CN117741850A - Method for manufacturing polarizing plate with anti-reflection layer - Google Patents
Method for manufacturing polarizing plate with anti-reflection layer Download PDFInfo
- Publication number
- CN117741850A CN117741850A CN202311223268.7A CN202311223268A CN117741850A CN 117741850 A CN117741850 A CN 117741850A CN 202311223268 A CN202311223268 A CN 202311223268A CN 117741850 A CN117741850 A CN 117741850A
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- CN
- China
- Prior art keywords
- film
- layer
- antireflection layer
- protective film
- polarizing plate
- Prior art date
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- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- BYMUNNMMXKDFEZ-UHFFFAOYSA-K trifluorolanthanum Chemical compound F[La](F)F BYMUNNMMXKDFEZ-UHFFFAOYSA-K 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 239000004034 viscosity adjusting agent Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C55/00—Shaping by stretching, e.g. drawing through a die; Apparatus therefor
- B29C55/02—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets
- B29C55/04—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets uniaxial, e.g. oblique
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/02—Physical, chemical or physicochemical properties
- B32B7/023—Optical properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/11—Anti-reflection coatings
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors
- G02F1/133528—Polarisers
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K59/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic light-emitting element covered by group H10K50/00
- H10K59/80—Constructional details
- H10K59/8793—Arrangements for polarized light emission
Landscapes
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Nonlinear Science (AREA)
- Chemical & Material Sciences (AREA)
- Mathematical Physics (AREA)
- Mechanical Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Polarising Elements (AREA)
- Surface Treatment Of Optical Elements (AREA)
- Electroluminescent Light Sources (AREA)
- Adhesive Tapes (AREA)
- Devices For Indicating Variable Information By Combining Individual Elements (AREA)
Abstract
Provided is a method for manufacturing a polarizing plate with an antireflection layer, which can maintain the uniformity of the reflection characteristics. The manufacturing method includes a step Sa and a step Sb. In step Sa, an antireflection layer formed of at least 2 films is formed on one main surface side of a film base material (10). In the step Sb, at least 1 layer constituting the antireflection layer is formed, and then the layer is irradiated with visible light to detect the reflected light. The film base material (10) has, in order, a 1 st protective film (11), a 1 st adhesive layer (12), a polarizing element (13), a 2 nd adhesive layer (14), and a 2 nd protective film (15). From the two ends of the polarizer (13) in the width direction to the part (P)The distance (D) between the 1 st protective film (11) and the 2 nd protective film (15) in at least one part 1 ) The distance (D) between the 1 st protective film (11) and the 2 nd protective film (15) is smaller than that between the portions sandwiching the widthwise ends of the polarizer (13) 2 ) Narrow.
Description
Technical Field
The present invention relates to a method for manufacturing a polarizing plate with an antireflection layer.
Background
An antireflection film is disposed on the recognition side of an image display device such as a liquid crystal display or an organic EL display in order to prevent degradation of image quality due to reflection of external light, improve contrast, and the like. The antireflection film includes an antireflection layer formed of a laminate of a plurality of films having different refractive indices on a film base material.
One embodiment of the antireflection film is a polarizing plate with an antireflection layer (a polarizing film with an antireflection layer). The polarizing plate with the antireflection layer is formed by a method of attaching an antireflection film to the surface of the polarizing plate and a method of attaching an antireflection film as a protective film to the surface of the polarizing element. In addition, a method of forming a polarizing plate with an antireflection layer by forming an antireflection layer on the polarizing plate is also known (for example, patent document 1).
Prior art literature
Patent literature
Patent document 1: japanese patent laid-open No. 2014-34701
Disclosure of Invention
Problems to be solved by the invention
The anti-reflection layer reduces the reflectivity of visible light by utilizing the multi-reflection interference of the thin film. Therefore, when the refractive index and the film thickness of the thin film change, the reflected light characteristics such as the reflectance and the hue of the reflected light change. In the formation of the antireflection layer, even when film formation conditions of the thin film are strictly controlled and kept constant, there are cases where variations in film thickness, refractive index, and the like of the thin film occur due to variations in characteristics of raw materials, temporal variations in film formation environment, and the like.
In the production of a thin film, an on-line measurement is performed in a production process, and the measurement result is fed back to a preceding process, thereby maintaining the quality of the thin film constant. For example, in patent document 1, as an in-line inspection in a process of manufacturing a polarizing plate with an antireflection layer, reflected light characteristics are measured in-line, and the measurement result is fed back to film forming conditions of a thin film.
However, in the technique described in patent document 1, there is room for improvement in maintaining the reflection characteristics of the polarizing plate with the antireflection layer uniform.
The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a method for manufacturing a polarizing plate with an antireflection layer, which can maintain the uniformity of the reflected light characteristics.
Solution for solving the problem
< embodiment of the invention >
The present invention includes the following embodiments.
[1] A method for manufacturing a polarizing plate with an antireflection layer, the polarizing plate with an antireflection layer having a film base material and an antireflection layer provided on one main surface side of the film base material, the method comprising:
a step Sa of forming the antireflection layer formed of at least 2 films on the one main surface side of the film base material, and
a step Sb of irradiating at least one layer constituting the antireflection layer with visible light after the layer is formed, and detecting the reflected light,
the step Sa and the step Sb are continuously performed while the film base material is conveyed in one direction,
the film base material is a laminate having a 1 st protective film, a 1 st adhesive layer, a polarizing element, a 2 nd adhesive layer, and a 2 nd protective film in this order,
The 1 st protective film and the polarizer are bonded by the 1 st adhesive layer,
the 2 nd protective film and the polarizer are bonded by the 2 nd adhesive layer,
the 1 st protective film and the 2 nd protective film are each larger than the width of the polarizing member and protrude from both ends in the width direction of the polarizing member,
the 1 st protective film and the 2 nd protective film are spaced apart at least in a part of the portions protruding from the both ends more than the 1 st protective film and the 2 nd protective film in a portion sandwiching the widthwise end portions of the polarizing member.
[2] The method for producing a polarizing plate with an antireflection layer according to item [1], wherein in step Sb, after all the layers constituting the antireflection layer are formed, the antireflection layer is irradiated with visible light, and the reflected light is detected.
[3] The method for producing a polarizing plate with an antireflection layer according to the above [1] or [2], wherein the film formation condition of the antireflection layer in the step Sa is adjusted according to the detection result of the reflected light in the step Sb.
[4] The method for producing a polarizing plate with an antireflection layer according to any one of [1] to [3], wherein in the step Sb, a plurality of portions in the width direction of the layer are irradiated with visible light, and the reflected light is detected.
[5] The method for producing a polarizing plate with an antireflection layer according to any one of [1] to [4], wherein in the step Sa, the antireflection layer is formed by a sputtering method.
[6] The method for producing a polarizing plate with an antireflection layer according to any one of [1] to [5], wherein the film base material further comprises a 3 rd adhesive layer for adhering the 1 st protective film and the 2 nd protective film to each other in at least a part of a portion extending from the both ends in a width direction.
[7] The method for producing a polarizing plate with an antireflection layer according to any one of [1] to [6], wherein the 2 nd protective film comprises a transparent film and a hard coat layer provided on one principal surface side of the transparent film,
in the step Sa, the antireflection layer is formed on the hard coat layer on the opposite side of the transparent film side.
[8] The method for producing a polarizing plate with an antireflection layer according to any one of the above [1] to [7], wherein the film base material further comprises an adhesive layer provided on the opposite side of the 1 st protective film to the polarizer side,
in the step Sa, the antireflection layer is formed on the side of the 2 nd protective film opposite to the polarizer side.
[9] The method for producing a polarizing plate with an antireflection layer according to item [8], wherein the film base material further comprises a release liner temporarily bonded to the adhesive layer on the side opposite to the 1 st protective film side.
[10] The method for producing a polarizing plate with an antireflection layer according to any one of the above [1] to [9], wherein a step Sc of forming a primer layer on the one principal surface side of the film base material is further provided before the step Sa,
in the step Sa, the antireflection layer is formed on the main surface of the primer layer on the opposite side of the film base material side.
ADVANTAGEOUS EFFECTS OF INVENTION
According to the present invention, a method for manufacturing a polarizing plate with an antireflection layer, which can maintain the uniformity of the reflected light characteristics, can be provided.
Drawings
FIG. 1 is a cross-sectional view showing an example of a film base material.
Fig. 2 is a cross-sectional view showing another example of the film base material.
Fig. 3 is a cross-sectional view showing another example of the film base material.
Fig. 4 is a schematic diagram showing an example of an antireflection layer deposition apparatus.
A, B and C of fig. 5 are sectional views divided by steps showing an example of a method for producing a polarizing plate with an antireflection layer according to the present invention.
