TW202414002A - Polarizing plate and organic EL display device with retardation layer - Google Patents
Polarizing plate and organic EL display device with retardation layer Download PDFInfo
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- TW202414002A TW202414002A TW112122888A TW112122888A TW202414002A TW 202414002 A TW202414002 A TW 202414002A TW 112122888 A TW112122888 A TW 112122888A TW 112122888 A TW112122888 A TW 112122888A TW 202414002 A TW202414002 A TW 202414002A
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- phase difference
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- adhesive
- difference layer
- polarizing plate
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- FRGPKMWIYVTFIQ-UHFFFAOYSA-N triethoxy(3-isocyanatopropyl)silane Chemical compound CCO[Si](OCC)(OCC)CCCN=C=O FRGPKMWIYVTFIQ-UHFFFAOYSA-N 0.000 description 1
Abstract
本發明提供一種耐熱性優異之附相位差層之偏光板。本發明之附相位差層之偏光板依序具有偏光板、第1相位差層、第1黏著劑層、第2相位差層、及第2黏著劑層，第1及第2相位差層包含液晶化合物，第1黏著劑層之厚度為8 μm以下，且25℃下之彈性模數為10 5Pa～10 6Pa，且第2黏著劑層係由基礎聚合物中包含70重量%以上之(甲基)丙烯酸烷基酯之黏著劑所構成，且25℃下之彈性模數為5.0×10 5Pa以下。 The present invention provides a polarizing plate with a phase difference layer having excellent heat resistance. The polarizing plate with a phase difference layer of the present invention sequentially comprises a polarizing plate, a first phase difference layer, a first adhesive layer, a second phase difference layer, and a second adhesive layer, the first and second phase difference layers contain liquid crystal compounds, the first adhesive layer has a thickness of 8 μm or less, and an elastic modulus of 10 5 Pa to 10 6 Pa at 25°C, and the second adhesive layer is composed of an adhesive containing 70 wt % or more of alkyl (meth)acrylate in a base polymer, and an elastic modulus of 5.0×10 5 Pa or less at 25°C.
Description
本發明係關於一種附相位差層之偏光板及有機EL顯示裝置。The present invention relates to a polarizing plate with a phase difference layer and an organic EL display device.
近年來，隨著薄型顯示器之普及，提出搭載有機EL面板之圖像顯示裝置(有機EL(Electroluminescence，電致發光)顯示裝置)。有機EL面板具有反射性較高之金屬層，容易產生外界光反射或背景之映入等問題。因此，已知藉由將附相位差層之偏光板(圓偏光板)設置於視認側而防止該等問題。然而，於將利用黏著劑貼合包含液晶化合物之2層相位差層而成之積層體用作此種附相位差層之偏光板之相位差層，且經由黏著劑將該附相位差層之偏光板貼合於有機EL面板的情形時，耐熱性較低，有出現於相位差層產生龜裂或者產生不均等問題之情形。進而，有出現附相位差層之偏光板容易產生劃痕或者發生捲曲等問題之情形。 先前技術文獻 專利文獻 In recent years, with the popularity of thin displays, image display devices equipped with organic EL panels (organic EL (Electroluminescence) display devices) have been proposed. Organic EL panels have a highly reflective metal layer, which is prone to problems such as reflection of external light or background reflection. Therefore, it is known to prevent such problems by placing a polarizing plate (circular polarizing plate) with a phase difference layer on the viewing side. However, when a laminate formed by bonding two phase difference layers containing liquid crystal compounds with an adhesive is used as the phase difference layer of such a polarizing plate with a phase difference layer, and the polarizing plate with a phase difference layer is bonded to an organic EL panel with an adhesive, the heat resistance is low, and there are cases where problems such as cracking or unevenness occur in the phase difference layer. Furthermore, there are cases where the polarizing plate with a phase difference layer is prone to scratches or curling. Prior art literature Patent literature
專利文獻1：日本專利第3325560號公報Patent document 1: Japanese Patent No. 3325560
[發明所欲解決之問題][The problem the invention is trying to solve]
本發明係為了解決上述先前問題而成，其主要目的在於提供一種耐熱性優異、不易產生劃痕、且不易產生捲曲之附相位差層之偏光板、及使用此種附相位差層之偏光板之有機EL顯示裝置。 [解決問題之技術手段] The present invention is made to solve the above-mentioned previous problems, and its main purpose is to provide a polarizing plate with a phase difference layer that has excellent heat resistance, is not easy to be scratched, and is not easy to be curled, and an organic EL display device using such a polarizing plate with a phase difference layer. [Technical means for solving the problem]
本發明之附相位差層之偏光板依序具有偏光板、第1相位差層、第1黏著劑層、第2相位差層、及第2黏著劑層，上述第1相位差層及上述第2相位差層包含液晶化合物，上述第1黏著劑層之厚度為8 μm以下，且25℃下之彈性模數為10 5Pa～10 6Pa，且上述第2黏著劑層係由基礎聚合物中包含70重量%以上之(甲基)丙烯酸烷基酯之黏著劑所構成，且25℃下之彈性模數為5.0×10 5Pa以下。 於一實施形態中，附相位差層之偏光板於上述偏光板之視認側進而具有表面保護膜，且該表面保護膜之厚度為40 μm～90 μm。 根據本發明之另一態樣，提供一種有機EL顯示裝置。該有機EL顯示裝置具有上述附相位差層之偏光板。 [發明之效果] The polarizing plate with phase difference layer of the present invention comprises a polarizing plate, a first phase difference layer, a first adhesive layer, a second phase difference layer, and a second adhesive layer in order, wherein the first phase difference layer and the second phase difference layer comprise a liquid crystal compound, the first adhesive layer has a thickness of 8 μm or less, and an elastic modulus of 10 5 Pa to 10 6 Pa at 25° C., and the second adhesive layer is composed of an adhesive containing 70 wt % or more of alkyl (meth)acrylate in a base polymer, and an elastic modulus of 5.0×10 5 Pa or less at 25° C. In one embodiment, the polarizing plate with phase difference layer comprises a surface protective film on the visual side of the polarizing plate, and the thickness of the surface protective film is 40 μm to 90 μm. According to another aspect of the present invention, an organic EL display device is provided. The organic EL display device has the above-mentioned polarizing plate with a phase difference layer. [Effects of the Invention]
根據本發明，第1黏著劑層之厚度為8 μm以下，且25℃下之彈性模數為10 5Pa～10 6Pa，且第2黏著劑層於基礎聚合物中包含70重量%以上之(甲基)丙烯酸烷基酯，且25℃下之彈性模數為5.0×10 5Pa以下，藉此可實現耐熱性優異、不易產生劃痕、且不易產生捲曲之附相位差層之偏光板。 According to the present invention, the thickness of the first adhesive layer is 8 μm or less, and the elastic modulus at 25°C is 10 5 Pa to 10 6 Pa, and the second adhesive layer contains 70 wt % or more of alkyl (meth)acrylate in the base polymer, and the elastic modulus at 25°C is 5.0×10 5 Pa or less, thereby realizing a polarizing plate with a phase difference layer that has excellent heat resistance, is not prone to scratches, and is not prone to curling.
