TW202246807A - Optical laminate, display device, and method of manufacturing optical laminate - Google Patents
Optical laminate, display device, and method of manufacturing optical laminate Download PDFInfo
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- TW202246807A TW202246807A TW111110370A TW111110370A TW202246807A TW 202246807 A TW202246807 A TW 202246807A TW 111110370 A TW111110370 A TW 111110370A TW 111110370 A TW111110370 A TW 111110370A TW 202246807 A TW202246807 A TW 202246807A
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- film
- hard coat
- coat layer
- optical laminate
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- G02B5/30—Polarising elements
- G02B5/3083—Birefringent or phase retarding 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
- G02B5/3016—Polarising elements involving passive liquid crystal elements
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- 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
- B32B23/00—Layered products comprising a layer of cellulosic plastic substances, i.e. substances obtained by chemical modification of cellulose, e.g. cellulose ethers, cellulose esters, viscose
- B32B23/04—Layered products comprising a layer of cellulosic plastic substances, i.e. substances obtained by chemical modification of cellulose, e.g. cellulose ethers, cellulose esters, viscose comprising such cellulosic plastic substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B23/08—Layered products comprising a layer of cellulosic plastic substances, i.e. substances obtained by chemical modification of cellulose, e.g. cellulose ethers, cellulose esters, viscose comprising such cellulosic plastic substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- 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
- G02B5/3075—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state for use in the UV
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- G—PHYSICS
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- G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
- G09F9/00—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements
- G09F9/30—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements in which the desired character or characters are formed by combining individual elements
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/02—Details
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
-
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
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- B32B2305/55—Liquid crystals
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- 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
- B32B2307/00—Properties of the layers or laminate
- B32B2307/40—Properties of the layers or laminate having particular optical properties
- B32B2307/42—Polarizing, birefringent, filtering
Abstract
Description
本發明係關於光學積層體、圖像顯示裝置、光學積層體之製造方法。 The present invention relates to an optical laminate, an image display device, and a method for manufacturing an optical laminate.
於有機EL顯示裝置等圖像顯示裝置中，係為了抑制外界光反射而使用圓偏光板。圓偏光板為具有偏光膜與相位差層之光學積層體，且貼合於圖像顯示裝置之視認側表面。就相位差層而言，由於光學特性會因紫外線而逐漸劣化，因此已知有以抑制該劣化為目的而使接著層含有紫外線吸收劑之技術(例如專利文獻1)。 In image display devices such as organic EL display devices, circular polarizing plates are used to suppress reflection of external light. The circular polarizing plate is an optical laminate with a polarizing film and a retardation layer, and is attached to the viewing side surface of the image display device. Since the optical properties of the retardation layer gradually deteriorate due to ultraviolet rays, there is known a technique in which an ultraviolet absorber is contained in the adhesive layer for the purpose of suppressing the deterioration (for example, Patent Document 1).
[先前技術文獻] [Prior Art Literature]
[專利文獻] [Patent Document]
[專利文獻1]日本特開2020-3650號公報 [Patent Document 1] Japanese Patent Laid-Open No. 2020-3650
然而，根據本發明者所知，已判明即便應用專利文獻1之技術，於紫外線耐候試驗中光學積層體之面之中央部的色調變化雖被抑制，但於端部(周緣部)有產生色調變化之情形。另一方面，由於顯示裝置之顯示區域之擴大，對於光學積層體端部之顏色變化亦於近年來急速地變得要求嚴格。因此，本發明之目的在於提供一種即便於端部亦不易產生經時之色調變化之光學積層體。本發明之又一目的在於提供一種具備該光學積層體之顯示裝置。又，目的在於提供一種該光學積層體之製造方法。 However, according to the knowledge of the present inventors, it has been found that even if the technology of Patent Document 1 is applied, the change in the color tone of the surface of the optical layered body in the ultraviolet weathering test is suppressed, but the color tone is generated at the end (peripheral part). changing circumstances. On the other hand, due to the enlargement of the display area of the display device, the color change of the end portion of the optical layered body has also become rapidly and strictly required in recent years. Therefore, an object of the present invention is to provide an optical layered body in which a change in color tone over time does not easily occur even at an edge portion. Another object of the present invention is to provide a display device including the optical laminate. Moreover, it aims at providing the manufacturing method of this optical laminated body.
本發明者等係將利用含有紫外線吸收劑之黏著劑貼合偏光膜與相位差層而成之圓偏光板長時間曝露於紫外線(紫外線耐候試驗)，並藉由拉曼分光法對在端部產生色調變化之圓偏光板之剖面進行結構解析，結果判明黏著層之端部之紫外線吸收劑劣化。根據該結果，本發明者等人推測：由於圓偏光板之端面係曝露於光或外部空氣中，故黏著層或接著層中所含之紫外線吸收劑係從接近於端面之側開始劣化，造成特定波長區域(例如390nm至420nm)之穿透率上升，因此端部附近之相位差層之相位差值有所變動而產生外觀上之色調變化。本發明者等人有鑒於此種狀況，發現在包含圓偏光板之光學積層體中可不易產生端部之色調變化之構造，從而完成本發明。 The inventors of the present invention exposed a circular polarizing plate formed by bonding a polarizing film and a retardation layer with an adhesive containing an ultraviolet absorber to ultraviolet rays for a long time (ultraviolet weathering test), and analyzed the polarizing plate at the end by Raman spectroscopy. Structural analysis was performed on the section of the circular polarizing plate that changed the color tone. As a result, it was found that the ultraviolet absorber at the end of the adhesive layer deteriorated. Based on the results, the present inventors speculate that since the end face of the circular polarizing plate is exposed to light or outside air, the ultraviolet absorber contained in the adhesive layer or the adhesive layer starts to deteriorate from the side close to the end face, resulting in The transmittance of a specific wavelength region (for example, 390nm to 420nm) increases, so the retardation value of the retardation layer near the end changes, resulting in an apparent change in color tone. In view of such circumstances, the inventors of the present invention found a structure in which color tone changes at the ends are less likely to occur in an optical layered body including a circular polarizing plate, and completed the present invention.
本發明提供一種光學積層體，其係具有硬塗層、透明樹脂膜、偏光膜及相位差膜者，其中，硬塗層、透明樹脂膜及偏光膜係以於光學積 層體之使用時較相位差膜更朝向視認側之方式配置，硬塗層係含有紫外線吸收劑，相位差膜係包含聚合性液晶化合物所聚合而成之硬化物。 The present invention provides an optical laminate, which has a hard coat layer, a transparent resin film, a polarizing film and a retardation film, wherein the hard coat layer, the transparent resin film and the polarizing film are used on the optical product The layers are arranged so that they face the viewing side more than the retardation film. The hard coat layer contains an ultraviolet absorber, and the retardation film contains a cured product polymerized from a polymerizable liquid crystal compound.
硬塗層對於波長400nm的光之吸光度可為1.0至4.1，對於波長410nm的光之吸光度可為0.7至3.0。又，硬塗層亦可為於波長380nm至420nm之範圍內具有吸收最大譜峰者。又，硬塗層之厚度亦可為2μm至7μm。又，硬塗層亦可為鉛筆硬度在7B至B之範圍。又，硬塗層之壓痕彈性模數亦可為1000MPa至4000MPa。 The absorbance of the hard coating layer for light with a wavelength of 400 nm may be 1.0 to 4.1, and the absorbance for light with a wavelength of 410 nm may be 0.7 to 3.0. Also, the hard coat layer may have an absorption maximum peak in the wavelength range of 380nm to 420nm. In addition, the thickness of the hard coat layer may be 2 μm to 7 μm. Also, the hard coat layer may have a pencil hardness in the range of 7B to B. Also, the indentation elastic modulus of the hard coat layer may be 1000 MPa to 4000 MPa.
相位差膜亦可為顯示逆波長分散性者。 The retardation film may also show reverse wavelength dispersion.
於本發明之光學積層體中，透明樹脂膜係包含環烯烴系樹脂，硬塗層亦可直接積層於透明樹脂膜上。 In the optical laminate of the present invention, the transparent resin film contains cycloolefin-based resin, and the hard coat layer may be directly laminated on the transparent resin film.
本發明之光學積層體亦可依序積層硬塗層、透明樹脂膜、偏光膜、相位差膜。 The optical layered body of the present invention may also be laminated sequentially with a hard coat layer, a transparent resin film, a polarizing film, and a retardation film.
又，本發明提供一種具備上述光學積層體之顯示裝置。 Also, the present invention provides a display device including the above-mentioned optical layered body.
又，本發明提供一種光學積層體之製造方法，其係具有：積層膜準備步驟，係準備具備硬塗層及透明樹脂膜之積層膜；及貼合步驟，其係分別於偏光膜之兩面中之一側貼合積層膜，並於另一側貼合相位差膜、或是經由保護膜而貼合相位差膜；其中，硬塗層係含有紫外線吸收劑者，相位差膜係包含聚合性液晶化合物所聚合而成之硬化物者。 Also, the present invention provides a method for manufacturing an optical laminate, which comprises: a laminated film preparation step of preparing a laminated film with a hard coat layer and a transparent resin film; A laminated film is pasted on one side, and a retardation film is pasted on the other side, or a retardation film is pasted through a protective film; wherein, the hard coat layer contains an ultraviolet absorber, and the retardation film contains a polymerizable The cured product formed by the polymerization of liquid crystal compounds.
於該製造方法中，積層膜準備步驟亦可包含：從於積層膜之任一面積層有支撐膜之貼合膜將支撐膜剝離。 In this manufacturing method, the step of preparing the laminated film may also include: peeling the support film from the bonding film on which the support film is layered on any one surface of the laminated film.
於該製造方法中，支撐膜亦可為包含聚對苯二甲酸乙二酯系樹脂或聚烯烴之膜。 In this production method, the support film may be a film made of polyethylene terephthalate-based resin or polyolefin.
根據本發明，可提供一種即便於端部亦不易產生經時之色調變化之光學積層體。又，可提供一種具備該光學積層體之顯示裝置。又，可提供該光學積層體之製造方法。 According to the present invention, it is possible to provide an optical layered body in which a change in color tone over time does not easily occur even at an edge portion. Moreover, a display device including the optical layered body can be provided. Moreover, the manufacturing method of this optical laminated body can be provided.
1:光學積層體 1: Optical laminate
2:相位差膜 2: Retardation film
2A:第1相位差層 2A: The first retardation layer
2B:第2相位差層 2B: The second retardation layer
2B:相位差層 2B: Retardation layer
3:直線偏光板 3: Linear polarizer
4:黏著層 4: Adhesive layer
5:剝離膜 5: Peel off film
6:偏光膜 6: Polarizing film
7:保護膜 7: Protective film
8:透明樹脂膜 8: Transparent resin film
9:硬塗層 9: Hard coating
50:試驗體之端部 50: The end of the test body
51:劣化區域 51:Deteriorated area
52:正常區域 52: normal area
圖1係本實施形態之光學積層體之剖面圖。 Fig. 1 is a cross-sectional view of an optical laminate of this embodiment.