Fig. 6 is a graph showing the hue of the reflected light from the antireflection layer before adjustment of the film formation conditions in the example.
Fig. 7 is a graph showing the hue of the reflected light from the antireflection layer after the film formation conditions in the example were adjusted.
Fig. 8 is a graph showing the hue of the reflected light from the antireflection layer before adjustment of the film formation conditions in the comparative example.
Fig. 9 is a graph showing the hue of the reflected light from the antireflection layer after the film formation conditions of the comparative example were adjusted.
Description of the reference numerals
10. 20, 30: film substrate
11: 1 st protective film
12: 1 st adhesive layer
13: polarizing element
14: adhesive layer 2
15: 2 nd protective film
16: transparent film
17: hard coat layer
21: 3 rd adhesive layer
31: adhesive layer
32: release liner
100: polarizing plate with anti-reflection layer
101: anti-reflection layer
Detailed Description
Hereinafter, preferred embodiments of the present invention will be described in detail, but the present invention is not limited thereto. The entire academic literature and patent literature described in the present specification are incorporated by reference in the present specification.
First, terms used in the present specification will be described. The "refractive index" is the refractive index of light having a wavelength of 550nm in an atmosphere at a temperature of 23 ℃. The "main surface" of the laminate (more specifically, the film base material, the 1 st protective film, the 2 nd protective film, the transparent film, the hard coat layer, the primer layer, the adhesive layer, the release liner, the polarizing material, and the like) means a surface orthogonal to the thickness direction of the laminate.
The "bombardment treatment" refers to a surface treatment in which a predetermined gas (such as a rare gas or oxygen gas) is introduced and the surface of the thin film substrate is subjected to plasma treatment.
Unless specified, the number average secondary particle diameter of particles is a number average of the equivalent circle diameters (Heywood) of 100 primary particles measured using a scanning electron microscope and image processing software (for example, "ImageJ" manufactured by national institute of health).
The unit "sccm (Standard Cubic Centimeter per Minute)" of the flow rate is the unit "mL/min" of the flow rate in the standard state (temperature: 0 ℃ C., pressure: 101.3 kPa).
Hereinafter, the term "system" may be appended to the name of a compound, and the compound and its derivatives may be collectively referred to as "compound". In addition, when the term "system" is appended to the name of a compound to indicate the name of the polymer, it means that the repeating unit of the polymer is derived from the compound or a derivative thereof.
The components, functional groups, and the like exemplified in the present specification may be used alone or in combination of 2 or more kinds unless otherwise specified.
For ease of understanding, the drawings referred to in the following description are schematically represented mainly by the respective components, and the size, number, shape, and the like of the components shown in the drawings may be different from those in practice in terms of convenience in manufacturing the drawings. In the drawings described below, the same reference numerals are given to the same components as those in the drawings described above, and the description thereof may be omitted for convenience of description.
< method for producing polarizing plate with antireflection layer >
The method for producing a polarizing plate with an antireflection layer according to the present embodiment is a method for producing a polarizing plate with an antireflection layer, which includes a film base material and an antireflection layer provided on one main surface side of the film base material, and includes a step Sa and a step Sb. In step Sa, an antireflection layer formed of 2 or more films is formed on one principal surface side of the film base material. In step Sb, after at least one layer constituting the antireflection layer is formed, the layer is irradiated with visible light and the reflected light is detected (in-line reflected light measurement). The steps Sa and Sb are continuously performed while the film base material is conveyed in one direction. The film base material is a laminate having, in order, a 1 st protective film, a 1 st adhesive layer, a polarizer, a 2 nd adhesive layer, and a 2 nd protective film. The 1 st protective film and the polarizing element are bonded by the 1 st adhesive layer. The 2 nd protective film and the polarizing element are bonded by the 2 nd adhesive layer. The 1 st protective film and the 2 nd protective film are each larger than the width of the polarizing member and protrude from both ends in the width direction of the polarizing member. The distance between the 1 st protective film and the 2 nd protective film in at least a part of the portions protruding from both ends in the width direction of the polarizing element is narrower than the distance between the 1 st protective film and the 2 nd protective film in the portions sandwiching the ends in the width direction of the polarizing element.
According to the present embodiment, since the above-described structure is provided, a method for manufacturing a polarizing plate with an antireflection layer, which can maintain the uniformity of the reflected light characteristics, can be provided. Hereinafter, the step Sa may be referred to as an "antireflection layer forming step". The step Sb may be referred to as an "online reflected light measurement step".
Hereinafter, a detailed description will be given of a method for manufacturing a polarizing plate with an antireflection layer according to this embodiment, with reference to the drawings as appropriate. First, a film base material will be described.
[ film substrate ]
Fig. 1 is a cross-sectional view showing an example of a film base material that can be used in the present embodiment. The film base 10 shown in fig. 1 is a laminate having, in order, a 1 st protective film 11, a 1 st adhesive layer 12, a polarizer 13, a 2 nd adhesive layer 14, and a 2 nd protective film 15. The 2 nd protective film 15 includes a transparent film 16 and a hard coat layer 17 provided on one principal surface side of the transparent film 16 (in fig. 1, the principal surface 16a of the transparent film 16 on the side opposite to the 2 nd adhesive layer 14 side). The 1 st protective film 11 and the polarizer 13 are bonded by the 1 st adhesive layer 12. The 2 nd protective film 15 and the polarizer 13 are bonded via the 2 nd adhesive layer 14. The 1 st protective film 11 and the 2 nd protective film 15 are each larger than the width of the polarizing member 13, and protrude from both ends in the width direction of the polarizing member 13. The distance D between the 1 st protective film 11 and the 2 nd protective film 15 in at least a part of the portion P extending from both ends of the polarizer 13 in the width direction 1 The distance D between the 1 st protective film 11 and the 2 nd protective film 15 is smaller than the distance D between the 1 st protective film 11 and the 2 nd protective film 15 in the portion sandwiching the widthwise end portion of the polarizer 13 2 Narrow.
In general, a film base material for a polarizing plate having an antireflection layer is used in a state in which the above-mentioned protruding portion P is cut off (slit) when the antireflection layer is formed. According to the studies by the present inventors, it was found that when the antireflection layer is formed in a state where the above-mentioned protruding portion P is cut off, moisture in the polarizer 13 is likely to evaporate from the end face of the polarizer 13, and as a result, there is a tendency that the reflected light characteristics are deviated in the longitudinal direction or the width direction of the obtained polarizing plate with the antireflection layer. In detail, when a film base material in which the above-described protruding portion P is cut off is used, moisture in the polarizer 13 is easily evaporated from the end face of the polarizer 13, and the gas composition in the film forming chamber (particularly, the gas composition in the vicinity of the end face of the polarizer 13) is easily changed when the antireflection layer is formed. As a result, the thickness of the antireflection layer tends to vary widely in the longitudinal direction or the width direction of the obtained polarizing plate with the antireflection layer. Therefore, when a film base material obtained by cutting out the above-described protruding portion P is used, the variation in the thickness of the antireflection layer in the longitudinal direction or the width direction becomes large, and thus there is a tendency that the reflected light characteristics (for example, hue and the like) vary in the longitudinal direction or the width direction of the polarizing plate with the antireflection layer.
In the present embodiment, the distance D between the 1 st protective film 11 and the 2 nd protective film 15 in at least a part of the protruding portion P 1 The distance D between the 1 st protective film 11 and the 2 nd protective film 15 is smaller than the distance D between the 1 st protective film 11 and the 2 nd protective film 15 in the portion sandwiching the widthwise end portion of the polarizer 13 2 It is considered that it is difficult to release the gas from the end face of the polarizer 13 due to the pressure loss. Therefore, in the present embodiment, it is presumed that evaporation of moisture from the end surface of the polarizer 13 is suppressed, and as a result, fluctuation in the gas composition in the film forming chamber at the time of forming the antireflection layer is suppressed. In this way, the film formation conditions of the antireflection layer using the detection result obtained in the in-line reflected light measurement step described later can be easily adjusted, and therefore, the variation in thickness of the antireflection layer in the longitudinal direction or the width direction of the obtained polarizing plate with the antireflection layer becomes small. Therefore, according to the present embodiment, since the variation in the thickness of the antireflection layer in the longitudinal direction or the width direction is small, the variation in the reflected light characteristics (for example, hue or the like) in the longitudinal direction or the width direction of the polarizing plate with the antireflection layer is small. Therefore, according to the present embodiment, a method for manufacturing a polarizing plate with an antireflection layer, which can maintain the uniformity of the reflected light characteristics, can be provided.
