or less). It has been found that the film can be stretched at a magnification (5 times or more). More specifically, in a low-temperature (65 ° C. or lower) aqueous boric acid solution, a thin PVA-based resin layer formed on a resin base material is insolubilized by a crosslinking action, and the thin PVA-based resin layer thus insolubilized is resin-based. This means that the material can be stretched integrally with the material at a magnification of 5 times or more.
- a thin PVA-based resin layer can be stretched at a high magnification integrally with the resin base material even in a boric acid aqueous solution lower than the glass transition temperature of the resin base material itself due to the action of water molecules as a plasticizer. It is to gain knowledge. As a result, as shown in Examples 1 and 2 of FIG. 4 or FIG. 5, a large display element in which the dichroic substance is sufficiently adsorbed and oriented by high-stretching with suppressed crystallization of the PVA resin. It has been found that a thin polarizing film having high optical properties that can be used for the above, a so-called thin high-performance polarizing film can be obtained. Processes and operations used in the thin high-performance polarizing film and the manufacturing method thereof will be described below.
- the PVA resin layer can be insolubilized, so that it can be stretched at a high magnification of 5 times or more.
- the relationship between the glass transition temperature and the stretching temperature is the same for the PVA resin layer.
- a typical PVA resin has a glass transition temperature of about 80 ° C., and in the case of dry stretching, it is difficult to stretch uniformly at a lower temperature than this temperature at a high magnification. Further, in the case of dry stretching regardless of temperature, crystallization of the PVA resin proceeds by stretching, and it is difficult to make the total stretch ratio including the resin base material to be stretched 5 times or more of the original length.
- a high-order structure large structure that does not contribute to orientation, such as a lamellar structure or spherulite, is formed in the PVA-based resin, so that the dichroic substance can be sufficiently adsorbed and oriented in a higher order. Inferred to be impossible.
- the present inventors consider that this is a cause of low optical characteristics of the thin polarizing film produced by the conventional manufacturing method.
- a thin PVA resin formed on a resin substrate is stretched in a boric acid aqueous solution at 65 ° C. or lower.
- the resin substrate is a composition having a glass transition temperature of 65 ° C. or higher, and is preferably a resin substrate made of an amorphous ester-based or olefin-based thermoplastic resin. Even if the glass transition temperature of the resin substrate is 65 ° C. or higher, the resin substrate can be stretched even if it is 65 ° C. or lower due to the function of a water molecule as a plasticizer. Water molecules also function as plasticizers for PVA resins. Therefore, a thin PVA resin integrally with the resin base material can be stretched in a boric acid aqueous solution at 65 ° C. or lower.
- the thin PVA resin can be stretched at a high magnification of 5 times or more while preventing the crystallization of the PVA resin.
- the result leads to the inference that the orientation of the amorphous part of the thin PVA resin will increase.
- dichroic substances such as polyiodine ion complexes existing in the PVA-based resin are arranged in one direction in a high order.
- a thin polarizing film with high optical properties a so-called thin high-performance polarizing film is obtained.
- Embodiments of the present invention are as follows.
- a first aspect of the present invention is a thin high-performance polarizing film having a thickness of 7 ⁇ m or less and made of a PVA-based resin oriented with a dichroic material, which is integrally formed on a resin base material.
- a thin high-performance polarizing film having optical characteristics of 42.0% or more and a degree of polarization of 99.95% or more. See the table in FIG.
- the present inventors have made it possible to reduce the thickness of the display element, eliminate display unevenness, and reduce the energy consumption.
- the resin base material is an ester-based or olefin-based thermoplastic resin having a water absorption rate of 0.50% or more and a glass transition temperature in the range of 25 ° C to 85 ° C.
- An amorphous polyethylene terephthalate film of an ester resin film (amorphous polyethylene terephthalate film, A-PET film).
- a resin base material is transparent resin.
- the dichroic substance adsorbed and oriented on the thin high-functional polarizing film may be iodine, an organic dye, or a mixture thereof.
- a second aspect of the present invention is a thin high-performance polarizing film having a thickness of 7 ⁇ m or less and made of a PVA resin in which a dichroic material is oriented on a resin base material, and has a single transmittance of 42.0% or more.
- the present invention relates to a method for producing a thin high-performance polarizing film having an optical characteristic with a polarization degree of 99.95% or more. Specifically, first, a step of generating a PVA resin layer by applying and drying a PVA resin aqueous solution on a resin substrate having a thickness of at least 20 ⁇ m is included.
- the resin base material in the present invention is an ester-based or olefin-based thermoplastic resin having a water absorption rate of 0.50% or more and a glass transition temperature in the range of 25 ° C to 85 ° C.
- a transparent resin is preferable when an optical functional film that protects one surface of a thin high-performance polarizing film is used.
- the dichroic substance may be iodine, an organic dye, or a mixture thereof.
- the dichroic substance is adsorbed in the PVA resin layer by being immersed in an aqueous solution of 0.1 wt% or more and 4.5 wt% or less for 5 to 60 seconds.
- iodine it is more preferable to further add iodide, since dissolution of iodine can be promoted and dyeing efficiency can be further improved.
- the influence of the hydrophilic PVA resin dissolved in the aqueous solution is not a problem in the production of the thick polarizing film, but the technical problem cannot be ignored in the production of the thin polarizing film.