以下，對本發明之實施形態進行說明，但本發明並不限定於該等實施形態。Hereinafter, embodiments of the present invention will be described, but the present invention is not limited to these embodiments.
A.附相位差層之偏光板 圖1係本發明之一實施形態之附相位差層之偏光板之概略剖視圖。如圖1所示，附相位差層之偏光板100依序具有偏光板10、第1相位差層20、第1黏著劑層30、第2相位差層40、及第2黏著劑層50。即，第1相位差層20與第2相位差層40係經由第1黏著劑層30而積層。第1相位差層20及第2相位差層40係包含液晶化合物而構成。第1黏著劑層30於25℃下之彈性模數為10 5Pa～10 6Pa。第1黏著劑層30於一實施形態中厚度為5 μm～30 μm，於另一實施形態中厚度為8 μm以下。第2黏著劑層50係由基礎聚合物中包含70重量%以上之(甲基)丙烯酸烷基酯之黏著劑所構成。於一實施形態中，第2黏著劑層50於25℃下之彈性模數為9.0×10 4Pa以下，於另一實施形態中，25℃下之彈性模數為5.0×10 5Pa以下。附相位差層之偏光板亦可於偏光板之視認側進而具有表面保護膜(未圖示)。於此情形時，該表面保護膜之厚度為40 μm～90 μm。上述附相位差層之偏光板100之耐熱性優異，不易產生捲曲，可抑制第1相位差層20及/或第2相位差層40之劃痕之產生、龜裂之產生、以及不均之產生。 A. Polarizing plate with phase difference layer FIG1 is a schematic cross-sectional view of a polarizing plate with phase difference layer in one embodiment of the present invention. As shown in FIG1 , the polarizing plate with phase difference layer 100 has a polarizing plate 10, a first phase difference layer 20, a first adhesive layer 30, a second phase difference layer 40, and a second adhesive layer 50 in sequence. That is, the first phase difference layer 20 and the second phase difference layer 40 are laminated via the first adhesive layer 30. The first phase difference layer 20 and the second phase difference layer 40 are composed of liquid crystal compounds. The elastic modulus of the first adhesive layer 30 at 25°C is 10 5 Pa to 10 6 Pa. The first adhesive layer 30 has a thickness of 5 μm to 30 μm in one embodiment, and a thickness of 8 μm or less in another embodiment. The second adhesive layer 50 is composed of an adhesive containing 70% by weight or more of alkyl (meth)acrylate in a base polymer. In one embodiment, the elastic modulus of the second adhesive layer 50 at 25°C is 9.0×10 4 Pa or less, and in another embodiment, the elastic modulus at 25°C is 5.0×10 5 Pa or less. The polarizing plate with a phase difference layer may also have a surface protective film (not shown) on the visual side of the polarizing plate. In this case, the thickness of the surface protective film is 40 μm to 90 μm. The polarizing plate 100 with a phase difference layer has excellent heat resistance and is not prone to curling, and can suppress the generation of scratches, cracks, and unevenness of the first phase difference layer 20 and/or the second phase difference layer 40 .
以下，對構成附相位差層之偏光板100之各層進行詳細說明。Hereinafter, each layer constituting the polarizing plate with phase difference layer 100 will be described in detail.
B.偏光板 代表性而言，偏光板10具有偏光元件、配置於偏光元件之單側之第1保護層、及配置於偏光元件之另一側之第2保護層。偏光元件代表性而言為吸收型偏光元件。第1保護層及第2保護層中之一者亦可省略。 B. Polarizing plate Typically, the polarizing plate 10 has a polarizing element, a first protective layer disposed on one side of the polarizing element, and a second protective layer disposed on the other side of the polarizing element. The polarizing element is typically an absorption-type polarizing element. One of the first protective layer and the second protective layer may be omitted.
B-1.偏光元件 作為偏光元件，可採用任意適當之偏光元件。例如，形成偏光元件之樹脂膜可為單層之樹脂膜，亦可為兩層以上之積層體。 B-1. Polarizing element As the polarizing element, any appropriate polarizing element can be used. For example, the resin film forming the polarizing element can be a single-layer resin film or a laminated body of two or more layers.
作為由單層之樹脂膜構成之偏光元件之具體例，可列舉對聚乙烯醇(PVA)系膜、部分縮甲醛化PVA系膜、乙烯-乙酸乙烯酯共聚物系部分皂化膜等親水性高分子膜實施利用碘或二色性染料等二色性物質之染色處理及延伸處理而成者、PVA之脫水處理物或聚氯乙烯之脫氯化氫處理物等多烯系配向膜等。較佳為，因光學特性優異故而使用利用碘將PVA系膜染色並進行單軸延伸所獲得之偏光元件。Specific examples of polarizing elements composed of a single-layer resin film include polyvinyl alcohol (PVA) films, partially formalized PVA films, ethylene-vinyl acetate copolymer partially saponified films, etc., which are dyed with dichroic substances such as iodine or dichroic dyes and stretched, and polyene alignment films such as dehydrated PVA films or dehydrochlorinated polyvinyl chloride films. Preferably, a polarizing element obtained by dyeing a PVA film with iodine and uniaxially stretching it is used because of its excellent optical properties.
上述利用碘之染色例如係藉由將PVA系膜浸漬於碘水溶液而進行。上述單軸延伸之延伸倍率較佳為3～7倍。延伸可於染色處理後進行，亦可一面染色一面進行。又，亦可於延伸後染色。視需要對PVA系膜實施膨潤處理、交聯處理、洗淨處理、乾燥處理等。例如，藉由於染色前將PVA系膜浸漬於水進行水洗，不僅可將PVA系膜表面之污漬或抗黏連劑洗淨，而且可使PVA系膜膨潤而防止染色不均等。The dyeing using iodine is performed, for example, by immersing the PVA membrane in an iodine aqueous solution. The stretching ratio of the uniaxial stretching is preferably 3 to 7 times. The stretching can be performed after the dyeing treatment, or it can be performed while dyeing. In addition, it can be dyed after stretching. The PVA membrane is subjected to swelling treatment, crosslinking treatment, cleaning treatment, drying treatment, etc. as needed. For example, by immersing the PVA membrane in water and washing it before dyeing, not only can the stains or anti-adhesive agents on the surface of the PVA membrane be washed, but the PVA membrane can also be swelled to prevent uneven dyeing.