As a means for making the above-mentioned interval D 1 Than the above interval D 2 Examples of the method for narrowing include a method using cure shrinkage of the adhesive used for forming the 1 st adhesive layer 12 and the 2 nd adhesive layer 14. Specifically, when the 1 st protective film 11 is bonded to the polarizer 13 with an adhesive and the 2 nd protective film 15 is bonded to the polarizer 13 with an adhesive, the ends of the 1 st protective film 11 and the 2 nd protective film 15 are pulled close to each other with curing shrinkage of the adhesive. In addition, the ends of the 1 st protective film 11 and the 2 nd protective film 15 are also pulled close to each other by the interfacial tension when the adhesive wets and spreads near the ends of the polarizer 13 in the width direction. As a result, the above-mentioned interval D as shown in FIG. 1 can be obtained 1 Than the above interval D 2 A narrow film substrate 10.
In order to further suppress evaporation of moisture from the end face of the polarizer 13, it is preferable to use a film base 20 having a 3 rd adhesive layer 21 for bonding the 1 st protective film 1 and the 2 nd protective film 15 to each other in at least a part of the portion P extending from both ends in the width direction as shown in fig. 2. The adhesive used as the material of the 3 rd adhesive layer 21 may be the same type as or different from the adhesive used as the material of the 1 st adhesive layer 12 and the 2 nd adhesive layer 14. As the adhesive to be the material of the 3 rd adhesive layer 21, for example, an adhesive to be the material of the 1 st adhesive layer 12 described later can be used.
In order to further suppress evaporation of moisture from the end face of the polarizer 13, as shown in fig. 2, the 3 rd adhesive layer 21 is preferably integrally formed with the 1 st adhesive layer 12 and the 2 nd adhesive layer 14. In order to further suppress evaporation of moisture from the end face of the polarizer 13, it is preferable that the end face of the polarizer 13 in the width direction be sealed with the 3 rd adhesive layer 21, as shown in fig. 2. When the 3 rd adhesive layer 21 is formed integrally with the 1 st adhesive layer 12 and the 2 nd adhesive layer 14, the application amount of the adhesive may be adjusted so that the adhesive overflows to the above-described protruding portion P when the 1 st protective film 11 is adhered to the polarizer 13 by the adhesive and when the 2 nd protective film 15 is adhered to the polarizer 13 by the adhesive.
Next, elements of the film base material 10 will be described.
(1 st protective film 11)
The 1 st protective film 11 is, for example, a transparent resin film having flexibility. Examples of the material constituting the 1 st protective film 11 include polyester resins, polyolefin resins, polystyrene resins, acrylic resins, polycarbonate resins, polyether sulfone resins, polysulfone resins, polyamide resins, polyimide resins, cellulose resins, norbornene resins, polyarylate resins, and polyvinyl alcohol resins. Examples of the polyester resin include polyethylene terephthalate (PET), polybutylene terephthalate, and polyethylene naphthalate. Examples of the polyolefin resin include polyethylene, polypropylene, and cycloolefin polymer (COP). As the cellulose resin, for example, cellulose Triacetate (TAC) is cited. These materials may be used alone or in combination of two or more. As the material of the 1 st protective film 11, one selected from the group consisting of polyester resin, polyolefin resin, and cellulose resin is preferable, one selected from the group consisting of PET, COP, and TAC is more preferable, and TAC is further preferable from the viewpoints of transparency and strength. That is, as the 1 st protective film 11, one film selected from the group consisting of a polyester resin film, a polyolefin resin film, and a cellulose resin film is preferable, one film selected from the group consisting of a PET film, a COP film, and a TAC film is more preferable, and a TAC film is further preferable.
From the viewpoint of strength, the thickness of the 1 st protective film 11 is preferably 5 μm or more, more preferably 10 μm or more, and still more preferably 20 μm or more. From the viewpoint of operability, the thickness of the 1 st protective film 11 is preferably 300 μm or less, more preferably 200 μm or less.
One main surface or both main surfaces of the 1 st protective film 11 may be subjected to a surface modification treatment. Examples of the surface modification treatment include corona treatment, plasma treatment, ozone treatment, primer treatment, glow treatment, and coupling agent treatment.
From the viewpoint of improving the transparency of the polarizing plate with an antireflection layer, the total light transmittance (JIS K7375-2008) of the 1 st protective film 11 is preferably 80% or more, more preferably 90% or more, still more preferably 95% or more and 100% or less.
(polarizing element 13)
Examples of the polarizer 13 include polarizers obtained by uniaxially stretching hydrophilic polymer films such as polyvinyl alcohol films, partially formalized polyvinyl alcohol films, and ethylene-vinyl acetate copolymer partially saponified films by adsorbing dichroic materials such as iodine and dichroic dyes; and a multi-functional oriented film such as a dehydrated polyvinyl alcohol product or a desalted polyvinyl chloride product. Among them, from the viewpoint of having a high degree of polarization, a polyvinyl alcohol (PVA) type polarizer in which a polyvinyl alcohol film such as polyvinyl alcohol or partially formalized polyvinyl alcohol adsorbs a dichroic substance such as iodine or a dichroic dye and is aligned in a predetermined direction is preferable. The thickness of the polarizer 13 is, for example, 5 μm or more and 100 μm or less.
(transparent film 16)
As the material of the transparent film 16, the same materials as those described above as the material of the 1 st protective film 11 are preferably used. The preferable thickness range of the transparent film 16 is also the same as the preferable thickness range of the 1 st protective film 11. The material of the transparent film 16 and the material of the 1 st protective film 11 may be the same kind or different kinds. The thickness of the transparent film 16 may be the same as or different from the thickness of the 1 st protective film 11.
(1 st adhesive layer 12)
As the adhesive to be the material of the 1 st adhesive layer 12, an adhesive based on an acrylic polymer, a silicone polymer, a polyester, a polyurethane, a polyamide, a polyvinyl alcohol, a polyvinyl ether, a vinyl acetate/vinyl chloride copolymer, a modified polyolefin, an epoxy polymer, a fluorine polymer, a rubber polymer, or the like can be appropriately selected and used. The PVA-based polarizer is preferably bonded using a polyvinyl alcohol-based adhesive. The 1 st adhesive layer 12 has a thickness of, for example, 0.1 μm or more and 5.0 μm or less, preferably 0.2 μm or more and 3.0 μm or less.
(2 nd adhesive layer 14)
As the adhesive to be the material of the 2 nd adhesive layer 14, the same adhesives as those described above as the adhesive to be the material of the 1 st adhesive layer 12 are preferably used. The preferable thickness range of the 2 nd adhesive layer 14 is also the same as the preferable thickness range of the 1 st adhesive layer 12 described above. The adhesive used as the material of the 2 nd adhesive layer 14 and the adhesive used as the material of the 1 st adhesive layer 12 may be the same type or different types. The thickness of the 2 nd adhesive layer 14 may be the same as or different from the thickness of the 1 st adhesive layer 12.
(hard coating 17)
The hard coat layer 17 is a layer for improving mechanical properties such as hardness and elastic modulus of the polarizing plate with an antireflection layer. The hard coat layer 17 is formed of, for example, a cured product of a curable resin composition (composition for forming a hard coat layer). Examples of the curable resin contained in the curable resin composition include polyester resins, acrylic resins, urethane acrylate resins, amide resins, silicone resins, epoxy resins, and melamine resins. These curable resins may be used alone or in combination of two or more. From the viewpoint of improving the hardness of the hard coat layer 17, the curable resin is preferably at least one selected from the group consisting of an acrylic resin and a urethane acrylate resin, and more preferably a urethane acrylate resin.
Examples of the curable resin composition include an ultraviolet curable resin composition and a thermosetting resin composition. From the viewpoint of improving productivity of the polarizing plate with the antireflection layer, an ultraviolet-curable resin composition is preferable as the curable resin composition. The ultraviolet-curable resin composition contains at least one selected from the group consisting of ultraviolet-curable monomers, ultraviolet-curable oligomers, and ultraviolet-curable polymers. Specific examples of the ultraviolet-curable resin composition include a composition for forming a hard coat layer described in Japanese patent application laid-open No. 2016-179686.
The curable resin composition may contain particles having a number of uniform secondary particle diameters of 0.5 μm or more (hereinafter, sometimes referred to as "microparticles"). That is, the hard coat layer 17 may contain fine particles. By blending fine particles in the curable resin composition, adjustment of the hardness of the hard coat layer 17, adjustment of the surface roughness, adjustment of the refractive index, and adjustment of the antiglare property can be performed. Examples of the fine particles include metal (or semi-metal) oxide particles, glass particles, and organic particles. Examples of the material of the oxide particles of the metal (or semi-metal) include silica, alumina, titania, zirconia, calcium oxide, tin oxide, indium oxide, cadmium oxide, and antimony oxide. Examples of the material of the organic particles include polymethyl methacrylate, polystyrene, polyurethane, acrylic-styrene copolymer, benzoguanamine, melamine, and polycarbonate.