- the problem is prevention of elution of the PVA resin into the aqueous solution during dyeing. If the dyeing process is performed for a short time, there is no problem. Therefore, it is effective for the present inventors to insolubilize the PVA resin layer in advance before immersing the PVA resin layer produced on the resin base material in the staining solution. It was found that the PVA resin layer can be insolubilized by immersing it in an aqueous boric acid solution at room temperature.
- the method includes a step of stretching the PVA resin layer on which the dichroic substance is adsorbed integrally with the resin base material in an aqueous boric acid solution.
- the PVA-based resin layer that becomes thin during stretching dissolves, so that the total stretching ratio of the PVA-based resin layer is 5 times or more of the original length, that is, 5 of the original length of the PVA-based resin layer. It is difficult to stretch to more than double the length.
- a boric acid aqueous solution capable of simultaneously effecting crosslinking and insolubilization with boric acid, the PVA-based resin layer adsorbed with the dichroic substance could be stretched at a high magnification to enhance the alignment performance.
- the resin base material is made of a PVA resin in which a dichroic substance is oriented, the thickness is 7 ⁇ m or less, the single transmittance is 42.0% or more, and the polarization is changed.
- a thin high-performance polarizing film having an optical property of a degree of 99.95% or more can be formed.
- Another resin film is laminated on the surface of the thin high-performance polarizing film manufactured integrally with the resin base material via an adhesive on the surface not formed on the resin base material.
- the thin high-performance polarizing film may be transferred to another resin film by peeling.
- an optical functional film for the transferred resin film the optical functional film can be formed on one side of the manufactured thin high-functional polarizing film.
- a thin high-performance polarizing film having optical functional films formed on both sides can be manufactured.
- the third aspect of the present invention relates to a method for producing a laminate film including a thin high-functional polarizing film in which a dichroic material is oriented. Specifically, it is made of a PVA-based resin layer in which a dichroic material is oriented, has a thickness of 7 ⁇ m or less, a single transmittance of 42.0% or more, and a thin and high optical property having a polarization degree of 99.95% or more.
- the present invention relates to a method for producing a laminate film in which a functional polarizing film is formed on one surface of a resin substrate, and includes the following steps.
- the resin base material in the present invention is also an ester-based or olefin-based thermoplastic having a water absorption of 0.50% or more and a glass transition temperature in the range of 25 ° C to 85 ° C.
- a transparent resin is preferable.
- a PVA resin layer contained in a laminate film by immersing a laminate film containing a resin substrate and a PVA resin layer formed on one side of the resin substrate in a staining solution containing a dichroic substance. And a step of adsorbing the dichroic substance.
- the dichroic material may be iodine, an organic dye, or a mixture thereof.
- the staining solution as in the second embodiment, the dichroic substance is adsorbed in the PVA resin layer by immersing it in an aqueous solution of 0.1 wt% or more and 4.5 wt% or less for 5 to 60 seconds.
- iodine When iodine is used as the dichroic substance, it is more preferable to further add iodide, since dissolution of iodine can be promoted and dyeing efficiency can be further improved. Moreover, before immersing the PVA-type resin layer contained in a laminated body film in the dyeing liquid containing a dichroic substance, by previously immersing a laminated body film in normal temperature boric acid aqueous solution, It is more preferable to perform insolubilization treatment.
- the method includes a step of stretching the laminate film including the PVA resin layer on which the dichroic substance is adsorbed in a boric acid aqueous solution.
- the PVA-based resin layer that becomes thin with the resin base material is melted during stretching, so that the PVA-based resin layer contained in the laminate film has a total stretching ratio. It is difficult to stretch to a length of 5 times or more of the original length, that is, to a length of 5 times or more of the original length of the PVA resin layer.
- the PVA resin layer adsorbing the dichroic substance is stretched at a high magnification integrally with the resin base material.
- the orientation performance of the chromatic substance could be improved.
- a resin base that can be stretched at a high magnification even at a temperature lower than the glass transition temperature of the resin substrate itself contained in the laminate film. It is more preferable to stretch the laminate film in a boric acid aqueous solution at a low temperature of 65 ° C. or lower by selecting a material.
- a thickness of 7 ⁇ m or less and a single transmittance of 42.0% are formed of a PVA-based resin layer in which a dichroic substance is oriented on one side of a resin base material.
- a laminate film is produced in which a thin high-performance polarizing film having optical properties with a polarization degree of 99.95% or more is formed.
- the manufactured laminate film including a thin high-performance polarizing film made of a PVA-based resin in which a dichroic material is oriented is changed to an iodide salt having a temperature lower than the glass transition temperature of the resin substrate contained in the laminate film.
- the optical functional film is formed on both sides by the step of laminating the optical functional film on the other side of the thin high-performance polarizing film formed on one side of the resin base film contained in the dried laminate film. It is also possible to manufacture a thin high-functional polarizing film in which is formed. Alternatively, another resin film is laminated on the surface of the thin laminated high-performance polarizing film that is not formed on the resin base material via an adhesive, and at the same time, the resin base material is made thin and highly functional. By peeling from the polarizing film, the thin high-functional polarizing film can be produced by transferring the thin high-functional polarizing film to another resin film and forming an optical functional film composed of the resin film transferred on one side.
- Schematic of the manufacturing process of the thin high-performance polarizing film of the present invention Schematic diagram of manufacturing process of manufacturing method of the present invention and manufacturing method including dry stretching Comparison table of optical characteristic values of Examples and Comparative Examples Table of T / P values of Examples and Comparative Examples TP graph based on each T / P value of Example and Comparative Example Schematic diagram of TP graph
- the manufacture of the thin high-performance polarizing film 10 will be described based on Example 1.