圖2係表示試驗體於光學顯微鏡下的觀察圖像之圖。 Fig. 2 is a diagram showing observation images of a test body under an optical microscope.
圖3係表示將試驗體之觀察圖像轉換為黑白256灰階之資料之圖。 Fig. 3 is a diagram showing the data obtained by converting the observation image of the test object into black and white 256 grayscale.
以下，參照圖式詳細說明本發明之較佳實施形態。 Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the drawings.
<光學積層體> <Optical laminate>
如圖1所示，本實施形態之光學積層體1係相位差膜2與直線偏光板3經由黏著層4而積層而成之圓偏光板。於相位差膜2之外側面係具備用以貼合於顯示裝置之黏著層(未具圖示)、及具有保護該黏著層等功能之剝離膜5。相位差膜2係具備第1相位差層2A與第2相位差層2B(該等第1相位差層2A與第2相位差層2B亦可經由黏著層或接著層而貼附)。直線偏光板3係具備：偏光膜6、經由接著層而積層於其一面之保護膜7、經由接著層而積層於其另一面之透明樹脂膜8、及形成於透明樹脂膜8上之硬塗層9。再者，雖未具圖示，但亦可於第1相位差層2A與黏著層4之間、
及於第2相位差層2B與剝離膜5之間具備下述定向膜(水平定向膜、垂直定向膜)，亦可於第1相位差層2A與第2相位差層2B之間具備接著劑(接著層)等。又，關於偏光膜6與保護膜7或透明樹脂膜8之間任意存在之接著層，於圖1中亦未具圖示。
As shown in FIG. 1 , the optical laminate 1 of this embodiment is a circular polarizing plate in which a
光學積層體1於貼附於顯示裝置時，硬塗層9側係成為視認側。亦即，硬塗層9、透明樹脂膜8及偏光膜6係以於使用光學積層體1時較相位差膜2更朝向視認側之方式配置。
When the optical layered body 1 is attached to a display device, the side of the hard coat layer 9 becomes the viewing side. That is, the hard-coat layer 9, the transparent resin film 8, and the polarizing
[偏光膜] [Polarizing film]
偏光膜6係吸附有具有吸收異向性之碘等二色性色素之延伸膜，材料可列舉聚乙烯醇。又，偏光膜6亦可為塗佈包含二色性色素與聚合性液晶化合物之組成物並使其硬化而獲得者，亦即，亦可為於聚合性液晶化合物之硬化層中定向有二色性色素而成者。偏光膜6亦可為塗佈包含具有液晶性的二色性色素之組成物並使其硬化而獲得者。偏光膜6之厚度可為1μm至40μm，較佳為5μm至20μm。
The polarizing
[保護膜] [protective film]
保護膜7係物理性保護偏光膜6之層。構成材料並無特別限制，例如：包含多官能丙烯酸酯(甲基丙烯酸酯)、丙烯酸胺酯酯、丙烯酸聚酯酯、環氧丙烯酸酯等之丙烯酸系低聚物或聚合物；較佳為由含有聚乙烯醇、乙烯-乙烯醇共聚物、聚乙烯吡咯啶酮、澱粉類、甲基纖維素、羧甲基纖維素、藻酸鈉等水溶性聚合物與溶劑之保護層形成用組成物所形成。又，作為構成材料，可列舉：聚對苯二甲酸乙二酯或聚萘二甲酸乙二酯等聚酯系聚合物、二乙醯纖維素或三乙醯纖維素等纖維素系聚合物、聚甲基丙烯酸甲酯等丙
烯酸系聚合物、聚苯乙烯或丙烯腈-苯乙烯共聚物(AS樹脂)等苯乙烯系聚合物、聚碳酸酯系聚合物等。此外，可列舉聚乙烯、聚丙烯、具有環系或降冰片烯結構之聚烯烴、乙烯-丙烯共聚物等聚烯烴系聚合物。保護膜7之厚度較佳為0.1μm至40μm，更佳為0.5μm至35μm，又更佳為1μm至30μm。
The protective film 7 is a layer that physically protects the
[透明樹脂膜] [Transparent resin film]
透明樹脂膜8係物理性保護偏光膜6之層，亦可實質上與保護膜7相同。作為構成材料，較佳為包含環烯烴系樹脂。環烯烴系樹脂大多係使膜厚相對較厚地使用，於該情形時，透明樹脂膜之剖面曝露於光或外部空氣之面積變大。因此，透明樹脂膜8之厚度較佳為10μm至30μm。就偏光板之薄型化、及防止彎折時之破裂之觀點而言，透明樹脂膜8之厚度更佳為10μm至26μm，又更佳為12μm至23μm。薄的透明樹脂膜係難以將其以單體搬運，而必須貼合作為支撐基材之保護膜。於自此種積層體剝離保護膜時，由於透明樹脂膜之剛性不足，故而存在產生皺折或破損之情況。
The transparent resin film 8 is a layer that physically protects the
透明樹脂膜可為未延伸膜，亦可為延伸膜。相較於延伸膜，未延伸膜係有彈性模數較低之傾向。因此，相較於延伸膜，未延伸膜係容易產生後述的貼附等不良情況。於使用未延伸膜之情形時，為了避免該等不良情況，較佳為貼合成為支持基材之保護膜。 The transparent resin film may be an unstretched film or a stretched film. Unstretched films tend to have a lower modulus of elasticity than stretched films. Therefore, compared with stretched films, unstretched films are more likely to have problems such as sticking, which will be described later. In the case of using an unstretched film, in order to avoid these disadvantages, it is preferable to bond a protective film as a support base material.
[黏著層] [adhesive layer]
偏光膜6與透明樹脂膜8係經由接著層而積層。形成接著層之接著劑可列舉：環氧樹脂；和丙烯醯胺、丙烯酸酯、丙烯酸胺酯酯、環氧丙烯酸酯等丙烯酸系樹脂；和聚乙烯醇系之水系接著劑。其中，較佳為紫外線硬
化型接著劑。再者，雖未具圖示，但偏光膜6與保護膜7、偏光膜6與透明樹脂膜8亦經由接著層而積層。
The
[硬塗層] [hard coat]
硬塗層9係為了提高直線偏光板3之表面的硬度及耐刮性而設置。於本實施形態中，硬塗層9中含有紫外線吸收劑。硬塗層9例如為紫外線硬化型樹脂之硬化層。作為紫外線硬化型樹脂，例如可列舉：丙烯酸系樹脂、聚矽氧系樹脂、聚酯系樹脂、胺酯系樹脂、醯胺系樹脂、環氧系樹脂等。該等之中，紫外線硬化型樹脂較佳為於分子間交聯而硬化者。藉由交聯，紫外線吸收劑可適度地分散。硬塗層9較佳為直接積層於透明樹脂膜8。
The hard coat layer 9 is provided to improve the hardness and scratch resistance of the surface of the
作為硬塗層9所含有之紫外線吸收劑，可列舉：受阻胺系光穩定劑(HALS)、二苯甲酮系、苯并三唑系、苯甲酸酯系等化合物。相對於硬塗層之構成樹脂100質量份，紫外線吸收劑之含量較佳為1質量份至30質量份。為了使硬塗層之厚度變薄，相對於硬塗層之構成樹脂100質量份，紫外線吸收劑之含量尤佳係以設為5質量份至20質量份。 Examples of the ultraviolet absorber contained in the hard coat layer 9 include compounds such as hindered amine-based light stabilizers (HALS), benzophenone-based, benzotriazole-based, and benzoate-based compounds. The content of the ultraviolet absorber is preferably from 1 part by mass to 30 parts by mass relative to 100 parts by mass of the resin constituting the hard coat layer. In order to make the thickness of the hard coat layer thin, the content of the ultraviolet absorber is preferably 5 to 20 parts by mass with respect to 100 parts by mass of the constituent resin of the hard coat layer.
含有紫外線吸收劑之結果係以硬塗層9對於波長400nm的光之吸光度為1.0至4.1為較佳。又，含有紫外線吸收劑之結果係以硬塗層9較佳為對波長410nm的光之吸光度為0.7至3.0為較佳。又，含有紫外線吸收劑之結果係以硬塗層9於波長380nm至420nm之範圍內具有最大吸收為較佳。 As a result of containing the ultraviolet absorber, the absorbance of the hard coat layer 9 for light with a wavelength of 400 nm is preferably 1.0 to 4.1. Also, as a result of containing the ultraviolet absorber, the hard coat layer 9 preferably has an absorbance of 0.7 to 3.0 for light with a wavelength of 410 nm. In addition, as a result of containing the ultraviolet absorber, it is preferable that the hard coat layer 9 has the maximum absorption in the wavelength range of 380nm to 420nm.
為了進一步提高強度，硬塗層9亦可包含添加劑。添加劑並無限定，可列舉無機系微粒子、有機系微粒子、或該等之混合物。另外，硬塗層的厚度可為1μm至20μm，亦可為2μm至7μm。就抑制端部的顏色 變化的觀點而言，硬塗層的厚度較佳為設為3μm至5μm。於製造硬塗層9時，為了在使紫外線硬化型樹脂硬化時確實地硬化至硬塗層深部並提高與基材之密接性，較佳係厚度為7μm以下。因此，透明樹脂膜8與硬塗層9之合計厚度較佳為12至33μm之範圍，又更佳為16至28μm之範圍。 In order to further increase the strength, the hard coat layer 9 may also contain additives. The additive is not limited, and examples thereof include inorganic fine particles, organic fine particles, or mixtures thereof. In addition, the thickness of the hard coat layer may be 1 μm to 20 μm, or may be 2 μm to 7 μm. just suppress the color at the end From the viewpoint of variation, the thickness of the hard coat layer is preferably set at 3 μm to 5 μm. When the hard coat layer 9 is produced, the thickness is preferably 7 μm or less in order to securely harden the ultraviolet curable resin deep into the hard coat layer and improve the adhesion to the base material. Therefore, the total thickness of the transparent resin film 8 and the hard coat layer 9 is preferably in the range of 12 to 33 μm, and more preferably in the range of 16 to 28 μm.