In order to easily adjust the antiglare property of the hard coat layer 17, the number-average secondary particle diameter of the fine particles is preferably 1.0 μm or more and 5.0 μm or less, more preferably 2.0 μm or more and 4.0 μm or less.
In order to easily adjust the antiglare property of the hard coat layer 17, the amount of the fine particles in the hard coat layer 17 is preferably 5 parts by weight or more, or may be 10 parts by weight or more, 20 parts by weight or more, or 30 parts by weight or more, based on 100 parts by weight of the curable resin. The upper limit of the amount of the fine particles in the hard coat layer 17 is, for example, 90 parts by weight, preferably 80 parts by weight, and may be 70 parts by weight, relative to 100 parts by weight of the curable resin.
The curable resin composition may contain particles having a uniform number of secondary particle diameters of less than 0.5 μm (hereinafter, sometimes referred to as "nanoparticles"). When the hard coat layer 17 is formed of a cured product of a curable resin composition containing nanoparticles, fine irregularities are formed on the surface of the hard coat layer 17, and adhesion between the hard coat layer 17 and a layer formed thereon tends to be improved.
The number-uniform secondary particle diameter of the nanoparticles is preferably 20nm to 80nm, more preferably 25nm to 70nm, still more preferably 30nm to 60nm, from the viewpoint of forming fine irregularities contributing to improvement of adhesion.
As the material of the nanoparticles, inorganic oxides are preferable. Examples of the inorganic oxide include oxides of metals (or semi-metals) such as silicon oxide (silica), titanium oxide, aluminum oxide, zirconium oxide, niobium oxide, zinc oxide, tin oxide, cerium oxide, and magnesium oxide. The inorganic oxide may be a composite oxide of a plurality of (semi) metals. Among the exemplified inorganic oxides, silicon oxide is preferred from the viewpoint of high effect of improving adhesion. That is, as the nanoparticles, particles of silicon oxide (silica particles) are preferable. Functional groups such as acryl groups and epoxy groups may be introduced into the surface of the inorganic oxide particles as nanoparticles for the purpose of improving adhesion and affinity with the resin.
The amount of the nanoparticles in the hard coat layer 17 is preferably 5 parts by weight or more, and may be 10 parts by weight or more, 20 parts by weight or more, or 30 parts by weight or more, relative to 100 parts by weight of the curable resin. When the amount of the nanoparticles is 5 parts by weight or more, the adhesion to the layer formed on the hard coat layer 17 can be further improved. The upper limit of the amount of the nanoparticles in the hard coat layer 17 is, for example, 90 parts by weight, preferably 80 parts by weight, and may be 70 parts by weight, relative to 100 parts by weight of the curable resin.
The curable resin composition (hard coat layer-forming composition) contains, for example, the curable resin described above and a polymerization initiator (e.g., photopolymerization initiator), and if necessary, a solvent capable of dissolving or dispersing these components. In addition, the curable resin composition (hard coat layer forming composition) may contain, in addition to the above-described components, fine particles, nanoparticles, leveling agents, viscosity modifiers (thixotropic agents, thickening agents, and the like), antistatic agents, antiblocking agents, dispersants, dispersion stabilizers, antioxidants, ultraviolet absorbers, antifoaming agents, surfactants, lubricants, and the like.
From the viewpoint of improving the hardness of the hard coat layer 17, the thickness of the hard coat layer 17 is preferably 1 μm or more, more preferably 2 μm or more. From the viewpoint of ensuring the flexibility of the antireflection layer-attached polarizing plate, the thickness of the hard coat layer 17 is preferably 50 μm or less, more preferably 40 μm or less, further preferably 35 μm or less, further preferably 30 μm or less.
(method of Forming hard coating layer 17)
The hard coat layer 17 is formed, for example, by applying a curable resin composition (composition for forming a hard coat layer) to one main surface of the transparent film 16 (in fig. 1, the main surface 16a on the opposite side of the transparent film 16 from the 2 nd adhesive layer 14 side) and, if necessary, removing a solvent and curing the resin. By providing the hard coat layer 17 on one main surface of the transparent film 16, as shown in fig. 1, the 2 nd protective film 15 including the transparent film 16 and the hard coat layer 17 can be obtained.
As a coating method of the composition for forming a hard coat layer, any suitable method such as bar coating (bar coating method), roll coating, gravure coating, bar coating (rod coating method), slot coating, curtain coating, spray coating, comma coating, and the like can be used. The drying temperature of the coated film may be set to a suitable temperature depending on the composition of the composition for forming a hard coat layer, for example, 50 ℃ to 150 ℃. When the resin component in the composition for forming a hard coat layer is a thermosetting resin, the coating film is cured by heating. When the resin component in the composition for forming a hard coat layer is a photocurable resin, the coating film is cured by irradiation with active energy rays such as ultraviolet rays. The cumulative light quantity of the irradiated light is preferably 100mJ/cm 2 Above and 500mJ/cm 2 The following is given.
In order to improve the adhesion between the hard coat layer 17 and the layer formed thereon, the main surface of the hard coat layer 17 on the opposite side to the transparent film 16 side may be subjected to a bombardment treatment. The gas used in the bombardment treatment is preferably one or more selected from the group consisting of a rare gas (specifically, argon or the like) and oxygen.
In order to further improve the adhesion between the hard coat layer 17 and the layer formed thereon, it is preferable to subject the main surface of the hard coat layer 17 on the opposite side to the transparent film 16 side to a bombardment treatment under a pressure of 0.1Pa or more and 1.0Pa or less.
In order to further improve the adhesion of the hard coat layer 17 to the layer formed thereon, the effective power density in the bombardment treatment step is preferably 0.01 W.min/cm 2 M is more than,More preferably 0.02 W.min/cm 2 M or more, more preferably 0.03 W.min/cm 2 M or more. In order to suppress deformation of the thin film substrate in the bombardment treatment step, the effective power density in the bombardment treatment step is preferably 0.60 W.min/cm 2 M or less, more preferably 0.55 W.min/cm 2 M or less, more preferably 0.50 W.min/cm 2 M or less. The effective power density refers to the power density (W/cm) of the plasma output 2 ) Divided by the transport speed (m/min) of the film based on the roll-to-roll method. When the plasma output is the same but the transport speed is high, the effective processing power is reduced.
As described above, the example of the film base material usable in the present embodiment has been described, but the film base material usable in the present invention is not limited to the above example. For example, the film substrate usable in the present invention may not have a hard coat layer. When the film base material does not have a hard coat layer, a transparent film can be used as the 2 nd protective film, for example.
In the present invention, as shown in fig. 3, a film base 30 further including an adhesive layer 31 provided on the 1 st protective film 11 on the side opposite to the polarizer 13 side may be used. In the film base material 30 shown in fig. 3, the adhesive layer 31 is provided on the main surface 11a of the 1 st protective film 11 on the opposite side of the polarizer 13 side.
The pressure-sensitive adhesive constituting the pressure-sensitive adhesive layer 31 is not particularly limited, and for example, a transparent pressure-sensitive adhesive based on a polymer such as an acrylic polymer, a silicone polymer, a polyester, a polyurethane, a polyamide, a polyvinyl ether, a vinyl acetate-vinyl chloride copolymer, a modified polyolefin, an epoxy resin, a fluororesin, a natural rubber, or a synthetic rubber can be suitably selected and used. The thickness of the pressure-sensitive adhesive layer 31 is not particularly limited, but is preferably 5 μm or more and 100 μm or less from the viewpoint of both the thinness and the adhesiveness.
As shown in fig. 3, a release liner 32 may be temporarily bonded to a main surface 31a of the adhesive layer 31 on the opposite side of the 1 st protective film 11 side. The release liner 32 protects the surface of the adhesive layer 31, for example, during the period before the polarizing plate with the antireflection layer is attached to the image display unit (not shown). As a constituent material of the release liner 32, a plastic film formed of acrylic, polyolefin, cyclic polyolefin, polyester, or the like is suitably used. The thickness of the release liner 32 is, for example, 5 μm or more and 200 μm or less. The release treatment is preferably applied to the surface of the release liner 32. Examples of the release agent used in the release treatment include silicone materials, fluorine materials, long-chain alkyl materials, fatty acid amide materials, and the like.
[ anti-reflective layer Forming Process and Online reflected light measuring Process ]
Next, the antireflection layer forming step and the in-line reflected light measuring step will be described with reference to a to C of fig. 4 and 5. Fig. 4 is a schematic diagram showing an example of an antireflection layer deposition apparatus. Fig. 5 a to C are sectional views of an antireflection layer forming process in terms of steps.