- an amorphous polyethylene terephthalate film having a glass transition temperature of 80 ° C. is used as the resin base material 11.
- the resin base material 11 can support one surface of the thin high-performance polarizing film 10.
- the thickness of the resin substrate 11 before being stretched is preferably in the range of 20 ⁇ m to 500 ⁇ m.
- the resin base 11 may be made of a hydrophobic resin that is insoluble in water and does not swell in order to prevent staining with the dichroic substance 14 '.
- a resin that does not have a dissociating group such as a carboxyl group, a sulfonic acid group, or a quaternary amino group, or a nonionic hydrophilic group such as a hydroxyl group or an amide group in the molecular structure.
- a dissociating group such as a carboxyl group, a sulfonic acid group, or a quaternary amino group, or a nonionic hydrophilic group such as a hydroxyl group or an amide group in the molecular structure.
- Resin substrate 11 is, for example, an ester resin film or an olefin resin film, and preferably an amorphous polyethylene terephthalate film.
- a crystallized polyethylene terephthalate film generally has a high elastic modulus, and is difficult to stretch at low temperatures.
- the amorphous polyethylene terephthalate film can be stretched even at a low temperature.
- These surfaces may be subjected to surface modification treatment including corona treatment in order to improve adhesion with the PVA resin layer 12.
- An adhesive layer may be provided.
- the water absorption rate (JIS K 7209) of the resin base material 11 is preferably 0.3% or more, and more preferably 0.5% or more.
- the glass transition temperature (JIS K 7121 DSC method) of the resin base material is preferably 85 ° C. or lower, more preferably 25 ° C. to 85 ° C.
- a resin film having such physical properties can be stretched at a high magnification even in a boric acid aqueous solution at 65 ° C. or lower.
- the laminated body film 13 which consists of the resin base material 11 and the PVA-type resin layer 12 is produced by a process (A).
- Preparation process (A) prepares the film roll which consists of the resin base material 11 whose thickness is 100 micrometers first. Next, an aqueous solution of 3 to 10 parts by weight of a PVA resin is prepared with respect to 100 parts by weight of the solvent.
- the PVA-based resin layer having a thickness of 10 ⁇ m is prepared by drawing out the resin substrate 11 from the film roll, applying an aqueous solution of the PVA-based resin on the resin substrate, and drying in an oven at 60 ° C. 12 is formed on the resin substrate 11. You may make it wind up the continuous web of the laminated body film 13 produced in this way.
- the laminate film 13 is then processed in the following continuous process.
- the dyeing process (B). This is a step of immersing the laminate film 13 in the dyeing solution 14 and adsorbing the dichroic material 14 ′ to the PVA resin layer 12.
- a solvent for the staining solution 14 water is generally used.
- the dichroic substance 14 ′ is usually used at a ratio of 0.1 to 4.3 parts by weight (0.1 to 4.5 wt%) with respect to 100 parts by weight of the solvent mainly composed of water.
- Examples of the dichroic substance 14 ′ include iodine, organic dyes, a mixture thereof, and the like. One kind of these dichroic substances may be used, or two or more kinds may be used in combination.
- Iodide is preferably used in a proportion of 0.02 to 20 parts by weight, more preferably 0.1 to 10 parts by weight with respect to 100 parts by weight of the solvent.
- Specific examples of iodide include potassium iodide, lithium iodide, sodium iodide, zinc iodide, aluminum iodide, lead iodide, copper iodide, barium iodide, calcium iodide, tin iodide, and iodide.
- examples include titanium.
- the immersion time in the staining solution 14 is not particularly limited, but is usually about 5 seconds to 5 minutes.
- the temperature of the staining solution 14 is usually about 20 to 50 ° C.
- the laminate film 13 was immersed in a dyeing solution 14 containing iodine and potassium iodide having a liquid temperature of 30 ° C. for 30 seconds.
- iodine was adsorbed on the PVA-based layer 12.
- the iodine content of the dyeing solution 14 was 0.1 parts by weight with respect to 100 parts by weight of water, and the potassium iodide content was 0.7 parts by weight with respect to 100 parts by weight of water.
- the cross-linking step (C) is a step of cross-linking the PVA resin layer 12 in which the laminate film 13 is immersed in the boric acid aqueous solution 15 and the dichroic substance 14 'is adsorbed.
- This crosslinking step (C) is also an insolubilization step for preventing the swollen PVA resin from being dissolved in water.
- the boric acid aqueous solution 15 is obtained by dissolving boric acid or borate in water as a solvent.
- boron compounds such as borax, glyoxal, glutaraldehyde and the like can be used.
- the boric acid concentration is usually 1 to 10 parts by weight per 100 parts by weight of water.
- the concentration of iodide is preferably 0.05 to 15% by weight, more preferably 0.5 to 8% by weight. Specific examples of iodide are the same as those in the dyeing step (A).
- the immersion time in the boric acid aqueous solution 16 is not particularly limited, but is usually about 15 seconds to 5 minutes.
- the temperature of the boric acid aqueous solution 15 is usually about 20 to 70 ° C.