硬塗層9之壓痕彈性模數較佳為1000MPa至4000MPa。壓痕彈性模數更佳為1500MPa至3500MPa，又更佳為2500MPa至3200MPa。若硬塗層9之壓痕彈性模數為1500MPa以上，則不易產生捲取時之變形或源自保護膜之凹凸轉印，因此預先貼合保護膜之必要性變小。另一方面，若壓痕彈性模數為4000MPa以下，則於網膜(web)之搬運或保護膜之剝離時、及彎折試驗時，硬塗層不易產生破裂，故而較佳。此處，「壓痕彈性模數」係指作為於一片透明樹脂膜上之六處測定之平均值而求出之值。將透明樹脂膜經由黏著劑貼附於玻璃板，並於透明樹脂膜上假設有一邊為20mm之兩個正方形呈共用一邊而相鄰之形狀，且於該等正方形之6個頂點之位置測定壓痕彈性模數。正方形相鄰之方向係例如為透明樹脂膜製造時之TD方向。將施加1mN之荷重5秒鐘時之值作為壓痕彈性模數之值，求出六點之平均。測定機器可列舉Fischer Instruments製造之「超微小硬度計HM2000」。 The indentation elastic modulus of the hard coat layer 9 is preferably 1000 MPa to 4000 MPa. The indentation elastic modulus is more preferably from 1500 MPa to 3500 MPa, and more preferably from 2500 MPa to 3200 MPa. If the indentation elastic modulus of the hard coat layer 9 is 1500 MPa or more, deformation during winding or uneven transfer from the protective film is unlikely to occur, so the necessity of pre-attaching the protective film is reduced. On the other hand, if the indentation elastic modulus is 4000 MPa or less, the hard coat layer is less likely to be cracked during web transport, protective film peeling, and bending test, which is preferable. Here, the "indentation elastic modulus" refers to a value obtained as an average value of six measurements on one transparent resin film. Attach the transparent resin film to the glass plate through an adhesive, and assume that there are two squares with a side of 20mm on the transparent resin film that share one side and are adjacent to each other, and measure the pressure at the positions of the six vertices of these squares modulus of elasticity. The direction in which the squares are adjacent is, for example, the TD direction when the transparent resin film is produced. The value obtained when a load of 1 mN was applied for 5 seconds was used as the value of the indentation elastic modulus, and the average of six points was obtained. As a measuring machine, "ultramicro hardness tester HM2000" manufactured by Fischer Instruments may be mentioned.
硬塗層9較佳為鉛筆硬度為7B至B範圍，更佳為6B至2B，又更佳為5B至3B之範圍。藉由鉛筆硬度硬至7B以上，不易產生捲取時之變形或源自保護膜之凹凸轉印，因此預先貼合保護膜之必要性變小。另一方面，藉由鉛筆硬度軟於B以下，於網膜之搬運或保護膜之剝離時、及彎折試驗時，不易產生硬塗層之破裂，故而較佳。 The hard coat layer 9 preferably has a pencil hardness in the range of 7B to B, more preferably in the range of 6B to 2B, and more preferably in the range of 5B to 3B. Since the pencil hardness is hardened to 7B or more, it is difficult to cause deformation during winding or uneven transfer from the protective film, so the necessity of pre-attaching the protective film is reduced. On the other hand, since the pencil hardness is softer than B, cracking of the hard coat layer is less likely to occur during the transfer of the omentum, the peeling of the protective film, and the bending test, so it is preferable.
硬塗層9之耐擦傷性較佳為A’至D範圍，更佳為B至D，又更佳為C至D之範圍。藉由耐擦傷性為D以上，不易產生捲取時的變形或源自保護膜的凹凸轉印，因此預先貼合保護膜的必要性變小。另一方面，藉由耐擦傷性為A’以下，於網膜之搬運或保護膜之剝離時、及彎折試驗時，不易產生硬塗層之破裂，故而較佳。 The scratch resistance of the hard coat layer 9 is preferably in the range of A' to D, more preferably in the range of B to D, and more preferably in the range of C to D. When the scratch resistance is D or more, deformation during winding and unevenness transfer from the protective film are less likely to occur, so the need for attaching the protective film in advance is reduced. On the other hand, since the scratch resistance is A' or less, cracking of the hard coat layer is less likely to occur during the transportation of the omentum, the peeling of the protective film, and the bending test, which is preferable.
於附硬塗層之透明樹脂膜中，尤其是於硬塗層之鉛筆硬度較低之情形或透明樹脂膜8之厚度較小之情形時，係有因製造後之捲取時滑動性之惡化而產生貼附(沾黏)之不良情況。尤其，於硬塗層中含有紫外線吸收劑之情形時，由於容易阻礙紫外線硬化，故而硬塗層之鉛筆硬度會變低，而該傾向變得顯著。若產生貼附，則膜之平面性會受損，故於偏光板表面產生凹凸而品質降低。因此，藉由在製造步驟中於附硬塗層之透明樹脂膜之任一面設置表面保護膜，可防止因捲取時之貼附所導致之外觀不良。又，偏光板於製造過程中係能夠藉由一邊剝離其表面保護膜，一邊與偏光膜貼合，以兼顧品質與生產性。 In the transparent resin film with a hard coat layer, especially when the pencil hardness of the hard coat layer is low or the thickness of the transparent resin film 8 is small, there is a deterioration in sliding properties during winding after manufacture. And produce the adverse situation of sticking (sticking). In particular, when an ultraviolet absorber is contained in the hard coat layer, since ultraviolet curing is easily inhibited, the pencil hardness of the hard coat layer becomes low, and this tendency becomes remarkable. If sticking occurs, the planarity of the film will be impaired, and thus unevenness will be generated on the surface of the polarizing plate, resulting in a decrease in quality. Therefore, by providing a surface protective film on either side of the hard-coated transparent resin film in the manufacturing process, it is possible to prevent appearance defects due to sticking at the time of winding. In addition, the polarizing plate can be bonded to the polarizing film while peeling off the surface protection film during the manufacturing process, so as to balance quality and productivity.
硬塗層9之表面粗糙度較佳為0.010nm至0.030nm。 The surface roughness of the hard coat layer 9 is preferably 0.010 nm to 0.030 nm.
[相位差膜] [Retardation film]
相位差膜2可為包含一層者，亦可為包含複數層者。於本實施形態中，相位差膜2係包含第1相位差層2A與第2相位差層2B。相位差膜2可為包含一層者，亦可為包含複數層者，較佳為相位差膜2整體顯示逆波長分散性之光學特性者。
The
(第1相位差層) (1st retardation layer)
第1相位差層2A係至少具有面內方向之相位差之層。第1相位差層2A較佳為於膜平面內具有折射率各向異性，較佳為具有經單軸定向之正折射率各向異性。亦即，於將面內之折射率成為最大之方向之折射率設為nx，將於該面內與該方向正交之方向之折射率設為ny，將厚度方向之折射率設為nz時，較佳為滿足nx>ny≒nz(正A板)。藉此，可抑制因視角之變化而產生之基於偏光元件之軸變化的對比度之降低，從而可改善色偏。ny≒nz除了包含ny與nz完全相等之情形以外，亦包含ny與nz實質上相等(其差為0.01以內)之情形。
The
第1相位差層2A可為由作為上述保護膜7之構成材料而例示之樹脂所獲得之延伸膜或包含聚合性液晶化合物之組成物之聚合物。第1相位差層2A較佳為由包含聚合性液晶化合物之組成物之聚合物(硬化物)形成。聚合性液晶化合物係具有聚合性官能基、尤其是光聚合性官能基之液晶化合物。所謂光聚合性官能基，是指能夠藉由自光聚合起始劑產生的活性自由基或酸等而參與聚合反應的基。作為光聚合性官能基，可列舉：乙烯基、乙烯氧基、1-氯乙烯基、異丙烯基、4-乙烯基苯基、丙烯醯氧基、甲基丙烯醯氧基、氧雜環丙烷基、氧雜環丁基等。其中，較佳為丙烯醯氧基、甲基丙烯醯氧基、乙烯氧基、氧雜環丙烷基及氧雜環丁基，更佳為丙烯醯氧基。液晶性可為熱致性液晶，亦可為溶致性液晶，作為相序結構，可為向列型液晶，亦可為層列型液晶。
The
就光學積層體1之薄膜化之觀點而言，第1相位差層2A之膜厚較佳為5μm以下，更佳為3μm以下，又更佳為2.5μm以下。又，第
1相位差層2A之膜厚之下限較佳為0.1μm以上，更佳為0.5μm以上，又更佳為1.0μm以上。
From the viewpoint of thinning the optical layered body 1 , the film thickness of the
(第2相位差層) (2nd retardation layer)
第2相位差層2B係至少具有厚度方向之相位差之層。第2相位差層2B較佳係於相對於膜平面為垂直之方向具有折射率各向異性，較佳為具有經單軸定向之正折射率各向異性。亦即，於將面內之折射率成為最大之方向之折射率設為nx，將於該面內與該方向正交之方向之折射率設為ny，將厚度方向之折射率設為nz時，上述第2相位差層較佳為滿足nz>nx≒ny(正C板)。nx≒ny除了包含nx與ny完全相等之情形以外，還包含nx與ny為實質上相等(其差為0.01以內)之情形。作為具體例，可列舉棒狀液晶化合物。
The
作為第2相位差層2B之構成材料可應用棒狀液晶化合物或圓盤狀液晶化合物、或該等之混合物，尤佳為棒狀液晶化合物。作為棒狀液晶化合物之具體例，例如可較佳地使用日本特表平11-513019號公報之請求項1、或日本特開2005-289980號公報之段落[0026]至[0098]所記載者。作為圓盤狀液晶化合物，例如可較佳地使用日本特開2007-108732號公報的段落[0020]至段落[0067]、或日本特開2010-244038號公報的段落[0013]至段落[0108]中所記載者。
A rod-shaped liquid crystal compound, a discotic liquid crystal compound, or a mixture thereof can be used as a constituent material of the
就光學積層體1之薄膜化之觀點而言，第2相位差層2B之膜厚較佳為3μm以下，更佳為2μm以下，又更佳為1.5μm以下。又，第2相位差層2B之膜厚之下限較佳為0.1μm以上，更佳為0.3μm以上，又更佳為0.5μm以上。
From the viewpoint of reducing the thickness of the optical layered body 1 , the film thickness of the
(相位差層之形成方法及定向膜) (Formation method of retardation layer and alignment film)
為了形成第1相位差層2A及第2相位差層2B，亦可準備定向膜(定向膜於圖1中未具圖示)。一般而言，定向膜係具有使構成相位差層之聚合性液晶化合物定向於特定方向之定向限制力之膜。另外，根據定向膜的種類、摩擦條件或光照射條件，可以控制垂直定向、水平定向、混合定向及傾斜定向等各種定向。水平定向膜係具有使構成相位差層之聚合性液晶化合物於水平方向定向之定向限制力之定向膜，垂直定向膜係具有使構成相位差層之聚合性液晶化合物於垂直方向定向之定向限制力之定向膜。
In order to form the
作為定向膜之構成材料，例如可列舉：具有醯胺鍵之聚醯胺和明膠類、具有醯亞胺鍵之聚醯亞胺及其水解物之聚醯胺酸、聚乙烯醇、烷基改性聚乙烯醇、聚丙烯醯胺、聚噁唑、聚乙烯亞胺、聚苯乙烯、聚乙烯吡咯啶酮、聚丙烯酸及聚丙烯酸酯類。作為(甲基)丙烯酸酯系單體，可例示如：丙烯酸2-乙基己酯、丙烯酸環己酯、二乙二醇單2-乙基己醚丙烯酸酯、二乙二醇單苯醚丙烯酸酯、四乙二醇單苯醚丙烯酸酯、三羥甲基丙烷三丙烯酸酯、丙烯酸月桂酯、甲基丙烯酸月桂酯、丙烯酸異冰片酯甲基丙烯酸異冰片酯、丙烯酸2-苯氧基乙酯、丙烯酸四氫糠酯、丙烯酸2-羥基丙酯、丙烯酸苄酯、甲基丙烯酸四氫糠酯、甲基丙烯酸2-羥基乙酯、甲基丙烯酸苄酯、甲基丙烯酸環己酯、甲基丙烯酸、丙烯酸胺酯酯等。該等材料可單獨使用或組合兩種以上使用。 As the constituent material of the alignment film, for example, polyamide having an amide bond and gelatin, polyimide having an amide bond and polyamic acid of its hydrolyzate, polyvinyl alcohol, alkyl modified Polyvinyl alcohol, polyacrylamide, polyoxazole, polyethyleneimine, polystyrene, polyvinylpyrrolidone, polyacrylic acid and polyacrylates. Examples of (meth)acrylate-based monomers include: 2-ethylhexyl acrylate, cyclohexyl acrylate, diethylene glycol mono-2-ethylhexyl ether acrylate, diethylene glycol monophenyl ether acrylic acid ester, tetraethylene glycol monophenyl ether acrylate, trimethylolpropane triacrylate, lauryl acrylate, lauryl methacrylate, isobornyl acrylate, isobornyl methacrylate, 2-phenoxyethyl acrylate , tetrahydrofurfuryl acrylate, 2-hydroxypropyl acrylate, benzyl acrylate, tetrahydrofurfuryl methacrylate, 2-hydroxyethyl methacrylate, benzyl methacrylate, cyclohexyl methacrylate, methyl Acrylic, urethane acrylate, etc. These materials can be used individually or in combination of 2 or more types.