作為使用積層體所獲得之偏光元件之具體例，可列舉使用樹脂基材與積層於該樹脂基材之PVA系樹脂層(PVA系樹脂膜)之積層體、或樹脂基材與塗佈形成於該樹脂基材之PVA系樹脂層之積層體所獲得之偏光元件。使用樹脂基材與塗佈形成於該樹脂基材之PVA系樹脂層之積層體所獲得之偏光元件例如可藉由如下方式製作，即，將PVA系樹脂溶液塗佈於樹脂基材並使其乾燥而於樹脂基材上形成PVA系樹脂層，從而獲得樹脂基材與PVA系樹脂層之積層體；將該積層體延伸及染色而將PVA系樹脂層製成偏光元件。於本實施形態中，延伸代表性而言包含將積層體浸漬於硼酸水溶液中延伸。進而，延伸視需要可進而包含於硼酸水溶液中之延伸前將積層體於高溫(例如，95℃以上)下進行空中延伸。所獲得之樹脂基材/偏光元件之積層體可直接使用(即，可將樹脂基材作為偏光元件之保護層)，亦可自樹脂基材/偏光元件之積層體將樹脂基材剝離，並將視目的之任意適當之保護層積層於該剝離面而使用。此種偏光元件之製造方法之詳情例如記載於日本專利特開2012-73580號公報。該公報之整體之記載係以參考之形式引用至本說明書中。As specific examples of polarizing elements obtained using a laminate, there can be cited a laminate of a resin substrate and a PVA-based resin layer (PVA-based resin film) laminated on the resin substrate, or a laminate of a resin substrate and a PVA-based resin layer coated on the resin substrate. A polarizing element obtained by using a laminate of a resin substrate and a PVA-based resin layer coated on the resin substrate can be produced, for example, by coating a PVA-based resin solution on the resin substrate and drying it to form a PVA-based resin layer on the resin substrate, thereby obtaining a laminate of the resin substrate and the PVA-based resin layer; and stretching and dyeing the laminate to make the PVA-based resin layer into a polarizing element. In this embodiment, stretching typically includes immersing the laminate in a boric acid aqueous solution for stretching. Furthermore, stretching can further include stretching the laminate in the air at a high temperature (for example, above 95° C.) before stretching in a boric acid aqueous solution, if necessary. The obtained resin substrate/polarizing element laminate can be used directly (i.e., the resin substrate can be used as a protective layer of the polarizing element), or the resin substrate can be peeled off from the resin substrate/polarizing element laminate, and any appropriate protective layer can be laminated on the peeled surface according to the purpose. The details of the manufacturing method of such a polarizing element are described in, for example, Japanese Patent Publication No. 2012-73580. The entire description of the publication is cited in this specification as a reference.
偏光元件之厚度例如為1 μm～35 μm。於一實施形態中，偏光元件之厚度較佳為1 μm～15 μm，進而較佳為3 μm～10 μm，尤佳為3 μm～8 μm。若偏光元件之厚度為此種範圍，則可良好地抑制加熱時之捲曲且獲得良好之加熱時之外觀耐久性。The thickness of the polarizing element is, for example, 1 μm to 35 μm. In one embodiment, the thickness of the polarizing element is preferably 1 μm to 15 μm, more preferably 3 μm to 10 μm, and particularly preferably 3 μm to 8 μm. If the thickness of the polarizing element is within this range, curling during heating can be well suppressed and good appearance durability during heating can be obtained.
B-2.保護層 第1及第2保護層係由可作為保護偏光元件之膜使用之任意適當之保護膜所形成。作為成為該保護膜之主成分之材料之具體例，可列舉：三乙醯纖維素(TAC)等纖維素系樹脂、或聚酯系、聚乙烯醇系、聚碳酸酯系、聚醯胺系、聚醯亞胺系、聚醚碸系、聚碸系、聚苯乙烯系、聚降𦯉烯系、聚烯烴系、(甲基)丙烯酸系、乙酸酯系等之透明樹脂等。又，亦可列舉(甲基)丙烯酸系、胺基甲酸酯系、(甲基)丙烯酸胺基甲酸酯系、環氧系、聚矽氧系等之熱硬化型樹脂或紫外線硬化型樹脂等。此外，例如亦可列舉矽氧烷系聚合物等玻璃質系聚合物。又，亦可使用日本專利特開2001-343529號公報(WO01/37007)所記載之聚合物膜。作為該膜之材料，例如，可使用含有側鏈具有取代或未取代之醯亞胺基之熱塑性樹脂、及側鏈具有取代或未取代之苯基以及腈基之熱塑性樹脂之樹脂組合物，例如可列舉具有包含異丁烯及N-甲基順丁烯二醯亞胺之交替共聚物、及丙烯腈-苯乙烯共聚物的樹脂組合物。該聚合物膜例如可為上述樹脂組合物之擠出成形物。 B-2. Protective layer The first and second protective layers are formed of any appropriate protective film that can be used as a film to protect the polarizing element. Specific examples of the material that is the main component of the protective film include: cellulose resins such as triacetyl cellulose (TAC), or transparent resins such as polyester, polyvinyl alcohol, polycarbonate, polyamide, polyimide, polyether sulfone, polysulfone, polystyrene, polybutylene, polyolefin, (meth)acrylic, and acetate. In addition, thermosetting resins or ultraviolet curing resins such as (meth)acrylic, urethane, (meth)acrylic urethane, epoxy, and silicone can also be listed. In addition, for example, glassy polymers such as siloxane polymers can also be cited. In addition, the polymer film described in Japanese Patent Publication No. 2001-343529 (WO01/37007) can also be used. As the material of the film, for example, a resin composition containing a thermoplastic resin having a substituted or unsubstituted amide group on the side chain and a thermoplastic resin having a substituted or unsubstituted phenyl and nitrile group on the side chain can be used, for example, a resin composition containing an alternating copolymer of isobutylene and N-methylbutylene diimide and an acrylonitrile-styrene copolymer can be cited. The polymer film can be, for example, an extruded product of the above resin composition.