- the PVA-based resin layer 12 on which iodine is adsorbed is cross-linked in a boric acid aqueous solution 15 containing potassium iodide having a liquid temperature of 60 ° C., and a resin base is formed by a roll stretching machine 16 having a plurality of sets of rolls having different peripheral speeds.
- the material 11 was stretched integrally. This is the stretching step (D) integrated with the crosslinking step (C).
- the laminate film 13 was stretched up to a stretch ratio of 5.0 times in the longitudinal axis.
- the boric acid content of the boric acid aqueous solution 15 at this time was 4 parts by weight with respect to 100 parts by weight of water, and the potassium iodide content was 5 parts by weight with respect to 100 parts by weight of water.
- the temperature of the boric acid aqueous solution 15 is preferably 85 ° C. or lower. If the temperature exceeds 85 ° C., elution of iodine adsorbed on the PVA-based resin is likely to proceed, and the PVA-based resin may also be eluted, so that the optical characteristics of the thin high-performance polarizing film 10 to be manufactured are deteriorated. Moreover, when the thickness of the PVA-type resin layer 12 is thin, the PVA-type resin layer 12 will melt
- the temperature of the boric acid aqueous solution 15 is more preferably 30 ° C. to 65 ° C.
- the resin base material 11 and the PVA-based resin layer 12 cannot be sufficiently softened because the function as a plasticizer for water is not sufficiently exhibited. It is difficult to stretch the total stretching ratio of the body film 13 to 5 times or more of the original length.
- the draw ratio of the laminate film stretched in the boric acid aqueous solution 15 is preferably 5 times or more, more preferably 5.5 times or more of the original length of the laminate film 13.
- the draw ratio is less than 5 times, the dichroic material 14 'is not sufficiently oriented, and the optical characteristics of the obtained thin high-performance polarizing film 10 are lowered.
- the “stretch ratio” refers to a stretch ratio in the process when the stretching process is one stage. When a plurality of stretching machines are provided in an aqueous solution and stretched in multiple stages, the total stretching ratio (total stretching ratio) in each step is referred to.
- the cross-linking step using the boric acid aqueous solution can be provided in the pre-step of the dyeing step (B).
- This crosslinking step (E) is not necessary in the production of a thick polarizing film because dissolution of the PVA resin does not cause a problem.
- the dissolution of the PVA resin in the dyeing solution 14 is a problem that cannot be ignored. . Therefore, providing the crosslinking step (E) before the dyeing step (B) is effective in the production of a thin high-functional polarizing film having high optical characteristics.
- a crosslinking step (F) with an aqueous boric acid solution may be separately provided in the pre-step of the stretching step (D) in the aqueous boric acid solution from the viewpoint of reinforcing boric acid that has been lost during the dyeing step.
- the laminate film 13 stretched 5.0 times was taken out from the boric acid aqueous solution 15 and then sent to the cleaning step (G).
- the washing step (G) is a step of washing away unnecessary residues of the laminate film including the thin high-functional polarizing film 10 that has been subjected to various treatments. If this treatment is insufficient, boric acid may be deposited from the thin high-functional polarizing film 10 after the laminate film is dried.
- the cleaning is performed in a cleaning solution containing potassium iodide so that the PVA resin does not dissolve.
- the concentration of potassium iodide in the cleaning liquid is about 0.5 to 10% by weight.
- the temperature of the cleaning liquid is about 10 to 50 ° C.
- the immersion time is usually about 1 second to 1 minute.
- the final process is a drying process (H).
- Arbitrary appropriate methods for example, natural drying, ventilation drying, and heat drying, are employable as a drying process (H).
- Example 1 was dried with warm air of 60 ° C. for 30 seconds.
- the thickness of the PVA resin layer 12 stretched integrally with the resin base material 11 included in the finished laminate film was 3 ⁇ m.
- a thin high-performance polarizing film 10 made of PVA resin having a thickness of 3 ⁇ m and oriented with iodine was formed on the resin substrate 11. This is the thin high-performance polarizing film 10 of Example 1 whose characteristics are shown in the table of FIG.
- the laminate film in which the thin high-performance polarizing film 10 is formed on the resin base material 11 is further peeled off from the thin high-performance polarizing film 10 by the transfer step (I) shown in FIG.
- the thin high-functional polarizing film 10 may be transferred to another optical functional film.
- the PVA resin used in the present invention can be obtained by saponifying a polyvinyl acetate resin.
- the saponification degree is usually 85 to 100 mol%, and the polymerization degree is 1,000 to 10,000.
- This PVA resin is polyvinyl alcohol or ethylene-vinyl alcohol copolymer.
- the manufactured thin high-functional polarizing film 10 preferably exhibits absorption dichroism at any wavelength in the visible light region (wavelength 380 nm to 780 nm).
- the thickness is 7 ⁇ m or less, preferably 0.5 ⁇ m to 5 ⁇ m. Since this thin high-performance polarizing film 10 has a small shrinkage stress, it has excellent dimensional stability even in a high temperature environment, and exhibits optical characteristics with a single transmittance of 42.0% or more and a degree of polarization of 99.95% or more.
- Example 1 As the resin substrate, an amorphous polyethylene terephthalate film (Novaclear manufactured by Mitsubishi Plastics) having a glass transition temperature of 80 ° C. was used.