就薄膜化之觀點而言，定向膜之膜厚較佳為1μm以下，更佳為0.5μm以下，又更佳為0.3μm以下。定向膜之厚度之上限並無限定，但因為於以亦包含定向膜之構成將相位差層自基材轉印之情形，會變得容易 穩定實施將相位差層自基材剝離並轉印，因此有故意使定向膜變厚之情形。作為該情形時之定向膜之膜厚，較佳為5μm以下，更佳為3μm以下。 From the viewpoint of thinning, the film thickness of the alignment film is preferably 1 μm or less, more preferably 0.5 μm or less, still more preferably 0.3 μm or less. The upper limit of the thickness of the alignment film is not limited, but in the case of transferring the retardation layer from the substrate in a configuration that also includes the alignment film, it becomes easy Since the phase difference layer is peeled from the base material and transferred in a stable manner, the alignment film may be thickened on purpose. In this case, the film thickness of the alignment film is preferably 5 μm or less, more preferably 3 μm or less.
定向膜係形成於基材膜上。作為構成基材膜之樹脂，例如可列舉：聚乙烯、聚丙烯、降冰片烯系聚合物等聚烯烴；環狀烯烴系樹脂；聚乙烯醇；聚對苯二甲酸乙二酯；聚甲基丙烯酸酯；聚丙烯酸酯；三乙醯纖維素、二乙醯纖維素及纖維素乙酸酯丙酸酯等纖維素酯；聚萘二甲酸乙二酯；聚碳酸酯；聚碸；聚醚碸；聚醚酮；聚苯硫醚及聚伸苯醚等塑膠。可為對該基材表面實施如聚矽氧處理之脫模處理而成者。 The alignment film is formed on the base film. Examples of the resin constituting the base film include polyolefins such as polyethylene, polypropylene, and norbornene-based polymers; cyclic olefin-based resins; polyvinyl alcohol; polyethylene terephthalate; Acrylates; Polyacrylates; Cellulose esters such as triacetyl cellulose, diacetyl cellulose, and cellulose acetate propionate; Polyethylene naphthalate; Polycarbonate; Polyethylene; Polyether cellulose ; Polyether ketone; polyphenylene sulfide and polyphenylene ether and other plastics. It may be obtained by subjecting the surface of the substrate to release treatment such as silicone treatment.
基材較佳為容易積層定向膜且容易剝離之厚度。此種基材之厚度通常為5至300μm，較佳為20至200μm。 The base material is preferably of a thickness that is easy to laminate an alignment film and to be easily peeled off. The thickness of such a substrate is usually 5 to 300 μm, preferably 20 to 200 μm.
於所形成之定向膜上形成相位差層。於本實施形態中，係分別於水平定向膜上形成第1相位差層2A、於垂直定向膜上形成第2相位差層2B。分別可將包含聚合性液晶化合物之相位差層形成用組成物塗佈於定向膜上，繼而去除溶劑，並藉由加熱及/或活性能量射線使包含定向狀態之聚合性液晶化合物之相位差層形成用組成物硬化而獲得。
A retardation layer is formed on the formed alignment film. In this embodiment, the
根據所選擇之定向膜之種類和聚合性液晶化合物之種類，所形成之相位差層係成為具有正波長分散性之正A板，或成為具有逆波長分散性之正C板。尤其，藉由使複數個聚合性液晶化合物之混合比改變，可調整相位差層之波長分散性。 Depending on the type of alignment film and the type of polymerizable liquid crystal compound selected, the formed retardation layer is a positive A plate with positive wavelength dispersion, or a positive C plate with reverse wavelength dispersion. In particular, the wavelength dispersion of the retardation layer can be adjusted by changing the mixing ratio of the plurality of polymerizable liquid crystal compounds.
以紫外線硬化型接著劑將所形成之第1相位差層2A與第2相位差層彼此貼合，藉此成為相位差層之積層體，亦即相位差膜2。再者，
紫外線硬化型之接著劑之層並未示於圖1。相位差膜2之第1相位差層2A側係朝向直線偏光板3側。
The formed
[黏著層] [adhesive layer]
直線偏光板3與相位差膜2係經由黏著層4而積層。構成黏著層4之黏著劑係藉由將其本身貼附於光學膜或液晶層等被黏著體而表現接著性者，即所謂之被稱為感壓型接著劑(pressure sensitive adhesive，PSA)者。作為黏著劑，可無特別限制地使用過往周知之光學透明性優異之黏著劑，例如可使用具有丙烯酸系、胺酯酯系、聚矽氧系、聚乙烯醚系等基礎聚合物之黏著劑。黏著層之厚度可為3μm以上，亦可為5μm以上，又，可為35μm以下，亦可為30μm以下。
The
黏著層4亦可含有使用離子性化合物等之抗靜電劑、溶劑、交聯觸媒、黏著賦予樹脂(增黏劑)、塑化劑、軟化劑、染料、顏料、無機填料等添加劑。
The
[剝離膜] [Peel film]
於相位差膜2之第2相位差層2B側積層有黏著層，於黏著面貼合有剝離膜5。
An adhesive layer is laminated on the
[顯示裝置] [display device]
光學積層體1可應用於液晶顯示裝置或有機EL顯示裝置等顯示裝置。特別是適用於具有窄幅邊框之中小型有機EL顯示裝置。 The optical layered body 1 can be applied to a display device such as a liquid crystal display device or an organic EL display device. In particular, it is suitable for medium and small-sized organic EL display devices with narrow borders.
[效果] [Effect]
本實施形態之光學積層體1即便長時間曝露於紫外線(紫外線耐候試驗)，亦不易於端部(周緣部)產生色調變化。先前之光學積層體會由於曝露 於光或外部空氣而相位差性能劣化。咸認先前之光學積層體係於接著層或黏著層含有紫外線吸收劑，而保護相位差膜免於劣化用之紫外線吸收劑容易劣化。相對於此，本實施形態之光學積層體1中係於硬塗層含有紫外線吸收劑。尤其，當硬塗層為交聯性的樹脂之情形時，紫外線吸收劑會適度地分散，且紫外線吸收劑不易劣化。又，一般而言，硬塗層多形成為厚度薄於保護膜或黏著層，於厚度較薄之情形時，曝露於外部空氣中之部分小而尤其不易進行從端部開始之劣化。 Even if the optical layered body 1 of this embodiment is exposed to ultraviolet rays for a long time (ultraviolet weather resistance test), it is not easy to change the color tone of the edge part (periphery part). Previous optical laminate experience due to exposure Retardation performance degrades due to exposure to light or outside air. It is believed that the conventional optical lamination system contains ultraviolet absorbers in the adhesive layer or adhesive layer, and the ultraviolet absorbers used to protect the retardation film from deterioration tend to deteriorate. On the other hand, in the optical layered body 1 of this embodiment, the hard-coat layer contains an ultraviolet absorber. In particular, when the hard coat layer is a crosslinkable resin, the ultraviolet absorber is moderately dispersed, and the ultraviolet absorber is less likely to deteriorate. Also, generally speaking, the hard coat layer is often formed thinner than the protective film or adhesive layer. When the thickness is thinner, the portion exposed to the outside air is small, and it is particularly difficult to deteriorate from the edge.
此處，屬於相位差能力之劣化的指標之色調變化(色相變化)係根據從光學積層體1之端部(邊)開始的變色係深入進行至何種程度而評估。該觀察可使用光學顯微鏡進行。變色之進行程度越小，亦即朝向光學積層體1之中心部之變色之深度的距離越小，則可謂之為劣化範圍越窄而耐候性優異。將劣化之程度進行定量之方法可列舉如下方法：拍攝用光學顯微鏡所觀察到之影像，以灰階呈像，並將劣化部分與正常部分之灰階之中間處視為劣化部分之端點，測定從光學積層體1之端部(邊)起至該端點為止之距離。 Here, the color tone change (hue change) which is an index of deterioration of retardation capability is evaluated by how deeply the color change from the edge (side) of the optical layered body 1 progresses. This observation can be performed using an optical microscope. The smaller the progress of discoloration, that is, the smaller the distance of the depth of discoloration toward the center of the optical layered body 1 , the narrower the range of deterioration and excellent weather resistance. The method of quantifying the degree of degradation can include the following methods: take the image observed with an optical microscope, and form the image in gray scale, and regard the middle of the gray scale between the degraded part and the normal part as the end point of the degraded part, The distance from the end (side) of the optical layered body 1 to the end point was measured.