保護膜之厚度較佳為10 μm～100 μm。保護膜可經由接著層(具體而言，接著剤層、黏著劑層)積層於偏光元件，亦可密接(不經由接著層地)積層於偏光元件。接著劑層係由任意適當之接著劑所形成。作為接著劑，例如可列舉將聚乙烯醇系樹脂作為主成分之水溶性接著劑。將聚乙烯醇系樹脂作為主成分之水溶性接著劑較佳為可進而含有金屬化合物膠體。金屬化合物膠體可為金屬化合物微粒子分散於分散媒中而成者，且可為因微粒子之同種電荷之相互排斥而靜電穩定化且持續地具有穩定性者。只要不對偏光特性等光學特性造成不良影響，形成金屬化合物膠體之微粒子之平均粒徑可為任意適當之值。較佳為1 nm～100 nm，進而較佳為1 nm～50 nm。其原因在於：可使微粒子均勻地分散於接著劑層中，可確保接著性且抑制裂點。再者，所謂「裂點」係指產生於偏光元件與保護膜之界面之局部性凹凸缺陷。黏著劑層係由任意適當之黏著劑所構成。The thickness of the protective film is preferably 10 μm to 100 μm. The protective film can be laminated on the polarizing element via a bonding layer (specifically, a bonding agent layer, an adhesive layer), or can be laminated on the polarizing element in close contact (without a bonding layer). The bonding agent layer is formed by any appropriate bonding agent. As the bonding agent, for example, a water-soluble bonding agent having a polyvinyl alcohol resin as a main component can be cited. The water-soluble bonding agent having a polyvinyl alcohol resin as a main component can preferably further contain a metal compound colloid. The metal compound colloid may be a metal compound microparticle dispersed in a dispersion medium, and may be electrostatically stabilized and continuously stable due to the mutual repulsion of like charges of the microparticles. The average particle size of the microparticles forming the metal compound colloid may be any appropriate value as long as it does not adversely affect optical properties such as polarization properties. It is preferably 1 nm to 100 nm, and further preferably 1 nm to 50 nm. The reason is that the microparticles can be uniformly dispersed in the adhesive layer, adhesion can be ensured, and cracks can be suppressed. Furthermore, the so-called "cracks" refer to localized concave-convex defects generated at the interface between the polarizing element and the protective film. The adhesive layer is composed of any appropriate adhesive.
C.相位差層 如上所述，第1及第2相位差層係包含液晶化合物而構成。代表性而言，第1及第2相位差層可由含有液晶化合物之液晶性組合物之配向固化層所構成。本說明書中，所謂「配向固化層」係指液晶化合物於層內在特定方向上配向且其配向狀態固定之層。液晶化合物之配向固化層可藉由如下方式形成，即，對特定基材之表面實施配向處理，向該表面塗敷包含液晶化合物之塗敷液而使該液晶化合物於對應於上述配向處理之方向上配向，並將該配向狀態固定。於一實施形態中，基材為任意適當之樹脂膜，且形成於該基材上之配向固化層可轉印至構成附相位差層之偏光板之其他層之表面。液晶化合物之具體例及配向固化層之形成方法之詳情記載於日本專利特開2006-163343號公報。該公報之記載以參考之形式引用至本說明書中。 C. Phase difference layer As described above, the first and second phase difference layers are composed of liquid crystal compounds. Representatively, the first and second phase difference layers can be composed of an alignment solidified layer of a liquid crystal composition containing liquid crystal compounds. In this specification, the so-called "alignment solidified layer" refers to a layer in which the liquid crystal compound is aligned in a specific direction within the layer and its alignment state is fixed. The alignment solidified layer of the liquid crystal compound can be formed by performing an alignment treatment on the surface of a specific substrate, applying a coating liquid containing a liquid crystal compound to the surface so that the liquid crystal compound is aligned in a direction corresponding to the above-mentioned alignment treatment, and fixing the alignment state. In one embodiment, the substrate is any appropriate resin film, and the alignment solidified layer formed on the substrate can be transferred to the surface of other layers constituting the polarizing plate with a phase difference layer. The specific examples of liquid crystal compounds and the details of the method for forming the alignment solidified layer are described in Japanese Patent Publication No. 2006-163343. The contents of the publication are cited in this specification as a reference.
於一實施形態中，第1相位差層之面內相位差Re(550)較佳為200 nm～300 nm，且第2相位差層之面內相位差Re(550)較佳為100 nm～150 nm。因此，於此情形時，第1相位差層可作為λ/2板發揮作用，第2相位差層可作為λ/4板發揮作用。偏光元件之吸收軸與第1相位差層之遲相軸所成之角度較佳為5°～25°，尤佳為約15°。偏光元件之吸收軸與第2相位差層之遲相軸所成之角度較佳為65°～85°，尤佳為約75°。於另一實施形態中，第1相位差層之面內相位差Re(550)較佳為120 nm～160 nm，且第2相位差層之折射率橢圓體滿足nz＞nx＝ny之關係。因此，於此情形時，第1相位差層可作為λ/4板發揮作用，第2相位差層可作為所謂之陽極C板發揮作用。偏光元件之吸收軸與第1相位差層之遲相軸所成之角度較佳為39°～51°，尤佳為約45°。In one embodiment, the in-plane phase difference Re(550) of the first phase difference layer is preferably 200 nm to 300 nm, and the in-plane phase difference Re(550) of the second phase difference layer is preferably 100 nm to 150 nm. Therefore, in this case, the first phase difference layer can function as a λ/2 plate, and the second phase difference layer can function as a λ/4 plate. The angle formed by the absorption axis of the polarizing element and the retardation axis of the first phase difference layer is preferably 5° to 25°, and is preferably about 15°. The angle formed by the absorption axis of the polarizing element and the retardation axis of the second phase difference layer is preferably 65° to 85°, and is preferably about 75°. In another embodiment, the in-plane phase difference Re(550) of the first phase difference layer is preferably 120 nm to 160 nm, and the refractive index ellipse of the second phase difference layer satisfies the relationship nz＞nx＝ny. Therefore, in this case, the first phase difference layer can function as a λ/4 plate, and the second phase difference layer can function as a so-called anode C plate. The angle between the absorption axis of the polarizing element and the retardation axis of the first phase difference layer is preferably 39° to 51°, and is particularly preferably about 45°.