First, an example of an antireflection layer deposition apparatus will be described. The film forming apparatus shown in fig. 4 is a film forming apparatus capable of continuously performing an antireflection layer forming process and an in-line reflected light measuring process while conveying a thin film base material in one direction, and capable of reflecting the detection result in the in-line reflected light measuring process to the film forming condition in the antireflection layer forming process. The film forming apparatus shown in fig. 4 includes a 1 st film forming roller 281 and a 2 nd film forming roller 282. Along the circumferential direction of each of the film forming rollers 281 and 282, 4 film forming chambers (the 1 st film forming chamber 210, the 2 nd film forming chamber 220, the 3 rd film forming chamber 230, and the 4 th film forming chamber 240) are provided which are partitioned by partition walls. Cathodes 214, 224, 234 and 244 are disposed in each film forming chamber and are connected to power sources 216, 226, 236 and 246, respectively. Targets 213, 223, 233, and 243 are disposed on the cathodes 214, 224, 234, and 244, respectively, so as to oppose the film-forming rollers 281 and 282. A gas introduction pipe is connected to each of the film forming chambers 210, 220, 230, and 240, and valves 219, 229, 239, and 249 are provided upstream of the gas introduction pipe.
A roll of the film base material 10 (see a of fig. 5) is provided on the unwinding roller 251 in the preparation chamber 250. The film base material 10 unwound from the unwinding roller 251 is conveyed onto the 1 st film forming roller 281 and guided to the 1 st film forming chamber 210 and the 2 nd film forming chamber 220 in this order. In the 1 st film forming chamber 210, the high refractive index layer 102 is formed on the opposite side of the hard coat layer 17 to the transparent thin film 16 side (in a of fig. 5, the main surface 17a of the hard coat layer 17 to the opposite side of the transparent thin film 16 side), and in the 2 nd film forming chamber 220, the low refractive index layer 103 is formed on the high refractive index layer 102 (see B of fig. 5). The film substrate 10 having the high refractive index layer 102 and the low refractive index layer 103 formed thereon is conveyed to the 2 nd film forming roller 282, and the high refractive index layer 104 and the low refractive index layer 105 are formed in this order in the 3 rd film forming chamber 230 and the 4 th film forming chamber 240 (see C in fig. 5). Details of the high refractive index layer and the low refractive index layer will be described later. Through the above-described antireflection layer forming step, the antireflection layer 101 having the high refractive index layer 102, the low refractive index layer 103, the high refractive index layer 104, and the low refractive index layer 105 in this order is formed on the main surface of the hard coat layer 17 on the opposite side of the transparent film 16 side, and the antireflection-layer-attached polarizing plate 100 is obtained (see C of fig. 5).
The antireflection-layer-attached polarizing plate 100 having the antireflection layer 101 formed thereon is guided to the winding chamber 260 and wound by the winding roller 261, thereby obtaining a wound body of the antireflection-layer-attached polarizing plate 100.
In the winding chamber 260, a light irradiation portion 291 and a light detection portion 293 are disposed so as to face the antireflection layer 101 of the antireflection layer-attached polarizing plate 100. The light irradiated from the light irradiation portion 291 may be white light or monochromatic light as long as the light contains visible light. The light irradiation may be continuous or intermittent. In the in-line reflected light measurement step, the light detector 293 detects reflected light of light emitted from the light emitter 291 to the antireflection layer 101. The reflected light detected by the light detection unit 293 is converted into an electrical signal by a light receiving element (not shown), and is calculated by the calculation unit 273 as needed. The calculation unit 273 calculates the spectrum of the detected reflected light to a specific chromaticity system (for example, XYZ chromaticity system, L * a * b * Chromaticity system, etc.), or calculation of film thickness, etc. In order to intercept the reflected light from the film base material 10 including the polarizer 13, a polarizing plate (not shown) for polarizing the visible light irradiated from the light irradiation portion 291 is preferably disposed. General purpose medicine By cutting off the reflected light from the film base material 10 including the polarizer 13, only the reflected light characteristics of the formed antireflection layer 101 can be measured.
Further, the calculation unit 273 determines the difference between the detected reflection characteristic of the reflected light and the target reflection characteristic, and if the difference exceeds the threshold value, a signal is sent to the control unit 275 to change the film formation condition of the thin film. The control unit 275 adjusts the film forming conditions of the antireflection layer 101 so that the characteristics (reflectance, color, etc.) of the reflected light fall within a predetermined range.
The film forming conditions to be adjusted include the amount of gas introduced into the film forming chamber, the conveying speed of the thin film, the amount of electric power to be charged, and the like. For example, in the film forming apparatus shown in fig. 4, the control unit 275 can adjust the film forming conditions of the thin film in each film forming chamber by adjusting the rotational speeds of the unwinding roller 251, the winding roller 261, the 1 st film forming roller 281, and the 2 nd film forming roller 282, the amounts of electric power supplied from the power sources 216, 226, 236, and 246, and the opening degrees of the gas introducing valves 219, 229, 239, and 249. The change in the characteristics of the reflected light is mainly caused by the variation in the film thickness of the thin film. Therefore, it is preferable to adjust the film forming conditions of the thin film so that the thickness of the thin film formed in each film forming chamber is close to a set value. The film formation conditions are adjusted by, for example, PID control.
In order to determine the difference from the target reflected light characteristic, it is necessary to determine the reflected light characteristic to be a reference in advance. The reflected light characteristic as a reference is appropriately determined according to the specification of the product or the like. As an example, there are a method based on the center of the standard range of the product and a method based on the reflected light spectrum calculated by optical calculation based on the set film thickness and refractive index of each layer (see the example of japanese patent application laid-open No. 2016-122173). The reflected light spectrum of the product measured off-line may be used as a reference.
In the present embodiment, it is considered that evaporation of moisture from the end face of the polarizer 13 (see a of fig. 5) is suppressed, and as a result, it is considered that fluctuation in the gas composition in the film forming chamber at the time of forming the antireflection layer 101 is suppressed. Thus, adjustment of the film formation condition of the antireflection layer 101 (specifically, adjustment of the gas introduction amount or the like) using the detection result obtained in the in-line reflected light measurement step becomes easy. In particular, according to the present embodiment, the reflected light characteristics can be controlled within the allowable range even at the end in the width direction of the polarizing plate with the antireflection layer, and therefore the width of the polarizing plate with the antireflection layer that can be used as a product becomes large.
In order to further suppress the variation in the reflected light characteristics in the width direction of the polarizing plate with an antireflection layer, it is preferable to provide a plurality of light irradiation portions 291 and light detection portions 293 in the width direction of the antireflection layer 101, respectively, and to perform in-line reflected light measurement (irradiation of visible light and detection of reflected light) at a plurality of portions in the width direction of the antireflection layer 101. In this case, for example, if a plurality of gas introduction pipes are provided in each film forming chamber in the width direction of the thin film, the gas introduction amounts can be adjusted at a plurality of portions in the width direction of the thin film, respectively. By performing the in-line reflected light measurement at a plurality of portions in the width direction of the antireflection layer 101, the variation in the reflected light characteristics can be suppressed in both the longitudinal direction and the width direction of the polarizing plate with the antireflection layer. In order to suppress the variation in the reflected light characteristics in the width direction of the polarizing plate with the antireflection layer, a measuring head including a light irradiation section and a light detection section may be provided so as to be movable in the width direction of the film.
When the antireflection layer 101 is formed by the reactive sputtering method, it is preferable to control the amount of the reactive gas such as oxygen gas introduced by Plasma Emission Monitoring (PEM) control when adjusting the film forming conditions of the antireflection layer 101. In PEM control, the plasma emission intensity of the sputtered film is detected, and the amount of reactive gas introduced is adjusted so that the emission intensity becomes a predetermined control value (set point, hereinafter sometimes referred to as "SP"). By automatically adjusting the amount of gas introduced so that the plasma emission intensity is constant, film formation at a high rate can be performed while maintaining the transition region, and the film formation rate can be kept constant. However, when film formation is continuously performed for a long period of time, the film formation rate changes due to the influence of corrosion of the target or the like even if the plasma emission intensity is the same. Therefore, in the case of performing continuous film formation for a long period of time, in order to suppress variation in reflection characteristics in the longitudinal direction of the polarizing plate with an antireflection layer, it is preferable to appropriately adjust the SP of the PEM based on the measurement result of the optical characteristics in the in-line reflection measurement step.