<光學積層體之製造方法> <Manufacturing method of optical laminate>
就光學積層體1之製造方法進行說明。該製造方法係至少具有：積層膜準備步驟，係準備具備硬塗層9及透明樹脂膜8之積層膜；及貼合步驟，係於偏光膜6之一面之側貼合該積層膜，並於另一面之側貼合相位差膜2。其中，相位差膜2之貼合亦可為隔著保護膜而進行。
A method of manufacturing the optical layered body 1 will be described. The manufacturing method at least includes: a laminated film preparation step of preparing a laminated film with a hard coat layer 9 and a transparent resin film 8; and a bonding step of bonding the laminated film on one side of the
於積層膜準備步驟中，係準備透明樹脂膜8，並於其一側的面貼合具備黏著層的支撐體膜(暫時保護膜)。支撐膜較佳為聚對苯二甲酸乙 二酯系樹脂或聚烯烴。另外，使構成硬塗層之原料樹脂含有紫外線吸收劑，而製備硬塗層形成用組成物。 In the laminated film preparation step, a transparent resin film 8 is prepared, and a support film (temporary protective film) having an adhesive layer is bonded to one surface thereof. The support film is preferably polyethylene terephthalate Diester resin or polyolefin. Moreover, the raw material resin which comprises a hard-coat layer was made to contain an ultraviolet absorber, and the composition for hard-coat layer formation was prepared.
繼而，將硬塗層形成用組成物塗佈於透明樹脂膜之另一側之面而形成硬塗層，獲得積層膜。於使用該積層膜時，將支撐膜剝離。 Next, the composition for hard-coat layer formation was apply|coated on the other side surface of a transparent resin film, a hard-coat layer was formed, and the laminated|multilayer film was obtained. When using this laminated film, the support film is peeled off.
另一方面，製備水平定向膜形成用組成物與垂直定向膜形成用組成物，分別塗佈於不同之基材膜上，形成水平定向膜及垂直定向膜。繼而，於各者之上塗佈另行製備之相位差層形成用組成物，形成第1相位差層2A與第2相位差層2B。然後，利用紫外線硬化型接著劑將兩相位差層相互貼合，藉此獲得相位差層之積層體。
On the other hand, a composition for forming a horizontal alignment film and a composition for forming a vertical alignment film are prepared and coated on different substrate films to form a horizontal alignment film and a vertical alignment film. Then, the separately prepared composition for retardation layer formation was apply|coated on each, and the
於貼合步驟中，係自上述積層膜剝離支撐膜，使用接著劑貼合於偏光膜6之一面。於偏光膜6之另一面係貼合保護膜7，而獲得直線偏光板3。將上述相位差層之積層體經由黏著而貼合於所獲得之直線偏光板3之保護膜7側。經過該貼合步驟，可製造光學積層體1。
In the bonding step, the support film is peeled from the above-mentioned laminated film, and bonded to one surface of the
以上，係對本發明之較佳之實施形態進行說明，但本發明並不限定於上述實施形態。例如，於上述實施形態中係表示依序積層有硬塗層、透明樹脂膜、偏光膜及相位差膜之態樣，但亦可改變為硬塗層、透明樹脂膜及偏光膜之積層順序。又，於上述實施形態中，雖說明相位差膜較佳係具有逆波長分散性之光學特性，但相位差膜亦可為具有正波長分散性之光學特性者。具有正波長分散性之光學特性之相位差膜係較具有逆波長分散性之光學特性之相位差膜不易產生面內之色調變化，但亦可應用本發明。 As mentioned above, although the preferable embodiment of this invention was demonstrated, this invention is not limited to the said embodiment. For example, in the above embodiment, the hard coat layer, the transparent resin film, the polarizing film, and the retardation film are sequentially laminated, but the lamination order of the hard coat layer, the transparent resin film, and the polarizing film may be changed. In addition, in the above-mentioned embodiment, although it is described that the retardation film preferably has the optical characteristics of reverse wavelength dispersion, the retardation film may also have the optical characteristics of positive wavelength dispersion. A retardation film having optical properties of positive wavelength dispersion is less prone to in-plane color change than a retardation film having optical properties of reverse wavelength dispersion, but the present invention can also be applied.
[實施例] [Example]
以下，列舉實施例及比較例以更具體地說明本發明之內容。再者，本發明並不限定於下述實施例。 Hereinafter, examples and comparative examples are given to describe the content of the present invention more specifically. In addition, this invention is not limited to a following Example.
<實施例1> <Example 1>
[包含相位差層(1)之積層體之製作] [Manufacturing of a laminate including a retardation layer (1)]
將下述結構之光定向性材料5重量份(重量平均分子量：30,000)與環戊酮95重量份混合，將所獲得之混合物於80℃攪拌1小時，藉此獲得水平定向膜形成用組成物。 5 parts by weight of a photo-alignment material having the following structure (weight average molecular weight: 30,000) and 95 parts by weight of cyclopentanone were mixed, and the obtained mixture was stirred at 80° C. for 1 hour, thereby obtaining a composition for forming a horizontal alignment film .
相對於將以下所示之聚合性液晶化合物A及聚合性液晶化合物B以90：10之質量比混合而成之混合物100重量份，添加調平劑(F-556；DIC股份有限公司製造)1.0重量份及作為聚合起始劑之2-二甲基胺基-2-苄基-1-(4-嗎啉基苯基)丁烷-1-酮(「Irgacure369(Irg369)」、BASFJapan股份有限公司製)6重量份。 With respect to 100 parts by weight of a mixture of the polymerizable liquid crystal compound A and the polymerizable liquid crystal compound B shown below at a mass ratio of 90:10, 1.0 Parts by weight and 2-dimethylamino-2-benzyl-1-(4-morpholinophenyl)butan-1-one ("Irgacure369(Irg369)", BASFJapan Co., Ltd. company) 6 parts by weight.
進而，以固形物成分濃度成為13%之方式添加N-甲基-2-吡咯啶酮(NMP)，於80℃下攪拌1小時，藉此獲得相位差層形成用組成物(1)。 Furthermore, N-methyl-2-pyrrolidone (NMP) was added so that the solid content concentration might become 13%, and it stirred at 80 degreeC for 1 hour, and obtained the composition (1) for retardation layer formation.
聚合性液晶化合物A係藉由日本特開2010-31223號公報所記載之方法而製造。另外，聚合性液晶化合物B是依據日本特開2009-173893號公報所記載的方法來製造。以下係表示各自的分子結構。 The polymerizable liquid crystal compound A was produced by the method described in JP-A-2010-31223. In addition, the polymerizable liquid crystal compound B was produced according to the method described in JP-A-2009-173893. The following lines represent the respective molecular structures.
(聚合性液晶化合物A)
使用電暈處理裝置(AGF-B10，春日電機股份有限公司製造)，於輸出0.3kW、處理速度3m/分鐘之條件下，對包含環烯烴聚合物(COP)膜(日本ZEON股份有限公司製造，ZF-14，厚度23μm)之基材膜進行1次電暈處理。藉由棒式塗佈機將水平定向膜形成用組成物塗佈於經實施電暈處理之基材之表面。將塗佈膜於80℃乾燥1分鐘，使用偏光UV照射裝置(SPOT CURE SP-7；Ushio電機股份有限公司製造)，以100mJ/cm2之累計光量實施偏光UV曝光。以如此方式獲得附有水平定向膜之基材膜。以雷射顯微鏡(LEXT，Olympus股份有限公司製造)測定該水平定向膜之厚度，結果為100nm。 Using a corona treatment device (AGF-B10, manufactured by Kasuga Electric Co., Ltd.), under the conditions of an output of 0.3kW and a processing speed of 3m/min, a cycloolefin polymer (COP) film (manufactured by Japan ZEON Co., Ltd., The substrate film of ZF-14, thickness 23μm) is corona treated once. The composition for forming a horizontal alignment film was coated on the surface of the corona-treated substrate with a bar coater. The coating film was dried at 80° C. for 1 minute, and polarized UV exposure was performed at a cumulative light intensity of 100 mJ/cm 2 using a polarized UV irradiation device (SPOT CURE SP-7; manufactured by Ushio Electric Co., Ltd.). In this way, a substrate film with a horizontal alignment film was obtained. The thickness of the horizontal alignment film was measured with a laser microscope (LEXT, manufactured by Olympus Co., Ltd.), and found to be 100 nm.
繼而，於室溫25℃、濕度30%RH環境下，將相位差層形成用組成物(1)通過設為孔徑0.2μm之PTFE製膜濾器(ADVANTEC TOYO(股)製造，型號：T300A025A)，使用棒式塗佈機塗佈於保溫在25℃之附水平定向膜之基材膜的水平定向膜側。將塗膜於120℃乾燥1分鐘後，使用高壓水銀燈(Unicure VB-15201BY-A，Ushio電機股份有限公司製造)照射紫外線(氮氣環境下，波長：365nm、於波長365nm之累積光量： 1000mJ/cm2)，藉此製成光學膜。用雷射顯微鏡(LEXT，Olympus股份有限公司製造)測定所獲得的塗膜的厚度，結果為2μm。 Next, the retardation layer-forming composition (1) was passed through a PTFE membrane filter (manufactured by ADVANTEC TOYO Co., Ltd., model: T300A025A) with a pore size of 0.2 μm at a room temperature of 25° C. and a humidity of 30% RH. Use a bar coater to coat on the side of the horizontally oriented film of the substrate film with the horizontally oriented film kept at 25°C. After the coating film was dried at 120°C for 1 minute, it was irradiated with ultraviolet light (Unicure VB-15201BY-A, manufactured by Ushio Electric Co., Ltd.) using a high-pressure mercury lamp (under nitrogen atmosphere, wavelength: 365nm, cumulative light intensity at 365nm wavelength: 1000mJ/cm 2 ), thereby making an optical film. When the thickness of the obtained coating film was measured with a laser microscope (LEXT, manufactured by Olympus Co., Ltd.), it was 2 μm.
以如此方式獲得積層體，該積層體係依序地積層有：聚合性液晶化合物硬化而成之層(相位差層(1))、水平定向膜及基材膜。相位差層(1)係顯示λ/4之相位差值的相位差層。相位差層(1)係顯示逆波長分散性。 In this way, a layered body is obtained. The layered system is sequentially layered with a layer formed by hardening a polymerizable liquid crystal compound (retardation layer (1)), a horizontal alignment film, and a base film. The retardation layer (1) is a retardation layer showing a retardation value of λ/4. The retardation layer (1) exhibits reverse wavelength dispersion.