C-1.第1相位差層 於一實施形態中，第1相位差層可由含有實質上垂直地配向之圓盤狀液晶化合物之液晶性組合物之配向固化層所構成。於本說明書中，所謂「圓盤狀液晶化合物」係指分子結構中具有圓板狀之液晶原基且2～8條側鏈由醚鍵或酯鍵放射狀地鍵結於該液晶原基者。第1相位差層之厚度可以獲得所需之面內相位差之方式進行設定，較佳為1 μm～20 μm，更佳為1 μm～12 μm。上述含有圓盤狀液晶化合物之液晶性組合物只要包含圓盤狀液晶化合物且顯示液晶性則並無特別限制。上述液晶性組合物中之圓盤狀液晶化合物之含量相對於液晶性組合物之總固形物成分100重量份較佳為40重量份以上且未達100重量份。作為包含上述含有實質上垂直地配向之圓盤狀液晶化合物之液晶性組合物之配向固化層之相位差膜，可藉由日本專利特開2001-56411號公報所記載之方法獲得。 C-1. The first phase difference layer In one embodiment, the first phase difference layer can be composed of an oriented solidified layer of a liquid crystal composition containing a discotic liquid crystal compound that is substantially vertically oriented. In this specification, the so-called "discotic liquid crystal compound" refers to a liquid crystal unit having a disc-shaped liquid crystal unit in the molecular structure and 2 to 8 side chains radially bonded to the liquid crystal unit by ether bonds or ester bonds. The thickness of the first phase difference layer can be set in a manner to obtain the desired in-plane phase difference, preferably 1 μm to 20 μm, and more preferably 1 μm to 12 μm. The above-mentioned liquid crystal composition containing a discotic liquid crystal compound is not particularly limited as long as it contains a discotic liquid crystal compound and exhibits liquid crystal properties. The content of the discotic liquid crystal compound in the above-mentioned liquid crystal composition is preferably 40 parts by weight or more and less than 100 parts by weight relative to 100 parts by weight of the total solid content of the liquid crystal composition. The phase difference film as an alignment cured layer of the above-mentioned liquid crystal composition containing a discotic liquid crystal compound that is substantially vertically aligned can be obtained by the method described in Japanese Patent Publication No. 2001-56411.
於另一實施形態中，第1相位差層可由棒狀之液晶化合物排列於相位差層之遲相軸方向上之狀態進行配向(水平配向)之配向固化層所構成。作為液晶化合物，例如可列舉液晶相為向列相之液晶化合物(向列型液晶)。作為此種液晶化合物，例如可使用液晶聚合物或液晶單體。液晶化合物之液晶性之表現機制為溶致或熱致均可。於液晶化合物為液晶單體之情形時，該液晶單體較佳為聚合性單體及交聯性單體。其原因在於：藉由使液晶單體聚合或交聯，可固定液晶單體之配向狀態。可採用任意適當之液晶單體作為上述液晶單體。例如，可使用日本專利特表2002-533742(WO00/37585)、EP358208(US5211877)、EP66137(US4388453)、WO93/22397、EP0261712、DE19504224、DE4408171、及GB2280445等所記載之聚合性液晶原化合物等。作為此種聚合性液晶原化合物之具體例，例如可列舉：BASF公司之商品名LC242、Merck公司之商品名E7、Wacker-Chem公司之商品名LC-Sillicon-CC3767。第1相位差層之厚度可以獲得所需之面內相位差之方式進行設定，較佳為1 μm～10 μm，更佳為1 μm～6 μm。In another embodiment, the first phase difference layer may be composed of an alignment solidified layer in which rod-shaped liquid crystal compounds are arranged in the direction of the phase axis of the phase difference layer for alignment (horizontal alignment). As the liquid crystal compound, for example, a liquid crystal compound whose liquid crystal phase is a nematic phase (nematic liquid crystal) can be cited. As such a liquid crystal compound, for example, a liquid crystal polymer or a liquid crystal monomer can be used. The liquid crystal compound may exhibit a mechanism of lyotropic or thermotropic properties. When the liquid crystal compound is a liquid crystal monomer, the liquid crystal monomer is preferably a polymerizable monomer and a crosslinking monomer. The reason is that the alignment state of the liquid crystal monomer can be fixed by polymerizing or crosslinking the liquid crystal monomer. Any appropriate liquid crystal monomer can be used as the above-mentioned liquid crystal monomer. For example, the polymerizable liquid crystal compounds described in Japanese Patent Table 2002-533742 (WO00/37585), EP358208 (US5211877), EP66137 (US4388453), WO93/22397, EP0261712, DE19504224, DE4408171, and GB2280445 can be used. Specific examples of such polymerizable liquid crystal compounds include: BASF's trade name LC242, Merck's trade name E7, and Wacker-Chem's trade name LC-Sillicon-CC3767. The thickness of the first phase difference layer can be set in a manner to obtain the desired in-plane phase difference, preferably 1 μm to 10 μm, and more preferably 1 μm to 6 μm.
C-2.第2相位差層 可作為λ/4板發揮作用之第2相位差層可藉由關於第1相位差層於上述C-1項中所說明之材料及方法而形成。 C-2. Second phase difference layer The second phase difference layer that can function as a λ/4 plate can be formed by using the materials and methods described in the above C-1 regarding the first phase difference layer.
可作為陽極C板發揮作用之第2相位差層只要折射率橢圓體滿足nz＞nx＝ny之關係，則可由任意適當之液晶化合物構成。此種液晶化合物之詳情記載於日本專利第4186980號公報及日本專利第6055569號公報。該公報之記載係以參考之形式引用至本說明書中。於一實施形態中，第2相位差層可由下述化學式(I)(式中之數字65及35表示單體單元之莫耳%，方便起見以嵌段聚合物表示：重量平均分子量5000)所表示之側鏈型液晶聚合物、及顯示向列型液晶相之聚合性液晶所構成。The second phase difference layer that can function as an anode C plate can be composed of any appropriate liquid crystal compound as long as the refractive index ellipse satisfies the relationship of nz＞nx＝ny. The details of such liquid crystal compounds are described in Japanese Patent Gazette No. 4186980 and Japanese Patent Gazette No. 6055569. The description of the gazette is cited in this specification as a reference. In one embodiment, the second phase difference layer can be composed of a side-chain liquid crystal polymer represented by the following chemical formula (I) (the numbers 65 and 35 in the formula represent the molar % of the monomer unit, and for convenience, it is represented by a block polymer: the weight average molecular weight is 5000), and a polymerizable liquid crystal showing a nematic liquid crystal phase.