In PEM control, in order to control the state of sputter film formation in each film formation chamber, the plasma emission intensity is constantly monitored by the PEM, and the gas introduction amount into each film formation chamber is feedback-controlled based on the SP set to the emission intensity in a predetermined range. By providing a plurality of PEM in the width direction of the membrane, SP can be set individually in each PEM. Accordingly, the balance of the gas introduction amounts introduced to the positions in the width direction corresponding to the PEM can be adjusted, and therefore, the antireflection layer 101 having a uniform film thickness in the width direction can be formed. For example, in the in-line reflected light measuring step, the reflected light is detected, the film thickness is calculated based on the detection result, and the SP is changed based on the calculation result so that the film thickness of the antireflection layer 101 becomes uniform in the longitudinal direction or the width direction of the thin film, whereby the reflected light characteristics in the longitudinal direction or the width direction of the thin film can be maintained uniform. Hereinafter, a series of operations of detecting reflected light in the in-line reflected light measuring step, calculating a film thickness from the detection result, and changing the SP based on the calculation result so that the film thickness of the antireflection layer becomes uniform in the longitudinal direction or the width direction of the thin film may be referred to as "feedback operation". The feedback operation is repeated until, for example, the variation in film thickness in the longitudinal direction or the width direction of the antireflection layer 101 becomes an allowable range. According to the present embodiment, the fluctuation of the gas composition in the film forming chamber at the time of forming the antireflection layer can be suppressed, and therefore the number of feedback operations becomes small. This can improve the productivity of the polarizing plate with the antireflection layer.
[ anti-reflection layer 101]
Next, details of the antireflection layer 101 will be described. The antireflection layer 101 is formed of 2 or more thin films. The antireflection layer 101 shown in fig. 5C has 4 layers of a high refractive index layer 102, a low refractive index layer 103, a high refractive index layer 104, and a low refractive index layer 105 in this order from the hard coat layer 17 side. The antireflection layer of the polarizing plate with an antireflection layer is not limited to a 4-layer structure such as the antireflection layer 101, and may be a 2-layer structure, a 3-layer structure, a 5-layer structure, or a laminated structure of 6 or more layers. In order to reduce reflection at the air interface, the antireflection layer of the polarizing element with an antireflection layer is preferably the outermost layer (layer farthest from the polarizing element) that is a low refractive index layer.
In general, the optical film thickness (product of refractive index and thickness) of the thin film of the antireflection layer is adjusted so that the inverted phases of the incident light and the reflected light cancel each other. By using a multilayer laminate in which the antireflection layer is a film of 2 or more layers having different refractive indices, the reflectance can be reduced in a wavelength range of a wide band of visible light.
Examples of the material of the thin film constituting the antireflection layer 101 include oxides, nitrides, and fluorides of metals (or semi-metals). The antireflection layer 101 is preferably an alternating stack of high refractive index layers and low refractive index layers, and more preferably an alternating stack of 2 or more high refractive index layers and 2 or more low refractive index layers.
The refractive index of the high refractive index layer is, for example, 1.9 or more, preferably 2.0 or more. Examples of the material of the high refractive index layer include titanium oxide, niobium oxide, zirconium oxide, tantalum oxide, zinc oxide, indium Tin Oxide (ITO), antimony doped tin oxide (ATO), and the like. Among them, one or more selected from the group consisting of titanium oxide and niobium oxide is preferable. The refractive index of the low refractive index layer is, for example, 1.6 or less, preferably 1.5 or less. Examples of the material of the low refractive index layer include silicon oxide, titanium nitride, magnesium fluoride, barium fluoride, calcium fluoride, hafnium fluoride, lanthanum fluoride, and the like. Among them, silicon oxide is preferable. It is particularly preferable to alternately laminate niobium oxide (Nb 2 O 5 ) Thin film and silicon oxide (SiO) as low refractive index layer 2 ) A film. In addition to the low refractive index layer and the high refractive index layer, a medium refractive index layer having a refractive index of more than 1.6 and less than 1.9 may be provided.
The film thickness of the high refractive index layer and the low refractive index layer is preferably 5nm to 200nm, more preferably 10nm to 150nm, respectively. The film thickness of each layer may be designed so that the reflectance of visible light becomes smaller, depending on the refractive index, the laminated structure, and the like. For example, the laminated structure of the high refractive index layer and the low refractive index layer includes 4 layers including, from the film base material 10 side, a high refractive index layer having an optical film thickness of 20nm to 55nm, a low refractive index layer having an optical film thickness of 35nm to 60nm, a high refractive index layer having an optical film thickness of 65nm to 250nm, and a low refractive index layer having an optical film thickness of 100nm to 150 nm.
The antireflection layer 101 is made of niobium oxide (Nb 2 O 5 ) Film and silicon oxide (SiO) as a low refractive index layer 2 ) In the case of a 4-layer alternating laminate in which thin films are alternately laminated, examples of the structure of the antireflection layer 101 include a structure including a niobium oxide thin film having a thickness of 5nm to 20nm, a silicon oxide thin film having a thickness of 20nm to 60nm, a niobium oxide thin film having a thickness of 25nm to 120nm, and a silicon oxide thin film having a thickness of 50nm to 100nm, in this order from the hard coat layer 17 side.
In order to obtain a polarizing material with an antireflection layer excellent in high-temperature durability, the thickness of the antireflection layer 101 is preferably 100nm or more and 300nm or less, more preferably 120nm or more and 280nm or less, still more preferably 140nm or more and 260nm or less, still more preferably 160nm or more and 240nm or less. In the present specification, the "thickness of the antireflection layer" is the total (total thickness) of the thicknesses of the respective layers constituting the antireflection layer.
The method for forming the antireflection layer 101 is not particularly limited, and may be either a wet coating method or a dry coating method. Since a thin film having a uniform thickness can be formed, a dry coating method such as a vacuum deposition method, a CVD method, or a sputtering method is preferable, and a sputtering method is more preferable. From the viewpoint of improving productivity, a method of forming a film using a roll-to-roll type sputter film forming apparatus as shown in fig. 4 (roll-to-roll type sputter method) is preferable as the method of forming the antireflection layer 101. In the sputtering method, a film is formed while introducing an inert gas such as argon and a reactive gas such as oxygen as needed into a film forming chamber. In the case of forming an oxide film by a sputtering method, it can be performed by any one of a method using an oxide target and a reactive sputtering method using a metal (or semi-metal) target.
When an insulating oxide such as silicon oxide is formed using an oxide target, RF discharge is required, and thus the film formation rate tends to be low and the productivity tends to be low. Therefore, the sputtering film formation of the oxide is preferably a reactive sputtering method using a metal target. In the reactive sputtering method, a film is formed while introducing an inert gas such as argon and a reactive gas such as oxygen into a film forming chamber. In the reactive sputtering method, the amount of oxygen is preferably adjusted to form a transition region between the metal region and the oxide region. When film formation is performed in a metal region where the oxygen content is insufficient, the oxygen content of the obtained oxide film is significantly smaller than the stoichiometric composition, and the oxide film tends to have metallic luster and lower transparency. In addition, in the oxide region where the oxygen amount is large, the film formation rate tends to be extremely lowered. The sputtering film formation can form an oxide film at a high rate by adjusting the oxygen amount to form a transition region. In the case of forming the antireflection layer 101 by the reactive sputtering method, the amount of the reactive gas introduced can be controlled by the PEM control described above, and thus adjustment of the film forming conditions of the antireflection layer 101 becomes easier. As a sputtering power source used in the reactive sputtering method, a DC power source or an MFAC power source (an AC power source having a frequency band of several kHz to several MHz) is preferable.
The power density when the sputtering method is carried out is, for example, 0.1W/cm 2 Above and 20W/cm 2 Hereinafter, it is preferably 1W/cm 2 Above 15W/cm 2 The following is given. The surface temperature of the film-forming roller when the sputtering method is performed is, for example, from-25 ℃ to 25 ℃, preferably from-20 ℃ to 0 ℃. The pressure in the film forming chamber when the sputtering method is performed is, for example, 0.01Pa to 10Pa, preferably 0.1Pa to 1.0 Pa.
The polarizing plate with an antireflection layer obtained by the manufacturing method of the present embodiment is used for a display such as a liquid crystal display device or an organic EL display device. Particularly in the case of being used as the outermost layer of the display, the visibility of the display based on the antireflection is improved.
Preferred embodiment of method for producing polarizing plate with antireflection layer
In the present embodiment, in order to further maintain the reflected light characteristics uniformly, the following condition 1 is preferably satisfied, the following condition 2 is more preferably satisfied, and the following condition 3 is more preferably satisfied.
Condition 1: the film base material further comprises the 3 rd adhesive layer.
Condition 2: the condition 1 is satisfied, and the 3 rd adhesive layer is integrally formed with the 1 st adhesive layer and the 2 nd adhesive layer.
Condition 3: the condition 2 is satisfied, and the end face in the width direction of the polarizer is sealed by the 3 rd adhesive layer.