- the laminated body film containing the resin base material and the polyvinyl alcohol layer was produced as follows. First, a resin base material having a thickness of 100 ⁇ m was prepared. Next, an aqueous solution of polyvinyl alcohol (NH26 manufactured by Nippon Synthetic Chemical Co., Ltd.) was applied onto the resin substrate, and a polyvinyl alcohol layer having a thickness of 10 ⁇ m was formed while drying at a temperature of 60 ° C.
- polyvinyl alcohol NH26 manufactured by Nippon Synthetic Chemical Co., Ltd.
- the produced laminate film was immersed in a staining solution containing iodine and potassium iodide at a liquid temperature of 30 ° C. for an arbitrary time so that the final transmittance of the polarizing film was 40 to 44%.
- iodine was adsorbed on the polyvinyl alcohol layer.
- the iodine content of the dyeing solution was 0.1 parts by weight with respect to 100 parts by weight of water, and the potassium iodide content was 0.7 parts by weight with respect to 100 parts by weight of water.
- a boric acid aqueous solution containing boric acid and potassium iodide having a liquid temperature of 60 ° C. a laminate film containing a polyvinyl alcohol layer in which iodine is adsorbed on a resin base material is passed between a plurality of sets of rolls having different peripheral speeds. The laminate film was stretched until just before it was broken uniaxially. The draw ratio (maximum draw ratio) at this time was 5.0 times.
- the boric acid content of the boric acid aqueous solution was 4 parts by weight with respect to 100 parts by weight of water, and the potassium iodide content was 5 parts by weight with respect to 100 parts by weight of water.
- the “immediately before breaking” and the “maximum draw ratio” are determined after confirming the draw ratio at which breakage occurs in advance. Specifically, it means stretching at a magnification that is about 0.2 times lower than the broken stretching ratio confirmed in advance.
- the laminate film stretched 5.0 times was taken out of the boric acid aqueous solution and then dried with hot air at 60 ° C.
- the thickness of the polyvinyl alcohol layer stretched integrally with the resin substrate was 3 ⁇ m. In this way, a 3 ⁇ m-thick polyvinyl alcohol resin layer in which iodine was oriented was formed on the resin substrate.
- Example 2 A polymethylpentene film (TPI, manufactured by Mitsui Chemicals) having a glass transition temperature of 30 ° C. was used as the resin substrate.
- Example 2 is a boric acid aqueous solution containing boric acid and potassium iodide at a liquid temperature of 60 ° C. in the same manner as in Example 1 except that a laminate film containing a polyvinyl alcohol layer having iodine adsorbed on a resin base material is used.
- the laminate film was stretched through a plurality of sets of rolls having different peripheral speeds until just before breaking in a longitudinal uniaxial manner. The draw ratio (maximum draw ratio) at that time was 5.5 times.
- Example 1 As the resin substrate, an amorphous polyethylene terephthalate film (Novaclear manufactured by Mitsubishi Plastics) having a glass transition temperature of 80 ° C. was used. In the same manner as in Example 1, a laminate film was produced in which a polyvinyl alcohol resin layer having a thickness of 10 ⁇ m was formed on a resin substrate having a thickness of 100 ⁇ m. Next, in the oven at 110 ° C., the produced laminate film was stretched until immediately before breaking in a longitudinal uniaxial direction. The draw ratio (maximum draw ratio) at that time was 4.0 times.
- the term “immediately before breaking” and “maximum stretching ratio” as used herein mean stretching at a ratio lower by about 0.2 times than the fractured stretching ratio confirmed in advance, as in the case of Example 1.
- the stretched laminated film was immersed in the dyeing solution in the same manner as in Example 1 for an arbitrary time so that the final transmittance of the polarizing film was 40 to 44%.
- the laminate film taken out from the staining solution was dried with hot air at 60 ° C.
- the thickness of the polyvinyl alcohol resin layer stretched integrally with the resin base material was 4 ⁇ m. In this way, a 4 ⁇ m-thick polyvinyl alcohol resin layer in which iodine was oriented was formed on the resin substrate.
- Example 2 A laminate film in which a polyvinyl alcohol resin layer having a thickness of 10 ⁇ m was formed on a resin substrate having a thickness of 100 ⁇ m was produced in the same manner as in Example 1.
- the produced laminate film was immersed in the staining solution in the same manner as in Example 1 for an arbitrary time so that the final transmittance of the polarizing film was 40 to 44%.
- the laminate film taken out from the staining solution was dried with hot air at 60 ° C. Next, in a 90 ° C. oven, the laminate film on which iodine was adsorbed was stretched until immediately before it was broken uniaxially.
- the draw ratio (maximum draw ratio) at that time was 4.5 times.
- the term “immediately before breaking” and “maximum stretching ratio” as used herein mean stretching at a ratio that is approximately 0.2 times lower than the fractured stretching ratio confirmed in advance, as in the case of Example 1.
- the thickness of the polyvinyl alcohol layer stretched integrally with the resin base material was 4 ⁇ m. In this way, a 4 ⁇ m-thick polyvinyl alcohol resin layer in which iodine was oriented was formed on the resin substrate.
- Polarization degree P (%) ⁇ (Tp ⁇ Tc) / (Tp + Tc) ⁇ 1/2 ⁇ 100
- the contrast ratio (CR) of the polarizing film was obtained from the following equation.
- CR Tp / Tc
- the contrast ratio (CR) of the display was obtained from the following equation.