[化1] [Chemistry 1]
D.第1及第2黏著劑層 第1黏著劑層於25℃下之彈性模數為10 5Pa～10 6Pa。於一實施形態中，第1黏著劑之厚度為5 μm～30 μm，較佳為10 μm～25 μm。於另一實施形態中，第1黏著劑層之厚度為8 μm以下，較佳為5 μm～8 μm。上述彈性模數較佳為1.1×10 5Pa～1.9×10 5Pa，更佳為1.2×10 5Pa～1.8×10 5Pa。 D. The first and second adhesive layers The elastic modulus of the first adhesive layer at 25°C is 10 5 Pa to 10 6 Pa. In one embodiment, the thickness of the first adhesive is 5 μm to 30 μm, preferably 10 μm to 25 μm. In another embodiment, the thickness of the first adhesive layer is 8 μm or less, preferably 5 μm to 8 μm. The elastic modulus is preferably 1.1×10 5 Pa to 1.9×10 5 Pa, more preferably 1.2×10 5 Pa to 1.8×10 5 Pa.
第2黏著劑層係由基礎聚合物中包含70重量%以上之(甲基)丙烯酸烷基酯之黏著劑所構成。構成第2黏著劑層之黏著劑之基礎聚合物中之(甲基)丙烯酸烷基酯之含量較佳為75重量%～99重量%，更佳為80重量%～95重量%。於一實施形態中，第2黏著劑層於25℃下之彈性模數為9.0×10 4Pa以下，較佳為1.0×10 3Pa～9.0×10 4Pa，更佳為1.0×10 4Pa～8.5×10 4Pa。於另一實施形態中，上述彈性模數為5.0×10 5Pa以下，較佳為1.0×10 3Pa～2.0×10 5Pa，更佳為1.0×10 4Pa～1.6×10 5Pa。 The second adhesive layer is composed of an adhesive containing 70 wt% or more of alkyl (meth)acrylate in a base polymer. The content of alkyl (meth)acrylate in the base polymer of the adhesive constituting the second adhesive layer is preferably 75 wt% to 99 wt%, more preferably 80 wt% to 95 wt%. In one embodiment, the elastic modulus of the second adhesive layer at 25°C is 9.0×10 4 Pa or less, preferably 1.0×10 3 Pa to 9.0×10 4 Pa, and more preferably 1.0×10 4 Pa to 8.5×10 4 Pa. In another embodiment, the elastic modulus is 5.0×10 5 Pa or less, preferably 1.0×10 3 Pa to 2.0×10 5 Pa, and more preferably 1.0×10 4 Pa to 1.6×10 5 Pa.
第1及第2黏著劑層之凝膠分率較佳為40%～95%，更佳為50%～95%，進而較佳為65%～93%，尤佳為80%～93%。於黏著劑層之凝膠分率較小之情形時，凝聚力較差，有加工性或處理性出現問題之情形。又，就防止糊凹痕等外觀不良之觀點而言，剛形成黏著劑層後之凝膠分率較佳為60%以上，更佳為63%以上，進而較佳為66%以上，尤佳為70%以上。The gel fraction of the first and second adhesive layers is preferably 40% to 95%, more preferably 50% to 95%, further preferably 65% to 93%, and particularly preferably 80% to 93%. When the gel fraction of the adhesive layer is small, the cohesion is poor, and there may be problems with processability or handling. In addition, from the perspective of preventing poor appearance such as paste dents, the gel fraction immediately after the adhesive layer is formed is preferably 60% or more, more preferably 63% or more, further preferably 66% or more, and particularly preferably 70% or more.
構成第1黏著劑層及/或第2黏著劑層之黏著劑可根據目的及用途於黏著劑組合物中包含交聯劑、紫外線吸收劑、色素化合物等。The adhesive constituting the first adhesive layer and/or the second adhesive layer may contain a crosslinking agent, an ultraviolet absorber, a pigment compound, etc. in the adhesive composition according to the purpose and application.
D-1.基礎聚合物 構成第1及第2黏著劑層(以下，有時簡稱為「黏著劑層」)之黏著劑只要滿足上述特性，則可由任意適當之材料形成。於一實施形態中，作為構成黏著劑層之黏著劑之基礎聚合物，可列舉(甲基)丙烯酸系聚合物、橡膠系聚合物等。較佳為，基礎聚合物為(甲基)丙烯酸系聚合物。 D-1. Base polymer The adhesive constituting the first and second adhesive layers (hereinafter, sometimes referred to as "adhesive layers") can be formed of any appropriate material as long as it satisfies the above-mentioned characteristics. In one embodiment, as the base polymer of the adhesive constituting the adhesive layer, (meth) acrylic polymers, rubber polymers, etc. can be listed. Preferably, the base polymer is a (meth) acrylic polymer.
(甲基)丙烯酸系聚合物含有作為單體單元之(甲基)丙烯酸烷基酯作為主成分。作為(甲基)丙烯酸烷基酯，可列舉酯末端具有直鏈狀或支鏈狀之碳數1～24之烷基者。(甲基)丙烯酸烷基酯可單獨使用1種或將2種以上組合而使用。再者，「(甲基)丙烯酸烷基酯」係指丙烯酸烷基酯及/或甲基丙烯酸烷基酯。The (meth)acrylic polymer contains an alkyl (meth)acrylate as a monomer unit as a main component. Examples of the alkyl (meth)acrylate include those having a linear or branched alkyl group with 1 to 24 carbon atoms at the end of the ester. The alkyl (meth)acrylate may be used alone or in combination of two or more. In addition, "alkyl (meth)acrylate" refers to alkyl acrylate and/or alkyl methacrylate.
關於構成第1黏著劑層之黏著劑，酯末端具有碳數1～24之烷基之(甲基)丙烯酸烷基酯相對於形成(甲基)丙烯酸系聚合物之單官能性單體成分之總量較佳為40重量%以上，更佳為50重量%以上，進而較佳為60重量%以上。關於構成第2黏著劑層之黏著劑，如上所述，(甲基)丙烯酸烷基酯相對於形成(甲基)丙烯酸系聚合物之單官能性單體成分之總量為70重量%以上。Regarding the adhesive constituting the first adhesive layer, the amount of the alkyl (meth)acrylate having an alkyl group with 1 to 24 carbon atoms at the ester terminal is preferably 40% by weight or more, more preferably 50% by weight or more, and further preferably 60% by weight or more relative to the total amount of the monofunctional monomer components forming the (meth)acrylic polymer. Regarding the adhesive constituting the second adhesive layer, as described above, the amount of the alkyl (meth)acrylate is 70% by weight or more relative to the total amount of the monofunctional monomer components forming the (meth)acrylic polymer.