Other embodiments
The method for manufacturing the polarizing plate with an antireflection layer according to the present embodiment has been described above, but the present invention is not limited to the above-described embodiment. For example, the in-line reflected light measurement step may be performed at any stage as long as it is performed after at least 1 thin film is formed. For example, after the high refractive index layer 102 and the low refractive index layer 103 are formed on the 1 st film formation roller 281, the low refractive index layer 103 may be irradiated with visible light from the light irradiation unit 297 (see fig. 4), and the reflected light may be detected by the light detection unit 299 (see fig. 4), thereby performing on-line detection of the reflected light. In addition, the reflected light may be detected at two or more places on-line. For example, after the high refractive index layer 102 and the low refractive index layer 103 are formed, the light irradiation portion 297 and the light detection portion 299 may perform on-line detection of the reflected light, and after the high refractive index layer 104 and the low refractive index layer 105 are formed, the light irradiation portion 291 and the light detection portion 293 may perform on-line detection of the reflected light. If the on-line measurement is performed at two or more places in this way, it is easy to determine the film forming chamber in which the film forming conditions should be adjusted, and finer control can be performed.
As described above, the method of forming the antireflection layer is not limited to the sputtering method, and various dry coating methods and wet coating methods may be used. When a thin film is formed by a method other than the sputtering method, the formation condition of the thin film is adjusted based on the on-line detection result of the reflected light, whereby a polarizing plate with an antireflection layer excellent in uniformity of the reflected light characteristic is obtained.
The production method of the present invention may further include a step Sc of forming a primer layer on one principal surface side of the film base material before the antireflection layer forming step. In the case where the production method of the present invention further includes the step Sc, an antireflection layer is formed on the main surface of the primer layer on the side opposite to the film base material side in the antireflection layer forming step.
By providing the primer layer, the adhesion between the film base material and the antireflection layer is improved. Examples of the material of the primer layer include metals (or semi-metals) such as silicon, nickel, chromium, tin, gold, silver, platinum, zinc, titanium, indium, tungsten, aluminum, zirconium, and palladium; alloys of these metals (or semi-metals); oxides, fluorides, sulfides, or nitrides of these metals (or semi-metals), and the like. The oxide constituting the primer layer may be a composite oxide such as Indium Tin Oxide (ITO). Among them, as a material of the primer layer, an inorganic oxide is preferable, silicon oxide, indium oxide or ITO is more preferable, and SiO is further preferable x (x<2)。
In order to improve the adhesion between the film base material and the antireflection layer and to ensure the light transmittance of the primer layer, the thickness of the primer layer is preferably 0.5nm or more and 20nm or less, more preferably 0.5nm or more and 10nm or less, and still more preferably 1.0nm or more and 10nm or less.
The method of forming the primer layer is not particularly limited, and may be any of a wet coating method and a dry coating method. Since a thin film having a uniform thickness can be formed, a dry coating method such as a vacuum deposition method, a CVD method, or a sputtering method is preferable, and a sputtering method is more preferable. From the viewpoint of improving productivity, as a method of forming the primer layer, a method of forming a film using a roll-to-roll type sputtering film forming apparatus (roll-to-roll type sputtering method) is preferable. In the roll-to-roll sputtering method, a long film base material can be continuously formed into, for example, a primer layer and an antireflection layer while being conveyed in the longitudinal direction (MD direction). In forming the primer layer by sputtering, for example, the film forming conditions can be appropriately set among the conditions described in the above [ anti-reflection layer 101 ].
The method for producing a polarizing plate with an antireflection layer according to the present invention may further include a step of forming an antifouling layer after the in-line reflected light measurement step. As a material of the antifouling layer, a fluorine-containing compound is preferable.
The method for producing a polarizing plate with an antireflection layer according to the present invention may further include a step of cutting out portions extending from both ends in the width direction of the polarizing material after the in-line reflected light measurement step.
The method for producing a polarizing plate with an antireflection layer according to the present invention may include a pre-film-forming step for the purpose of setting initial conditions for film formation at the start of film formation. In this case, the antireflection layer forming step and the in-line reflected light measuring step are performed in a main film forming step after the prefilming step. Details of the prefilming step are described in, for example, japanese patent application laid-open No. 2017-218674.
Examples
Hereinafter, examples of the present invention will be described, but the present invention is not limited to the following examples.
< example >
[ prefilming ]
First, the prefilming will be described. In the pre-film formation, a black PET film (width 1300 mm) having a thickness of 100 μm and a visible light transmittance of 0.01% and a refractive index of 1.65 was set on an unwinding roller of a roll-to-roll sputtering apparatus, and film formation conditions of each layer were adjusted when a primer layer and an antireflection layer were sequentially formed on the black PET film by a reactive sputtering method. SiO with a film-forming target thickness of 3.5nm as a primer layer x Layer (x)<2). As an antireflection layer, the 1 st layer was formed by: nb with target thickness of 12nm 2 O 5 Layer (refractive index: 2.33), layer 2: siO with target thickness of 28nm 2 Layer (refractive index: 1.46), layer 3: nb with target thickness of 100nm 2 O 5 Layer, and layer 4: siO with target thickness of 85nm 2 A layer. In forming (film formation) each layer (oxide film), a film is formed while introducing argon gas and oxygen gas into the film formation chamber.
In addition, in the film formation of each of the primer layer and the antireflection layer, the power supply was set to MFAC power supply (frequency: 40 kHz). In the formation of the primer layer, a Si target was used as a target material, and the power density was set to 3W/cm 2 The pressure in the film forming chamber was set to 0.4Pa. In the film formation of the 1 st layer and the 3 rd layer of the antireflection layer, nb target was used to set the power density to 13W/cm 2 The pressure in the film forming chamber was set to 0.5Pa. Si targets were used for the film formation of the 2 nd and 4 th antireflection layers, respectively, and the power density was set at 8W/cm 2 The pressure in the film forming chamber was set to 0.5Pa.
In addition, at the time of forming (film formation) each layer (oxide film), the pressure was kept constant by adjusting the introduction amount of argon gas and the exhaust amount, and the introduction amount of oxygen gas was adjusted by Plasma Emission Monitoring (PEM) control so that the film formation mode maintained the transition region. When the film formation conditions of the respective layers are adjusted, the film thickness calculation and the change of the set value (SP) of the plasma emission intensity are repeated until the film thickness distribution in the width direction of the respective layers becomes an allowable range by adjusting the film thickness by the method described in paragraphs [0124] to [0126] of japanese patent application laid-open No. 2017-218674.
Next, a method for producing the film base material used in examples will be described.
[ production of film base Material ]
(hard coat layer Forming step)
A composition for forming a hard coat layer having a solid content of 45% by weight was prepared by mixing 100 parts by weight of an ultraviolet-curable urethane acrylate monomer (refractive index: 1.51), 14 parts by weight of polystyrene beads (refractive index: 1.59, number-average secondary particle diameter: 3.0 μm), 5 parts by weight of an alkylbenzene ketone photopolymerization initiator, 135 parts by weight of toluene and 10 parts by weight of ethyl acetate. Next, the composition for forming a hard coat layer was applied to one main surface of a TAC film (thickness: 80 μm, refractive index: 1.49) as a transparent film to form a coating film. Then, the coating film was dried by heating at 80℃for 2 minutes, and then cured by irradiation with ultraviolet rays. Thus, an antiglare hard coat layer (hard coat layer having a surface with a concave-convex structure) was formed on one main surface of the TAC film to obtain a hard coat layer-attached transparent film (2 nd protective film).
(step of producing polarizing plate)
A TAC film of the 2 nd protective film was laminated on one principal surface of a separately prepared polarizing material, and a TAC film (thickness: 80 μm, refractive index: 1.49) of the 1 st protective film separately prepared was laminated on the other principal surface of the polarizing material, to prepare a polarizing plate. As the polarizer, a PVA-based polarizer in which a polyvinyl alcohol film having an average polymerization degree of 2700 and a thickness of 75 μm was stretched to 6 times while being iodine-dyed was used. In addition, for the lamination (adhesion) of the PVA-based polarizer and the TAC film, a film prepared by the following weight ratio 3:1 an adhesive comprising an acetoacetyl group-containing polyvinyl alcohol resin (average polymerization degree: 1200, saponification degree: 98.5 mol%, acetoacetylation degree: 5 mol%) and an aqueous solution of methylolmelamine, was bonded by a roll bonding machine, and then heated and dried in an oven.
(step of producing polarizing plate with adhesive layer)
A release liner (a PET film subjected to release treatment with a silicone release agent) having a thickness of 38 μm was separately prepared, an acrylic adhesive was coated on one main surface of the release liner, and then the release liner was dried at 120 ℃ for 2 minutes to form an adhesive layer on one main surface of the release liner. Next, the obtained adhesive layer was bonded to the TAC film of the polarizing plate (specifically, TAC film on the side not in contact with the hard coat layer), to obtain a polarizing plate (film base material) with an adhesive layer. The width of each layer in the resulting film substrate was: release liner: 1317mm, adhesive layer: 1250mm, 1 st protective film: 1330mm, polarizer: 1280mm, protective film 2: 1330mm.