[包含相位差層(2)之積層體之製作] [Manufacture of laminate including retardation layer (2)]
作為垂直定向膜形成用組成物，係使用將丙烯酸2-苯氧基乙酯、丙烯酸四氫糠酯、二季戊四醇三丙烯酸酯、及雙(2-乙烯氧基乙基)醚以1：1：4：5之比率混合，且以4%之比率添加LUCIRIN TPO作為聚合起始劑之混合物。 As a composition for vertical alignment film formation, a mixture of 2-phenoxyethyl acrylate, tetrahydrofurfuryl acrylate, dipentaerythritol triacrylate, and bis(2-vinyloxyethyl)ether was used in a ratio of 1:1: Mix at a ratio of 4:5, and add LUCIRIN TPO at a ratio of 4% as a mixture of polymerization initiators.
相位差層形成用組成物(2)係以固形物成分成為1至1.5g之方式調製光聚合性向列型液晶化合物(Merck公司製造，RMM28B)與溶劑而製作。作為溶劑，使係用以質量比(MEK：MIBK：CHN)計為35：30：35的比例混合有甲基乙基酮(MEK)、甲基異丁基酮(MIBK)和環己酮(CHN)而成的混合溶劑。 The composition (2) for retardation layer formation prepared by adjusting the photopolymerizable nematic liquid crystal compound (manufactured by Merck, RMM28B) and a solvent so that the solid content may become 1 to 1.5 g. As a solvent, methyl ethyl ketone (MEK), methyl isobutyl ketone (MIBK) and cyclohexanone ( CHN) made of mixed solvents.
準備厚度38μm之聚對苯二甲酸乙二酯(PET)膜作為基材膜。於基材膜之單面以膜厚成為3μm之方式塗佈垂直定向膜形成用組成物，並照射200mJ/cm2之紫外線，而製作垂直定向膜。 A polyethylene terephthalate (PET) film with a thickness of 38 μm was prepared as a base film. A composition for forming a vertical alignment film was applied to one side of the base film so that the film thickness became 3 μm, and 200 mJ/cm 2 of ultraviolet rays were irradiated to produce a vertical alignment film.
於垂直定向層上，藉由模式塗佈來塗設相位差層形成用組成物(2)。 On the vertical alignment layer, the retardation layer forming composition (2) was applied by pattern coating.
塗設量為4至5g(濕重)。將乾燥溫度設為75℃，將乾燥時間設為120秒，使塗膜乾燥。其後，對塗膜照射紫外線(UV)，使聚合性液晶化合物聚合。 The application amount is 4 to 5g (wet weight). The drying temperature was set at 75° C., and the drying time was set at 120 seconds to dry the coating film. Thereafter, the coating film is irradiated with ultraviolet rays (UV) to polymerize the polymerizable liquid crystal compound.
以如此方式，獲得積層體，該積層體係依序積層有：聚合性液晶化合物硬化而成之層(相位差層(2))、垂直定向膜及基材膜。相位差層(2)為正C板。相位差層(2)與垂直定向膜之合計厚度為4μm。 In this way, a layered body is obtained. The layered system is sequentially layered: a layer formed by hardening a polymerizable liquid crystal compound (retardation layer (2)), a vertical alignment film, and a base film. The retardation layer (2) is a positive C plate. The total thickness of the retardation layer (2) and the vertical alignment film was 4 μm.
[相位差層之積層體之製作] [Manufacturing of the laminated body of the retardation layer]
將包含相位差層(1)之積層體與包含相位差層(2)之積層體藉由紫外線硬化性接著劑而以各自之相位差層面(與基材膜側之表面為相反側之表面)成為貼合面之方式貼合。繼而，照射紫外線而使紫外線硬化性接著劑硬化。以如此方式，製作具有相位差層(1)及相位差層(2)之2層相位差層的相位差層之積層體。 The laminate including the retardation layer (1) and the laminate including the retardation layer (2) are separated into respective retardation layers (the surface on the opposite side to the surface of the substrate film side) by an ultraviolet curable adhesive It becomes the way of fitting surface to fit. Next, ultraviolet rays are irradiated to harden the ultraviolet curable adhesive. In this manner, a laminate of a retardation layer having two retardation layers of the retardation layer (1) and the retardation layer (2) was produced.
[偏光膜之製作] [Production of Polarizing Film]
將厚度20μm、聚合度2,400、皂化度99.9%以上之聚乙烯醇膜以乾式且延伸倍率4.5倍進行單軸延伸，保持緊繃狀態，於28℃浸漬於染色浴60秒，該染色浴係於每100重量份水含有碘0.05重量份及碘化鉀5重量份。 A polyvinyl alcohol film with a thickness of 20 μm, a degree of polymerization of 2,400, and a degree of saponification of 99.9% or more is uniaxially stretched in a dry type with an elongation ratio of 4.5 times, kept in a tight state, and immersed in a dyeing bath at 28°C for 60 seconds. 0.05 parts by weight of iodine and 5 parts by weight of potassium iodide are contained per 100 parts by weight of water.
繼而，在每100重量份水含有硼酸5.5重量份及碘化鉀15重量份之硼酸水溶液1中於64℃浸漬110秒。繼而，在每100重量份水含有硼酸5.5重量份及碘化鉀15重量份之硼酸水溶液2中於67℃浸漬30秒鐘。其後，用3℃之純水進行水洗、乾燥，而獲得偏光膜。
Then, it was immersed in the boric-acid aqueous solution 1 containing 5.5 weight part of boric acids and 15 weight part of potassium iodide per 100 weight part of water at 64 degreeC for 110 second. Then, it was immersed in the boric-acid
所獲得之偏光膜之視感度修正單體穿透率為42.15%，視感度修正偏光度為99.995%。偏光膜之單體色相a*為-0.88，單體色相b*為3.69。偏光膜之收縮應力為99.9N/mm2。 The sensitivity-corrected monomer transmittance of the obtained polarizing film was 42.15%, and the sensitivity-corrected polarization degree was 99.995%. The individual hue a* of the polarizing film is -0.88, and the individual hue b* is 3.69. The shrinkage stress of the polarizing film is 99.9N/mm 2 .
[含紫外線吸收劑之硬塗層之形成] [Formation of hard coat layer containing ultraviolet absorber]
於作為透明樹脂膜之環烯烴聚合物(COP)膜(日本ZEON股份有限公司製造，ZF-14，厚度23μm)之單面，貼合以38μ聚對苯二甲酸乙二酯作為基材膜且具備厚度15μm之黏著層的暫時保護膜。 On one side of a cycloolefin polymer (COP) film (manufactured by Japan ZEON Co., Ltd., ZF-14, thickness 23 μm) as a transparent resin film, a 38 μ polyethylene terephthalate film is attached as a base film and Temporary protective film with an adhesive layer with a thickness of 15 μm.
將作為紫外線吸收劑(1)之芝麻酚(sesamol)型苯并三唑系化合物和MMA反應鍵結而成之丙烯酸系聚合物、與二季戊四醇六丙烯酸酯與二季戊四醇五丙烯酸酯之混合物(製品名「KAYARADDPHA」，日本化藥股份有限公司製造)以固形物成分質量比45：55進行混合，並於其中添加聚合起始劑(IGMResinsB.V.公司製之Omnirad184及DKSH Japan公司製之ESACUREONE之質量比50：50)4重量份、及調平劑(製品名「F-568」，DIC股份有限公司製造)0.2重量份，並充分攪拌，製備硬塗層形成用組成物。 A mixture of an acrylic polymer formed by reacting a sesamol-type benzotriazole compound and MMA as a UV absorber (1), and a mixture of dipentaerythritol hexaacrylate and dipentaerythritol pentaacrylate (product "KAYARADDPHA", manufactured by Nippon Kayaku Co., Ltd.) was mixed at a solid content mass ratio of 45:55, and a polymerization initiator (Omnirad 184 produced by IGM Resins B.V. and ESACUREONE produced by DKSH Japan Co., Ltd. Mass ratio 50:50) 4 parts by weight, and leveling agent (product name "F-568", manufactured by DIC Co., Ltd.) 0.2 parts by weight, and fully stirred to prepare a composition for forming a hard coat layer.
繼而，於上述COP膜之另一側之面用繞線棒塗佈上述硬塗層形成用組成物而形成塗膜。對於所形成之塗膜以0.5m/s之流速使70℃之乾燥空氣流通30秒鐘，藉此使溶劑蒸發，並藉由於氮氣環境(氧濃度200ppm以下)以累計光量成為200mJ/cm2之方式照射紫外線並使其硬化，而形成膜厚為5μm之硬塗層。藉此，獲得依序具備PET基材的暫時保護膜、黏著層、環烯烴聚合物膜、硬塗層的積層膜。硬塗層之壓痕彈性模數 為2950MPa。硬塗層之壓痕彈性模數係使用Fischer Instruments製造之「超微小硬度計HM2000」，藉由上述方法進行測定。 Next, the above-mentioned composition for forming a hard coat layer was applied to the other surface of the above-mentioned COP film with a wire bar to form a coating film. For the formed coating film, let dry air at 70°C flow for 30 seconds at a flow rate of 0.5m/s to evaporate the solvent, and make the cumulative light intensity 200mJ/ cm2 in a nitrogen atmosphere (oxygen concentration below 200ppm) It is irradiated with ultraviolet rays and hardened to form a hard coat layer with a film thickness of 5 μm. Thereby, a laminated film comprising a temporary protection film of a PET base material, an adhesive layer, a cycloolefin polymer film, and a hard coat layer in this order was obtained. The indentation elastic modulus of the hard coating is 2950MPa. The indentation elastic modulus of the hard coat layer was measured by the above-mentioned method using "ultramicro hardness meter HM2000" manufactured by Fischer Instruments.