上述單體成分可包含(甲基)丙烯酸烷基酯以外之共聚單體作為單官能性單體成分。共聚單體可用作單體成分中之(甲基)丙烯酸烷基酯之殘部。作為共聚單體，例如可包含環狀含氮單體。作為上述環狀含氮單體，可使用具有含有(甲基)丙烯醯基或乙烯基等不飽和雙鍵之聚合性官能基且具有環狀氮結構者，並無特別限制。環狀氮結構較佳為環狀結構內具有氮原子者。環狀含氮單體之含量相對於形成(甲基)丙烯酸系聚合物之單官能性單體成分之總量較佳為0.5～50重量%，更佳為0.5～40重量%，進而更佳為0.5～30重量%。The above-mentioned monomer component may contain a copolymer monomer other than the (meth) alkyl ester as a monofunctional monomer component. The copolymer monomer may be used as a residue of the (meth) alkyl ester in the monomer component. As a copolymer monomer, for example, a cyclic nitrogen-containing monomer may be included. As the above-mentioned cyclic nitrogen-containing monomer, a monomer having a polymerizable functional group containing an unsaturated double bond such as a (meth)acryl group or a vinyl group and having a cyclic nitrogen structure may be used without any particular limitation. The cyclic nitrogen structure is preferably one having a nitrogen atom in the cyclic structure. The content of the cyclic nitrogen-containing monomer is preferably 0.5 to 50% by weight, more preferably 0.5 to 40% by weight, and even more preferably 0.5 to 30% by weight relative to the total amount of the monofunctional monomer component forming the (meth) acrylic polymer.
形成(甲基)丙烯酸系聚合物之單體成分可包含其他含官能基單體。作為此種單體，例如可列舉含羧基單體、具有環狀醚基之單體。於含有含羧基單體之情形時，含量較佳為0.05～10重量%，更佳為0.1～8重量%，進而較佳為0.2～6重量%。藉由含有含羧基單體，可將黏著劑層之凝膠分率設為較佳範圍內之值，其結果為，可抑制相位差層中之龜裂之產生。The monomer component forming the (meth)acrylic polymer may include other functional group-containing monomers. Examples of such monomers include carboxyl group-containing monomers and monomers having a cyclic ether group. When a carboxyl group-containing monomer is contained, the content is preferably 0.05 to 10% by weight, more preferably 0.1 to 8% by weight, and further preferably 0.2 to 6% by weight. By containing a carboxyl group-containing monomer, the gel fraction of the adhesive layer can be set to a value within a preferred range, and as a result, the generation of cracks in the phase difference layer can be suppressed.
又，上述單體成分可含有含羥基單體。作為含羥基單體，可使用具有含有(甲基)丙烯醯基或乙烯基等不飽和雙鍵之聚合性官能基且具有羥基者，並無特別限制。就提高接著力、凝聚力之方面而言，上述含羥基單體之含量相對於形成(甲基)丙烯酸系聚合物之單官能性單體成分之總量較佳為1重量%以上，更佳為2重量%以上，進而較佳為3重量%以上。另一方面，含羥基單體之含量之上限相對於形成(甲基)丙烯酸系聚合物之單官能性單體成分之總量較佳為30重量%，更佳為27重量%，進而較佳為25重量%。若含羥基單體過多，則有黏著劑層變硬、接著力降低之情形，又，有黏著劑之黏度過高之情形。Furthermore, the above-mentioned monomer component may contain a hydroxyl-containing monomer. As the hydroxyl-containing monomer, a polymerizable functional group containing an unsaturated double bond such as a (meth)acryl group or a vinyl group and having a hydroxyl group can be used without any particular limitation. In terms of improving adhesion and cohesion, the content of the above-mentioned hydroxyl-containing monomer is preferably 1% by weight or more, more preferably 2% by weight or more, and further preferably 3% by weight or more, relative to the total amount of the monofunctional monomer components forming the (meth)acrylic polymer. On the other hand, the upper limit of the content of the hydroxyl-containing monomer is preferably 30% by weight, more preferably 27% by weight, and further preferably 25% by weight relative to the total amount of the monofunctional monomer components forming the (meth)acrylic polymer. If the amount of hydroxyl monomer is too high, the adhesive layer may become hard and the adhesive strength may decrease. Also, the viscosity of the adhesive may be too high.
於形成(甲基)丙烯酸系聚合物之單體成分中，除上述單官能性單體外，可視需要含有任意適當之多官能性單體以調整黏著劑之凝聚力。The monomer components forming the (meth)acrylic polymer may contain any appropriate multifunctional monomer in addition to the above-mentioned monofunctional monomers as needed to adjust the cohesive force of the adhesive.
(甲基)丙烯酸系聚合物通常係使用重量平均分子量為50萬～300萬之範圍者。若考慮耐久性、尤其是耐熱性，較佳為使用重量平均分子量為70萬～270萬者。進而較佳為80萬～250萬。若重量平均分子量小於50萬，則耐熱性方面欠佳。又，若重量平均分子量大於300萬，則需要大量之稀釋溶劑以調整至適於塗敷之黏度，導致成本上升，故而欠佳。再者，重量平均分子量係指藉由GPC(凝膠滲透層析法)進行測定並利用聚苯乙烯換算而算出之值。構成第1黏著劑層之黏著劑之(甲基)丙烯酸系聚合物之重量平均分子量較佳為150萬～250萬，更佳為180萬～230萬。構成第2黏著劑層之黏著劑之(甲基)丙烯酸系聚合物之重量平均分子量較佳為100萬～200萬，更佳為120萬～180萬。(Meth)acrylic polymers generally have a weight average molecular weight of 500,000 to 3,000,000. Considering durability, especially heat resistance, it is preferred to use a weight average molecular weight of 700,000 to 2,700,000. Further preferred is 800,000 to 2,500,000. If the weight average molecular weight is less than 500,000, the heat resistance is poor. Furthermore, if the weight average molecular weight is greater than 3,000,000, a large amount of diluent is required to adjust the viscosity to a suitable coating viscosity, resulting in increased costs, which is not preferred. Furthermore, the weight average molecular weight refers to the value measured by GPC (gel permeation chromatography) and calculated by polystyrene conversion. The weight average molecular weight of the (meth)acrylic polymer of the adhesive constituting the first adhesive layer is preferably 1,500,000 to 2,500,000, and more preferably 1,800,000 to 2,300,000. The weight average molecular weight of the (meth)acrylic acid polymer of the adhesive constituting the second adhesive layer is preferably 1 million to 2 million, more preferably 1.2 million to 1.8 million.