In the obtained film base material, the 1 st protective film and the polarizing material are bonded by the 1 st adhesive layer formed of the cured product of the adhesive, and the 2 nd protective film and the polarizing material are bonded by the 2 nd adhesive layer formed of the cured product of the adhesive. In addition, the 1 st protective film and the 2 nd protective film protrude from both ends of the polarizer in the width direction.
In the obtained film base material, the distance between the 1 st protective film and the 2 nd protective film in the portions protruding from the both ends is smaller than the distance between the 1 st protective film and the 2 nd protective film in the portions sandwiching the ends in the width direction of the polarizing material. The obtained film base material further includes a 3 rd adhesive layer (adhesive layer formed of a cured product of the adhesive) for bonding the 1 st protective film and the 2 nd protective film to each other in a part of the portion extending from the both ends in the width direction. The 3 rd adhesive layer is integrally formed with the 1 st adhesive layer and the 2 nd adhesive layer. The end face in the width direction of the polarizer was sealed with the 3 rd adhesive layer.
(bombardment treatment Process)
The pressure was 0.6Pa and the effective power density was 0.34 W.min/cm by using a roll-to-roll plasma processing apparatus 2 M, the film base material is conveyed and the main surface of the hard coat layer of the film base material (specifically, the main surface of the hard coat layer on the opposite side to the TAC film side) is subjected to bombardment treatment. In the bombardment treatment, argon (flow: 1049 sccm) and oxygen (flow: 1 sccm) were introduced into the apparatus and then treated.
[ formal film formation ]
Next, the main film formation will be described. In the main film formation, the film base material after the bombardment treatment is set on an unwinding roller of a sputtering apparatus of a roll-to-roll type to form the [ prefilming ]]The film-forming conditions adjusted in the step (a) are used as initial film-forming conditions, and SiO is formed on one main surface of the hard coat layer (the main surface of the hard coat layer opposite to the TAC film side) x After the layers, nb is formed in sequence 2 O 5 Layer, siO 2 Layer, nb 2 O 5 Layer and SiO 2 A layer (an antireflection layer forming step), and an on-line reflected light measurement (an on-line reflected light measurement step) of the obtained antireflection layer is performed. The antireflection layer forming step and the in-line reflected light measuring step are continuously performed while the film base material is conveyed in one direction. The on-line reflected light measurement was performed at 23 positions in the width direction of the antireflection layer (width: 1274 mm), and based on the obtained reflected light spectrum, the film thicknesses at the 23 positions in the width direction were calculated, and the set value (SP) of the plasma emission intensity was changed so that the film thicknesses were uniform in the width direction. Thereby, the film forming conditions of the antireflection layer are adjusted. In the case of the main film formation, the on-line reflected light measurement was performed In order to intercept the reflected light from the film base material including the polarizer, a polarizing plate for polarizing the visible light irradiated from the light irradiation unit is disposed.
Comparative example
The film formation conditions of the antireflection layer were adjusted in the same manner as in the above-described examples, except that film substrates obtained by cutting off the both end portions of the 1 st protective film and the 2 nd protective film (specifically, portions extending from both ends in the width direction of the polarizer) were used.
< results >
FIG. 6 is a graph (L) showing the hue of reflected light from the antireflection layer before the film formation condition adjustment (immediately after the initiation of film formation) in the above-described embodiment * a * b * A of the chromaticity System * b * Chromaticity diagram). Fig. 7 is a graph showing the hue of the reflected light from the antireflection layer after the film formation condition adjustment (after 15 feedback operations) in the above example. Fig. 8 is a graph showing the hue of the reflected light from the antireflection layer before the film formation condition adjustment (immediately after the initiation of the main film formation) in the comparative example. Fig. 9 is a graph showing the hue of the reflected light from the antireflection layer after the film formation condition adjustment (after 52 feedback operations) in the comparative example. In fig. 6 to 9, a is drawn for a total of 5 parts, namely, two ends (2 parts), a center (1 part), and a part (2 parts) between the two ends and the center, of the measurement parts (23 parts in the width direction of the antireflection layer) of the reflected light * And b * Is a value of (2). The areas indicated by broken lines in fig. 6 to 9 are areas indicating the allowable range of the hue.
As shown in fig. 7, in the above embodiment, the hue is within the allowable range through 15 feedback operations. On the other hand, as shown in fig. 9, in the above comparative example, even though 52 feedback operations were performed, the hues at both ends (2 sites) were not within the allowable range. As shown in fig. 6 and 8, the above-described examples have smaller variations in hue in the width direction before the film formation condition adjustment (immediately after the initiation of the main film formation) than the above-described comparative examples.
From the above results, it is apparent that the present invention can provide a method for producing a polarizing plate with an antireflection layer, which can maintain the uniformity of the reflected light characteristics.
Claims (10)
1. A method for manufacturing a polarizing plate with an antireflection layer, the polarizing plate with an antireflection layer having a film base material and an antireflection layer provided on one main surface side of the film base material, the method comprising:
a step Sa of forming the antireflection layer formed of at least 2 films on the one main surface side of the film base material, and
a step Sb of irradiating at least one layer constituting the antireflection layer with visible light after the layer is formed, and detecting the reflected light,
The step Sa and the step Sb are continuously performed while the film base material is conveyed in one direction,
the film base material is a laminate having a 1 st protective film, a 1 st adhesive layer, a polarizing element, a 2 nd adhesive layer, and a 2 nd protective film in this order,
the 1 st protective film and the polarizer are bonded by the 1 st adhesive layer,
the 2 nd protective film and the polarizer are bonded by the 2 nd adhesive layer,
the 1 st protective film and the 2 nd protective film are each larger than the width of the polarizing member and protrude from both ends in the width direction of the polarizing member,
the 1 st protective film and the 2 nd protective film are spaced apart at least in a part of the portions protruding from the both ends more than the 1 st protective film and the 2 nd protective film in a portion sandwiching the widthwise end portions of the polarizing member.
2. The method for producing a polarizing plate with an antireflection layer according to claim 1, wherein in the step Sb, after all layers constituting the antireflection layer are formed, the antireflection layer is irradiated with visible light, and the reflected light is detected.
3. The method for manufacturing a polarizing plate with an antireflection layer according to claim 1, wherein a film formation condition of the antireflection layer in the step Sa is adjusted according to a detection result of the reflected light in the step Sb.
4. The method for producing a polarizing plate with an antireflection layer according to claim 1, wherein in the step Sb, a plurality of portions in the width direction of the layer are irradiated with visible light, and reflected light thereof is detected.
5. The method for manufacturing a polarizing plate with an antireflection layer according to claim 1, wherein in the step Sa, the antireflection layer is formed by a sputtering method.
6. The method for producing a polarizing plate with an antireflection layer according to claim 1, wherein the film base material further comprises a 3 rd adhesive layer for adhering the 1 st protective film and the 2 nd protective film to each other in at least a part of a portion extending from the both ends in a width direction.
7. The method for producing a polarizing plate with an antireflection layer according to claim 1, wherein the 2 nd protective film comprises a transparent film and a hard coat layer provided on one principal surface side of the transparent film,
in the step Sa, the antireflection layer is formed on the hard coat layer on the opposite side of the transparent film side.
8. The method for producing a polarizing plate with an antireflection layer according to claim 1, wherein the film base material further comprises an adhesive layer provided on a side of the 1 st protective film opposite to the polarizer side,
In the step Sa, the antireflection layer is formed on the side of the 2 nd protective film opposite to the polarizer side.
9. The method for producing a polarizing plate with an antireflection layer according to claim 8, wherein the film base material further comprises a release liner temporarily adhered to a side of the adhesive layer opposite to the 1 st protective film side.
10. The method for producing a polarizing plate with an antireflection layer according to claim 1, further comprising a step Sc of forming a primer layer on the one principal surface side of the film base material before the step Sa,
in the step Sa, the antireflection layer is formed on the main surface of the primer layer on the opposite side of the film base material side.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2022151163A JP2024046025A (en) | 2022-09-22 | 2022-09-22 | Antireflection layer-attached polarizer manufacturing method |
| JP2022-151163 | 2022-09-22 |
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| Publication Number | Publication Date |
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| CN117741850A true CN117741850A (en) | 2024-03-22 |
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| CN202311223268.7A Pending CN117741850A (en) | 2022-09-22 | 2023-09-20 | Method for manufacturing polarizing plate with anti-reflection layer |
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| Country | Link |
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| JP (1) | JP2024046025A (en) |
| KR (1) | KR20240041223A (en) |
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