- CR maximum brightness / minimum brightness
Abstract
Description
薄型高機能偏光膜およびその製造方法に用いられる工程および作用について、以下、説明する。
厚みが十数μm以下の薄いPVA系樹脂フィルムを水溶液中で高倍率に延伸するためには、厚みが20μm以上の樹脂基材に形成されていたとしても、PVA系樹脂フィルム自体に延伸時にかかる張力に耐え、延伸中に水に溶解しない耐水性が付与されていなければならない。すなわち不溶化されたPVA系樹脂フィルムでなければならない。
H3BO3+H2O ←→ H++[B(OH)4]-
このテトラヒドロキシホウ酸アニオンは、ビニルアルコール系ポリマーのヒドロキシ基と水素結合し、ビニルアルコール系ポリマーを架橋させると推察される。
この架橋状態として化学式(1)のような状態が推定モデルの一つとして考えられる(化学式(1)の点線のボンドが架橋結合)。この架橋により、ビニルアルコール系ポリマーが不溶化する。
図2の比較例1および2に提示される、樹脂基材と一体に薄いPVA系樹脂を乾式で延伸する従来製法によっては、例えば単体透過率が42.0%以上で偏光度が99.95%以上の光学特性を有する薄型偏光膜を得ることは難しい。その要因は、「乾式延伸」といわれる延伸方法を用いていることに起因する。乾式延伸は、延伸対象の樹脂基材のガラス転移温度より低い温度で延伸することが難しい。通常は延伸対象の樹脂基材が破断する。それを延伸できたとしても均一延伸にはならない。そのため、乾式延伸は、一般的に延伸対象の樹脂基材のガラス転移温度より高い温度で延伸することになる。65℃以下の低温で延伸する場合には、必然的に、ガラス転移温度が65℃以下の延伸対象の樹脂基材が選択されることになる。
薄型高機能偏光膜10の製造は、実施例1に基づき説明することとする。図1に示すように、樹脂基材11は、例えば、ガラス転移温度が80℃の非晶質ポリエチレンテレフタレートフィルムを用いる。樹脂基材11は、薄型高機能偏光膜10の片面を支持することができる。延伸される前の樹脂基材11の厚みは、好ましくは20μm~500μmの範囲にあればよい。樹脂基材11は、二色性物質14’による染色を防ぐため、水に不溶で、かつ、膨潤しない疎水性樹脂を用いるようにしてもよい。具体的には、分子構造中にカルボキシル基、スルホン酸基、第4アミノ基などの解離基や、水酸基、アミド基のような非イオン性の親水基を有しない樹脂をいう。
樹脂基材は、ガラス転移温度が80℃の非晶質ポリエチレンテレフタレートフィルム(三菱樹脂社製ノバクリアー)を用いた。樹脂基材とポリビニルアルコール層とを含む積層体フィルムは以下のように作製した。まず、厚みが100μmの樹脂基材を準備した。次に、その樹脂基材上にポリビニルアルコール(日本合成化学社製NH26)の水溶液を塗布して、60℃の温度で乾燥しながら、厚みが10μmのポリビニルアルコール層を製膜した。
樹脂基材はガラス転移温度が30℃のポリメチルペンテンフィルム(三井化学社製TPX、)を用いた。実施例2は、実施例1と同様の方法で、樹脂基材にヨウ素を吸着させたポリビニルアルコール層を含む積層体フィルムを、液温が60℃のホウ酸およびヨウ化カリウムを含むホウ酸水溶液中で、周速の異なる複数セットのロール間を通して、その積層体フィルムを縦一軸に破断する直前まで延伸した。そのときの延伸倍率(最大延伸倍率)は5.5倍であった。
樹脂基材は、ガラス転移温度が80℃の非晶質ポリエチレンテレフタレートフィルム(三菱樹脂社製ノバクリアー)を用いた。実施例1と同様の方法で、厚みが100μmの樹脂基材上に厚みが10μmのポリビニルアルコール樹脂層を製膜した積層体フィルムを作製した。次に110℃のオーブン内で、作製された積層体フィルムを縦一軸に破断する直前まで延伸した。そのときの延伸倍率(最大延伸倍率)は4.0倍であった。ここでいう「破断する直前」および「最大延伸倍率」は、実施例1の場合と同様に、事前に確認した破断した延伸倍率よりも0.2倍程度低い倍率の延伸を意味する。
厚みが100μmの樹脂基材上に厚みが10μmのポリビニルアルコール樹脂層を製膜した積層体フィルムを、実施例1と同様に、作製した。作製された積層体フィルムを実施例1と同様に染色液に、最終的な偏光膜の単体透過率が40~44%となるように任意の時間、浸漬した。染色液から取り出した積層体フィルムを60℃の温風で乾燥した。次に90℃のオーブン内で、ヨウ素を吸着させた積層体フィルムを縦一軸に破断する直前まで延伸した。そのときの延伸倍率(最大延伸倍率)は4.5倍であった。ここでいう「破断する直前」および「最大延伸倍率」は、実施例1の場合と同様に、事前に確認した破断した延伸倍率よりも0.2倍程度低い倍率の延伸を意味する。
[厚みの測定]
樹脂基材および薄型偏光膜の厚みは、デジタルマイクロメーター(アンリツ社製KC-351C)を用いて測定した。
[透過率および偏光度の測定]
薄型偏光膜の単体透過率T、平行透過率Tp、直交透過率Tcは、紫外可視分光光度計(日本分光社製V7100)を用いて測定した。これらの透過率T、Tp、Tcは、JIS Z 8701の2度視野(C光源)により測定して視感度補正を行なったY値である。
偏光度Pを上記の透過率を用い、次式により求めた。
偏光度P(%)={(Tp-Tc)/(Tp+Tc)}1/2×100
偏光膜のコントラスト比(CR)は、次式により求めた。
CR=Tp/Tc