[直線偏光板之製作] [Production of Linear Polarizer]
從具備含有紫外線吸收劑之硬塗層的積層膜將PET基材之暫時保護膜與黏著層一併剝離，並且對該剝離面進行電暈處理，經由水系接著劑利用夾輥而貼合於上述所獲得之偏光膜之一面。於偏光膜之另一面，經由水系接著劑利用夾輥而貼合經皂化處理之三乙醯纖維素(TAC)膜(富士軟片股份有限公司製造之ZRG20SL，厚度20μm)。將所獲得之貼合物之張力保持為430N/m，並且於60℃乾燥2分鐘，而獲得於偏光膜之兩面具有膜之直線偏光板。此處所使用之水系接著劑係於水100份中添加羧基改性聚乙烯醇(Kuraray股份有限公司製造之Kuraray Poval KL318)3重量份、及水溶性聚醯胺環氧樹脂(田崗化學工業股份有限公司製Sumirez Resin650固體成分濃度30%之水溶液)1.5重量份而製備。TAC膜之透濕度為1500g/m2．24hr。 The temporary protective film of the PET substrate and the adhesive layer are peeled off from the laminated film with a hard coat layer containing an ultraviolet absorber, and the peeled surface is subjected to corona treatment, and bonded to the above with a nip roller through a water-based adhesive. One side of the obtained polarizing film. On the other side of the polarizing film, a saponified triacetyl cellulose (TAC) film (ZRG20SL manufactured by Fujifilm Co., Ltd., thickness 20 μm) was pasted with a nip roller through a water-based adhesive. The tension of the obtained bonded product was kept at 430 N/m, and it was dried at 60 degreeC for 2 minutes, and the linear polarizing plate which has a film on both surfaces of a polarizing film was obtained. The water-based adhesive used here is to add 3 parts by weight of carboxyl-modified polyvinyl alcohol (Kuraray Poval KL318 manufactured by Kuraray Co., Ltd.) and water-soluble polyamide epoxy resin (Tian Gang Chemical Industry Co., Ltd.) to 100 parts of water. Co., Ltd. Sumirez Resin650 solid content concentration 30% aqueous solution) 1.5 parts by weight. The moisture permeability of TAC film is 1500g/m 2 . 24hr.
自上述相位差層之積層體剝離相位差層(1)側之基材膜，使用5μm厚之丙烯酸系黏著劑(LINTEC股份有限公司製造，商品名「#L2」)貼合於上述直線偏光板之TAC膜側。藉此，獲得具備硬塗層、COP膜(透明樹脂膜)、偏光膜、TAC膜、水平定向膜、相位差層(1)、紫外線硬化性接著層、相位差層(2)、垂直定向膜、PET膜之光學積層體。 The substrate film on the retardation layer (1) side was peeled off from the laminate of the above retardation layer, and bonded to the above linear polarizing plate with a 5 μm thick acrylic adhesive (manufactured by Lintec Co., Ltd., trade name "#L2") The TAC membrane side. Thereby, a hard coat layer, a COP film (transparent resin film), a polarizing film, a TAC film, a horizontal alignment film, a retardation layer (1), an ultraviolet curable adhesive layer, a retardation layer (2), and a vertical alignment film are obtained. , Optical laminates of PET film.
[端部劣化測試] [Tip deterioration test]
將所獲得之光學積層體以硬塗層側為上側而裁切為40mm×40mm之大小之正方形。剝離PET膜，並於垂直定向膜之面積層25μm厚之丙烯酸系 黏著劑(LINTEC股份有限公司製造，商品名「#L7」)，貼合於無鹼玻璃板[Corning公司製造，商品名「Eagle-XG」]。於硬塗層側亦積層該黏著劑，並貼合於相同玻璃板。以如此方式，獲得以玻璃板夾持光學積層體的兩面之實施例1之試驗體。將該試驗體以硬塗層側成為照射面之方式配置於台式(benchtop type)之氙氣試驗機，以輸出1.3W/m2放置400小時。 The obtained optical layered body was cut into a square of a size of 40 mm x 40 mm with the hard-coat side being the upper side. Peel off the PET film, and layer an acrylic adhesive (manufactured by LINTEC Co., Ltd., trade name "#L7") with a thickness of 25 μm on the area of the vertical alignment film, and attach it to an alkali-free glass plate [manufactured by Corning, trade name "Eagle -XG"]. The adhesive is also laminated on the hard coat side and bonded to the same glass plate. In this manner, the test body of Example 1 in which both surfaces of the optical layered body were sandwiched between the glass plates was obtained. This test piece was placed in a benchtop type xenon gas tester so that the hard coat side became the irradiated surface, and was left to stand for 400 hours at an output of 1.3 W/m 2 .
其後，將兩片試驗體以一邊彼此接觸之方式相鄰地排列，並以與該等成為正交偏光的關係之方式配置偏光板，而利用光學顯微鏡自偏光板之側進行觀察並保存圖像。光學顯微鏡係使用KEYENCE股份有限公司製之「VHX-7000」。若自試驗體之端部朝向積層體之內側方向觀察，則於靠近端部之側確認到劣化區域(產生變色之區域)，並於遠離端部之側確認到正常區域(未產生變色之區域)。於圖2所示之觀察照片中，符號50為試驗體之端部，符號51為劣化區域，符號52為正常區域。
Thereafter, the two test pieces were arranged adjacent to each other in such a way that one side was in contact with each other, and the polarizing plates were arranged in such a manner that they became crossed polarized light, and the images were observed from the side of the polarizing plates using an optical microscope. picture. As an optical microscope, "VHX-7000" manufactured by KEYENCE Co., Ltd. was used. When viewed from the end of the test body toward the inside of the laminate, a degraded area (area where discoloration occurs) is confirmed on the side close to the end, and a normal area (area where discoloration does not occur) is confirmed on the side far from the end. ). In the observation photograph shown in FIG. 2 , the
使用圖像解析軟體「ImageJ(免費軟體)」，將用光學顯微鏡所觀察到之圖像轉換為黑白256灰階(0至255)之灰色圖像。轉換為黑白256灰階(0至255)之方法係使用取RGB值之平均之方法。針對該灰色圖像，沿著所觀察到的變色區域與正常區域之部分(圖2之虛線部分)繪製灰階(圖3：橫軸表示從試驗體之端部算起之距離，縱軸表示灰階之灰度之數值)。求出表示灰度之數值之最大值與最小值之中間值，將呈現該灰度之部分作為劣化區域與正常區域之邊界。將從試驗體之端部算起至該邊界為止之距離設為劣化區域之深度。 Using the image analysis software "ImageJ (free software)", the image observed with the optical microscope was converted into a black and white 256 gray scale (0 to 255) gray image. The method of converting to black and white 256 grayscale (0 to 255) is to use the method of taking the average of RGB values. For this gray image, draw the gray scale (Figure 3: the horizontal axis represents the distance from the end of the test body, and the vertical axis represents gray value of the gray scale). Calculate the middle value between the maximum value and the minimum value of the value representing the gray level, and use the part showing the gray level as the boundary between the degraded area and the normal area. The distance from the end of the test body to the boundary was defined as the depth of the deteriorated region.
[面內色相變化之測定] [Measurement of in-plane hue change]
將進行了上述端部劣化試驗之試驗體以硬塗層側成為上側之方式放置於反射板(Alanod公司製造，MIRO5 5011GP)上，使用分光測色計(CM2600d，Konica Minolta股份有限公司)測定反射光之色相。測定係安裝光自評估用試樣進入積分球時之開口部之直徑
△a*b*={(△a*)2+(△b*)2}1/2 △a*b*={(△a*) 2 +(△b*) 2 } 1/2
[鉛筆硬度測試] [Pencil hardness test]
使用安田精機製作所股份有限公司製(型號：No.553-M)鉛筆硬度試驗機。將荷重設定為500g，將刮痕長度設定為1.5cm，對硬塗層之面實施試驗。於傷痕、凹陷為5根中的1根以下之情形判定為OK，於2根以上之情形判定為NG，將成為OK之最高硬度設為鉛筆硬度。 A pencil hardness tester manufactured by Yasuda Seiki Co., Ltd. (model: No. 553-M) was used. The load was set to 500 g, the scratch length was set to 1.5 cm, and the test was implemented on the hard-coated surface. The case where one or less of five flaws and dents were present was judged as OK, and the case of two or more were judged as NG, and the highest hardness that became OK was defined as pencil hardness.
[耐擦傷性試驗] [Scratch resistance test]
使用大榮科學精機製作所股份有限公司製造之平面磨耗試驗。以試驗荷重成為250g/cm2之方式進行調整，使用Bonstar公司製造之鋼絲絨#0000實施往返10次之試驗。對硬塗層之面進行試驗，並以下述基準判定試驗後之傷痕道數。 A flat surface abrasion test manufactured by Daiei Scientific Seiki Co., Ltd. was used. The test load was adjusted so that the test load became 250 g/cm 2 , and the test was carried out 10 times back and forth using steel wool #0000 manufactured by Bonstar Corporation. The hard-coated surface was tested, and the number of scratches after the test was judged according to the following criteria.
A：無傷痕 A: no scars
A'：1至10道 A': 1 to 10 courses
B：11至20道 B: 11 to 20 lanes
C：21至30道 C: 21 to 30 lanes
D：31道以上 D: more than 31 courses
[平面性之確認] [Confirmation of planarity]
使用日立先端科技股份有限公司製造之掃描型白光干涉顯微鏡(VertScan)。使用5倍透鏡，測定硬塗層之面的表面形狀。根據所獲得之圖像算出面粗糙度(Sa)。 A scanning white light interference microscope (VertScan) manufactured by Hitachi Advanced Technology Co., Ltd. was used. Using a 5x lens, the surface shape of the hard-coated surface was measured. The surface roughness (Sa) was calculated from the obtained image.
<比較例1> <Comparative example 1>
除了使硬塗層不含紫外線吸收劑以外，以與實施例1相同之方式獲得比較例1之光學積層體。使用該光學積層體，與實施例1同樣地製作試驗體，並進行端部劣化試驗，測定面內之色相變化。又，測定硬塗層之壓痕彈性模數、鉛筆硬度、耐擦傷性、表面粗糙度。 An optical layered body of Comparative Example 1 was obtained in the same manner as in Example 1 except that the hard coat layer did not contain the ultraviolet absorber. Using this optical layered body, a test body was produced in the same manner as in Example 1, and an edge degradation test was performed to measure the change in hue in the plane. Also, the indentation elastic modulus, pencil hardness, scratch resistance, and surface roughness of the hard coat layer were measured.
<比較例2> <Comparative example 2>
除了使硬塗層不含紫外線吸收劑以外，以與實施例1相同之方式獲得比較例2之光學積層體。該積層體與比較例1之光學積層體相同。使用該光學積層體，與實施例1同樣地製作試驗體，並進行端部劣化試驗，測定面內之色相變化。又，測定硬塗層之壓痕彈性模數、鉛筆硬度、耐擦傷性、表面粗糙度。其中，於製作比較例2之試驗體時，係將用以將光學積層體之硬塗層側貼合於玻璃板之黏著層變更為以下者。 An optical laminate of Comparative Example 2 was obtained in the same manner as in Example 1 except that the hard coat layer was freed from the ultraviolet absorber. This laminate is the same as the optical laminate of Comparative Example 1. Using this optical layered body, a test body was produced in the same manner as in Example 1, and an edge degradation test was performed to measure the change in hue in the plane. Also, the indentation elastic modulus, pencil hardness, scratch resistance, and surface roughness of the hard coat layer were measured. However, when producing the test body of Comparative Example 2, the adhesive layer for bonding the hard coat side of the optical laminate to the glass plate was changed to the following.