ディスプレイのコントラスト比(CR)は、次式により求めた。
CR=最大輝度/最小輝度
11 樹脂基材
12 PVA系樹脂層
13 積層体フィルム
14 二色性物質14’を含む染色液
15 ホウ酸水溶液
16 周速の異なる複数セットのロールを有するロール延伸機
(A) 樹脂基材とPVA樹脂層を含む積層体フィルムの作製工程
(B) 染色工程
(C) 架橋工程
(D) 延伸工程
(E) 染色工程前の架橋工程
(F) 延伸工程(D)前の架橋工程
(G) 洗浄工程
(H) 乾燥工程
(I) 転写工程
Claims (24)
- 樹脂基材に一体に製膜される、二色性物質を配向させたポリビニルアルコール系樹脂からなる厚みが7μm以下の薄型高機能偏光膜であって、単体透過率が42.0%以上および偏光度が99.95%以上の光学特性を有することを特徴とする薄型高機能偏光膜。
- 樹脂基材が透明基材であることを特徴とする請求項1に記載の薄型高機能偏光膜。
- 二色性物質が、ヨウ素、有機染料又はそれらの混合物であることを特徴とする請求項1又は請求項2のいずれかに記載の薄型高機能偏光膜。
- 少なくとも20μmの厚みを有する樹脂基材に、ポリビニルアルコール系樹脂の塗布および乾燥によってポリビニルアルコール系樹脂層を生成し、生成されたポリビニルアルコール系樹脂層を二色性物質の染色液に浸漬して、ポリビニルアルコール系樹脂層に二色性物質を吸着させ、二色性物質を吸着させたポリビニルアルコール系樹脂層を、ホウ酸水溶液中において、樹脂基材と一体に総延伸倍率が元長の5倍以上となるように延伸することによって、樹脂基材に、二色性物質を配向させたポリビニルアルコール系樹脂からなる厚みが7μm以下の薄型高機能偏光膜であって、単体透過率が42.0%以上かつ偏光度が99.95%以上の光学特性を有する薄型高機能偏光膜を製造するようにしたことを特徴とする方法。
- 樹脂基材に生成されたポリビニルアルコール系樹脂層を二色性物質の染色液に浸漬するときに、予め、ポリビニルアルコール系樹脂層を不溶化しておくことを特徴とする請求項4に記載の方法。
- ホウ酸水溶液に浸漬することによって、ポリビニルアルコール系樹脂層を不溶化するようにしたことを特徴とする請求項5に記載の方法。
- ポリビニルアルコール系樹脂層を0.1wt%以上4.5wt%以下の二色性物質を含む染色液に5秒から60秒間、浸漬することによって、二色性物質を吸着させるようにしたことを特徴とする請求項4から請求項6のいずれかに記載の方法。
- 65℃以下のホウ酸水溶液において、二色性物質を吸着させたポリビニルアルコール系樹脂層を樹脂基材と一体に延伸するようにしたことを特徴とする請求項4から請求項7のいずれかに記載の方法。
- 樹脂基材のガラス転移温度より低い温度のホウ酸水溶液において、二色性物質を吸着させたポリビニルアルコール系樹脂層を樹脂基材と一体に延伸するようにしたことを特徴とする請求項4から請求項8のいずれかに記載の方法。
- 樹脂基材に生成されたポリビニルアルコール系樹脂層を浸漬するためのヨウ素からなる二色性物質を含む染色液およびヨウ素を二色性物質として吸着させたポリビニルアルコール系樹脂層を樹脂基材と一体に延伸するためのホウ酸水溶液のいずれにもヨウ化物塩をさらに含むことを特徴とする請求項4から請求項9のいずれかに記載の方法。
- 樹脂基材として透明基材を用いることによって、片面に透明基材からなる光学機能フィルムを形成するようにしたことを特徴とする請求項4から請求項10のいずれかに記載の方法。
- 薄型高機能偏光膜の樹脂基材には製膜されていない面に接着剤を介して他の樹脂膜を積層すると同時に、樹脂基材を薄型高機能偏光膜から剥離することによって、薄型高機能偏光膜を他の樹脂膜に転写し、片面に転写された樹脂膜からなる光学機能フィルムを形成するようにしたことを特徴とする請求項4から請求項11のいずれかに記載の方法。
- 片面に光学機能フィルムが形成された薄型高機能偏光膜の他面に接着剤を介して第2光学機能フィルムを積層することによって、両面に光学機能フィルムを形成するようしたことを特徴とする請求項11又は請求項12に記載の方法。
- 二色性物質を配向させた薄型高機能偏光膜を含む積層体フィルムを製造する方法であって、
少なくとも20μmの厚みを有する樹脂基材と、樹脂基材の片面にポリビニルアルコール系樹脂を含む水溶液を塗布および乾燥することによって形成されたポリビニルアルコール系樹脂層とを含む積層体フィルムを生成する工程と、
樹脂基材と樹脂基材の片面に形成されたポリビニルアルコール系樹脂層とを含む前記積層体フィルムを、二色性物質を含む染色液中に浸漬することによって、積層体フィルムに含まれるポリビニルアルコール系樹脂層に二色性物質を吸着させる工程と、
二色性物質を吸着させたポリビニルアルコール系樹脂層を含む前記積層体フィルムを、ホウ酸水溶液中において、総延伸倍率が元長の5倍以上となるように延伸する工程と、
二色性物質を吸着させたポリビニルアルコール系樹脂層が樹脂基材と一体に延伸されたことにより、樹脂基材の片面に、二色性物質を配向させたポリビニルアルコール系樹脂層からなる、厚みが7μm以下、単体透過率が42.0%以上かつ偏光度が99.95%以上の光学特性を有する薄型高機能偏光膜を製膜させた積層体フィルムを製造する工程と
を含むことを特徴とする方法。 - 樹脂基材と樹脂基材の片面に形成されたポリビニルアルコール系樹脂層とを含む積層体フィルムを染色液に浸漬する前に、積層体フィルムに含まれるポリビニルアルコール系樹脂層を不溶化する工程をさらに含むことを特徴とする請求項14に記載の方法。