[含紫外線吸收劑之黏著劑組成物之製作] [Production of adhesive composition containing ultraviolet absorber]
(丙烯酸樹脂之製備) (Preparation of Acrylic Resin)
於具備冷卻管、氮氣導入管、溫度計及攪拌機之反應容器中，投入作為溶劑之乙酸乙酯81.8重量份、作為單體之丙烯酸丁酯70.4重量份、丙 烯酸甲酯20.0重量份、丙烯酸2-苯氧基乙酯8.0重量份、丙烯酸2-羥基乙酯1.0重量份及丙烯酸0.6重量份之混合溶液。 In a reaction vessel equipped with a cooling pipe, a nitrogen introduction pipe, a thermometer and a stirrer, 81.8 parts by weight of ethyl acetate as a solvent, 70.4 parts by weight of butyl acrylate as a monomer, and propylene glycol were added. A mixed solution of 20.0 parts by weight of methyl acrylate, 8.0 parts by weight of 2-phenoxyethyl acrylate, 1.0 parts by weight of 2-hydroxyethyl acrylate and 0.6 parts by weight of acrylic acid.
將反應容器內置換成於氮氣環境下，並將反應容器之內溫提高至55℃。另外，準備將聚合起始劑之偶氮雙異丁腈0.14重量份溶解於乙酸乙酯10重量份而成之溶液，並將全部量之聚合起始劑溶液添加至內溫成為55℃之反應容器內。添加起始劑後，在此溫度下保持1小時。 The inside of the reaction container was replaced under a nitrogen atmosphere, and the internal temperature of the reaction container was raised to 55°C. In addition, prepare a solution in which 0.14 parts by weight of azobisisobutyronitrile as a polymerization initiator is dissolved in 10 parts by weight of ethyl acetate, and add the entire amount of the polymerization initiator solution to a reaction in which the internal temperature becomes 55°C inside the container. After addition of the starter, this temperature was maintained for 1 hour.
繼而，將內溫保持為54至56℃，並且將乙酸乙酯以添加速度17.3重量份/小時連續地添加至反應容器內。乙酸乙酯之添加係於所獲得之聚合物之濃度成為35質量%之時間點停止。 Then, while maintaining the internal temperature at 54 to 56° C., ethyl acetate was continuously added into the reaction container at an addition rate of 17.3 parts by weight/hour. Addition of ethyl acetate was stopped when the concentration of the obtained polymer became 35% by mass.
從乙酸乙酯之添加開始至經過12小時為止係保溫於54至56℃，之後添加乙酸乙酯，以聚合物之濃度成為20質量%之方式進行調節，而獲得目標之丙烯酸樹脂。 After 12 hours from the addition of ethyl acetate, the temperature was kept at 54 to 56° C., then ethyl acetate was added, and the concentration of the polymer was adjusted so that the concentration of the polymer became 20% by mass to obtain the target acrylic resin.
(紫外線吸收劑(2)之合成) (Synthesis of UV absorber (2))
將設置有戴氏冷凝管、溫度計的100mL-四頸燒瓶內設為氮氣環境，參考日本特開2017-120430號公報的合成例來合成下述結構的化合物。 A 100 mL-four-necked flask equipped with a Dairy condenser and a thermometer was set as a nitrogen atmosphere, and a compound of the following structure was synthesized with reference to the synthesis example in JP-A-2017-120430.
將該化合物的粉末2.0g、三乙二醇單甲醚(東京化成工業股份有限公司製造)1.2g、N,N-二甲基-4-胺基吡啶(東京化成工業股份有限公司 製造)20mg、氯仿8g加入至反應容器中，用磁力攪拌器進行攪拌，並以冰浴將內溫冷卻至0℃。 2.0 g of powder of this compound, 1.2 g of triethylene glycol monomethyl ether (manufactured by Tokyo Chemical Industry Co., Ltd.), 1.2 g of N,N-dimethyl-4-aminopyridine (manufactured by Tokyo Chemical Industry Co., Ltd. 20 mg of chloroform) and 8 g of chloroform were added to the reaction vessel, stirred with a magnetic stirrer, and the inner temperature was cooled to 0° C. with an ice bath.
調製將1-乙基-3-(3-二甲基胺基丙基)碳二醯亞胺鹽酸鹽(東京化成工業股份有限公司製)1.4g溶解於氯仿2.0g之溶液。將所製備之溶液使用滴液漏斗歷時2小時而滴加至內溫保持為0℃之上述反應容器內。滴加結束後，再於0℃保溫6小時。 A solution in which 1.4 g of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (manufactured by Tokyo Chemical Industry Co., Ltd.) was dissolved in 2.0 g of chloroform was prepared. The prepared solution was dripped into the said reaction container whose internal temperature was kept at 0 degreeC using the dropping funnel over 2 hours. After the dropwise addition, the mixture was kept at 0° C. for 6 hours.
反應結束後，使用蒸發器去除氯仿。將所得之油狀物溶解於乙酸乙酯，並以10%稀硫酸進行分液洗淨，接著以純水將乙酸乙酯溶液進行分液洗淨，直到水層pH成為>6為止。 After the reaction was complete, chloroform was removed using an evaporator. The obtained oil was dissolved in ethyl acetate, and washed with 10% dilute sulfuric acid, and then the ethyl acetate solution was washed with pure water until the pH of the aqueous layer became >6.
將洗淨後之有機層以芒硝乾燥，去除芒硝後，以蒸發器去除乙酸乙酯，藉此獲得作為紫外線吸收劑(2)之下述結構之化合物。 The washed organic layer was dried with Glauber's salt, and after removing Glauber's salt, ethyl acetate was removed with an evaporator to obtain a compound having the following structure as an ultraviolet absorber (2).
(含紫外線吸收劑(2)之黏著劑組成物之製作) (Production of adhesive composition containing ultraviolet absorber (2))
相對於所合成之丙烯酸樹脂之固形物成分100重量份，調配0.5重量份之交聯劑(Tosoh股份有限公司製造，商品名「Coronate」)、0.5重量份之3-縮水甘油氧基丙基三甲氧基矽烷(信越化學工業股份有限公司製造，商 品名「KBM-403」)、3.5重量份之紫外線吸收劑(2)。進而，以固形物成分濃度成為14質量%之方式添加2-丁酮。 With respect to 100 parts by weight of the solid content of the synthesized acrylic resin, 0.5 parts by weight of a crosslinking agent (manufactured by Tosoh Co., Ltd., trade name "Coronate"), 0.5 parts by weight of 3-glycidyloxypropyl trimethyl Oxysilane (manufactured by Shin-Etsu Chemical Co., Ltd. Product name "KBM-403"), 3.5 parts by weight of UV absorber (2). Furthermore, 2-butanone was added so that solid content concentration might become 14 mass %.
使用攪拌機(Yamato Scientific股份有限公司製造，商品名「Three-One Motor」)以300rpm將所獲得之組成物進行攪拌混合30分鐘，製備調配紫外線吸收劑(2)之黏著劑組成物。 The obtained composition was stirred and mixed at 300 rpm for 30 minutes using a mixer (manufactured by Yamato Scientific Co., Ltd., trade name "Three-One Motor") to prepare an adhesive composition containing an ultraviolet absorber (2).
(調配紫外線吸收劑(2)之黏著劑片之製作) (Preparation of adhesive sheet for blending UV absorber (2))
於經實施脫模處理之聚對苯二甲酸乙二酯膜(LINTEC股份有限公司製造，商品名「SP-PLR382050」)之脫模處理面，將上述黏著劑用塗佈器以乾燥後之黏著層之厚度成為20μm之方式進行塗佈。於100℃乾燥1分鐘而製作調配紫外線吸收劑(2)之黏著劑片。將該黏著劑片如上所述般地使用作為將比較例2之光學積層體貼合於玻璃板用之黏著層。 On the release-treated surface of a polyethylene terephthalate film (manufactured by LINTEC Co., Ltd., trade name "SP-PLR382050") that has undergone release treatment, apply the above-mentioned adhesive with a dry applicator. It applied so that the thickness of a layer may become 20 micrometers. Dry at 100° C. for 1 minute to prepare an adhesive sheet containing the ultraviolet absorber (2). This adhesive sheet was used as an adhesive layer for bonding the optical layered body of Comparative Example 2 to a glass plate as described above.
<比較例3> <Comparative example 3>
除了使用比較例2中所製作之黏著劑片作為將相位差層之積層體貼合於TAC膜用之黏著劑以外，以與比較例1相同之方式獲得比較例3之光學積層體。使用該光學積層體，與實施例1同樣地製作試驗體，進行端部劣化試驗，測定面內之色相變化。又，測定硬塗層之壓痕彈性模數、鉛筆硬度、耐擦傷性、表面粗糙度。 An optical layered body of Comparative Example 3 was obtained in the same manner as in Comparative Example 1 except that the adhesive sheet produced in Comparative Example 2 was used as an adhesive for bonding the layered body of the retardation layer to the TAC film. Using this optical layered body, a test body was produced in the same manner as in Example 1, and an end portion deterioration test was performed to measure a change in hue in the plane. Also, the indentation elastic modulus, pencil hardness, scratch resistance, and surface roughness of the hard coat layer were measured.
將實施例1、比較例1至3之測定結果示於表1。 Table 1 shows the measurement results of Example 1 and Comparative Examples 1 to 3.
[表1]
根據該等結果可知，於硬塗層中含有紫外線吸收劑之情形時，從光學積層體端部開始之劣化得到抑制，面內之色相變化亦得到抑制。 From these results, when the hard-coat layer contains an ultraviolet absorber, it turns out that deterioration from the edge part of an optical layered body is suppressed, and the change of the hue in a plane is also suppressed.
[產業上之可利用性] [Industrial availability]
本發明係可利用於偏光板領域。 The present invention is applicable to the field of polarizing plates.
1:光學積層體 1: Optical laminate
2:相位差膜 2: Retardation film
2A:第1相位差層 2A: The first retardation layer
2B:第2相位差層 2B: The second retardation layer
2B:相位差層 2B: Retardation layer
3:直線偏光板 3: Linear polarizer
4:黏著層 4: Adhesive layer
5:剝離膜 5: Peel off film
6:偏光膜 6: Polarizing film
7:保護膜 7: Protective film
8:透明樹脂膜 8: Transparent resin film
9:硬塗層 9: Hard coating
Claims (13)
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