- ホウ酸水溶液中に浸漬することによって、積層体フィルムに含まれるポリビニルアルコール系樹脂層を不溶化するようにしたことを特徴とする請求項15に記載の方法。
- 積層体フィルムに含まれる二色性物質を吸着させたポリビニルアルコール系樹脂層を、積層体フィルムに含まれる樹脂基材のガラス転移温度より低い温度のホウ酸水溶液中において、積層体フィルムと一体に延伸するようにしたことを特徴とする請求項14から請求項16のいずれかに記載の方法。
- 積層体フィルムに含まれる樹脂基材として透明樹脂を用いるようにしたことを特徴とする請求項14から請求項17のいずれかに記載の方法。
- 0.1wt%以上4.5wt%以下の二色性物質を含む染色液に積層体フィルムを5秒から60秒間、浸漬することによって、積層体フィルムに含まれるポリビニルアルコール系樹脂層に二色性物質を吸着させるようにしたことを特徴とする請求項14から請求項18のいずれかに記載の方法。
- 樹脂基材に生成されたポリビニルアルコール系樹脂層を含む積層体フィルムを浸漬するためのヨウ素からなる二色性物質を含む染色液およびヨウ素を二色性物質として吸着させたポリビニルアルコール系樹脂層を積層体フィルムと一体に延伸するためのホウ酸水溶液のいずれにもヨウ化物塩をさらに含むことを特徴とする請求項14から請求項19のいずれかに記載の方法。
- 二色性物質を配向させたポリビニルアルコール系樹脂からなる薄型高機能偏光膜を含む前記積層体フィルムを、積層体フィルムに含まれる樹脂基材のガラス転移温度より低い温度のヨウ化物塩を含む水溶液で洗浄する工程をさらに含むことを特徴とする請求項14から請求項20のいずれかに記載の方法。
- 洗浄された積層体フィルムを50℃以上100℃以下の温度で乾燥する工程をさらに含む請求項21に記載の方法。
- 乾燥された積層体フィルムに含まれる延伸された樹脂基材フィルムの片面に製膜された薄型高機能偏光膜の他面に接着剤を介して光学機能フィルムを積層する工程をさらに含む請求項22に記載の方法。
- 乾燥された積層体フィルムに含まれる、薄型高機能偏光膜の樹脂基材に製膜されていない面に接着剤を介して他の樹脂膜を積層すると同時に、樹脂基材を薄型高機能偏光膜から剥離することによって、薄型高機能偏光膜を他の樹脂膜に転写し、片面に転写された樹脂膜からなる光学機能フィルムを形成する工程をさらに含むことを特徴とする請求項23に記載の偏光子膜の製造方法。
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KR1020117021936A KR101175700B1 (ko) | 2009-03-05 | 2010-03-03 | 박형 고기능 편광막의 제조방법 |
EP10748516.1A EP2405288B1 (en) | 2009-03-05 | 2010-03-03 | Highly functional thin polarizing film and process for producing same |
CN2010800199157A CN102326105B (zh) | 2009-03-05 | 2010-03-03 | 薄型高功能偏振膜及其制造方法 |
US13/225,347 US8404066B2 (en) | 2009-03-05 | 2011-09-02 | Thin high-performance polarizing film and method for manufacturing the same |
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EP2405288B1 (en) | 2016-03-02 |
EP2405288A1 (en) | 2012-01-11 |
US20120327512A1 (en) | 2012-12-27 |
EP2518542A1 (en) | 2012-10-31 |
JP4751486B2 (ja) | 2011-08-17 |
TWI382210B (zh) | 2013-01-11 |
CN102736165A (zh) | 2012-10-17 |
TWI431343B (zh) | 2014-03-21 |
KR20110118825A (ko) | 2011-11-01 |
US9645292B2 (en) | 2017-05-09 |
TW201245781A (en) | 2012-11-16 |
US8404066B2 (en) | 2013-03-26 |
JPWO2010100917A1 (ja) | 2012-09-06 |
TW201044033A (en) | 2010-12-16 |
CN102326105B (zh) | 2013-06-05 |
CN102326105A (zh) | 2012-01-18 |
CN102736165B (zh) | 2016-08-10 |
EP2405288A4 (en) | 2012-08-29 |
KR101175700B1 (ko) | 2012-08-21 |
US20110315306A1 (en) | 2011-12-29 |
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