作為(甲基)丙烯酸系聚合物之製造方法，可採用溶液聚合、紫外線(UV)聚合等輻射聚合、塊狀聚合、乳化聚合等各種自由基聚合等任意適當之方法。又，所獲得之(甲基)丙烯酸系聚合物可為無規共聚物、嵌段共聚物、接枝共聚物等之任一種。As a method for producing a (meth)acrylic acid-based polymer, any appropriate method may be adopted, such as solution polymerization, radiation polymerization such as ultraviolet (UV) polymerization, block polymerization, various free radical polymerizations such as emulsion polymerization, etc. In addition, the obtained (meth)acrylic acid-based polymer may be any of a random copolymer, a block copolymer, a graft copolymer, etc.
於藉由自由基聚合製造(甲基)丙烯酸系聚合物之情形時，可向單體成分適當添加用於自由基聚合之聚合起始劑、鏈轉移劑、乳化劑等而進行聚合。用於自由基聚合之聚合起始劑、鏈轉移劑、乳化劑等並無特別限定，可適當選擇而使用。再者，(甲基)丙烯酸系聚合物之重量平均分子量可利用聚合起始劑、鏈轉移劑之使用量、反應條件進行控制，可根據其等之種類適當調整其使用量。When a (meth)acrylic acid polymer is produced by free radical polymerization, a polymerization initiator, a chain transfer agent, an emulsifier, etc. used for free radical polymerization can be appropriately added to the monomer component to perform polymerization. The polymerization initiator, chain transfer agent, emulsifier, etc. used for free radical polymerization are not particularly limited and can be appropriately selected and used. Furthermore, the weight average molecular weight of the (meth)acrylic acid polymer can be controlled by the amount of the polymerization initiator and chain transfer agent used and the reaction conditions, and the amount used can be appropriately adjusted according to the type of the polymerization initiator and chain transfer agent.
於藉由輻射聚合製造(甲基)丙烯酸系聚合物之情形時，可藉由向單體成分照射電子束、紫外線(UV)等放射線進行聚合而製造。該等之中，較佳為紫外線聚合。於進行紫外線聚合時，由於可縮短聚合時間之優點等，故而較佳為使單體成分含有光聚合起始劑。When the (meth)acrylic polymer is produced by radiation polymerization, it can be produced by irradiating the monomer component with radiation such as electron beams, ultraviolet rays (UV) and the like. Among these, ultraviolet polymerization is preferred. When ultraviolet polymerization is performed, it is preferred that the monomer component contains a photopolymerization initiator because of the advantage of shortening the polymerization time.
光聚合起始劑並無特別限定，較佳為於波長400 nm以上具有吸收帶之光聚合起始劑。作為此種光聚合起始劑，可列舉雙(2,4,6-三甲基苯甲醯基)-苯基氧化膦(BASF公司製造、製品名「Irgacure819」)、2,4,6-三甲基苯甲醯基-二苯基-氧化膦(BASF公司製造、「LUCIRIN TPO」)等。The photopolymerization initiator is not particularly limited, but preferably has an absorption band at a wavelength of 400 nm or more. Examples of such photopolymerization initiators include bis(2,4,6-trimethylbenzyl)-phenylphosphine oxide (manufactured by BASF, product name "Irgacure 819"), 2,4,6-trimethylbenzyl-diphenyl-phosphine oxide (manufactured by BASF, "LUCIRIN TPO"), and the like.
光聚合起始劑可含有於未達波長400 nm具有吸收帶之光聚合起始劑。作為此種光聚合起始劑，只要為藉由紫外線產生自由基並開始進行光聚合者，且為於未達波長400 nm具有吸收帶者，則並無特別限制，可適當使用通常所使用之任一種光聚合起始劑。例如，可使用：安息香醚系光聚合起始劑、苯乙酮系光聚合起始劑、α-酮醇系光聚合起始劑、光活性肟系光聚合起始劑、苯偶姻系光聚合起始劑、苯偶醯系光聚合起始劑、二苯甲酮系光聚合起始劑、縮酮系光聚合起始劑、9-氧硫𠮿系光聚合起始劑、醯基氧化膦系光聚合起始劑等。The photopolymerization initiator may contain a photopolymerization initiator having an absorption band at a wavelength less than 400 nm. As such a photopolymerization initiator, there is no particular limitation as long as it generates free radicals by ultraviolet light and starts photopolymerization, and has an absorption band at a wavelength less than 400 nm. Any commonly used photopolymerization initiator may be appropriately used. For example, benzoin ether-based photopolymerization initiators, acetophenone-based photopolymerization initiators, α-ketol-based photopolymerization initiators, photoactive oxime-based photopolymerization initiators, benzoin-based photopolymerization initiators, benzoyl-based photopolymerization initiators, benzophenone-based photopolymerization initiators, ketal-based photopolymerization initiators, 9-oxysulfonium-based photopolymerization initiators, and the like may be used. Photopolymerization initiator, acylphosphine oxide photopolymerization initiator, etc.
D-2.交聯劑 作為交聯劑，包含異氰酸酯系交聯劑、環氧系交聯劑、聚矽氧系交聯劑、㗁唑啉系交聯劑、氮丙啶系交聯劑、矽烷系交聯劑、烷基醚化三聚氰胺系交聯劑、金屬螯合物系交聯劑之交聯劑。交聯劑可單獨使用1種或將2種以上組合而使用。該等之中，較佳為使用異氰酸酯系交聯劑。 D-2. Crosslinking agent As the crosslinking agent, there are crosslinking agents including isocyanate crosslinking agents, epoxy crosslinking agents, polysiloxane crosslinking agents, oxazoline crosslinking agents, aziridine crosslinking agents, silane crosslinking agents, alkyl etherified melamine crosslinking agents, and metal chelate crosslinking agents. The crosslinking agent can be used alone or in combination of two or more. Among them, isocyanate crosslinking agents are preferably used.
於黏著劑中，相對於基礎聚合物100重量份之異氰酸酯交聯劑之含量較佳為0.1重量份～12重量份。In the adhesive, the content of the isocyanate crosslinking agent is preferably 0.1 to 12 parts by weight relative to 100 parts by weight of the base polymer.
異氰酸酯交聯劑係指1分子中具有2個以上之異氰酸基(包含藉由封端劑或數量體化等暫時地保護異氰酸基而成之異氰酸酯再生型官能基)之化合物。作為異氰酸酯交聯劑，可列舉：甲苯二異氰酸酯、二甲苯二異氰酸酯等芳香族異氰酸酯、異佛爾酮二異氰酸酯等脂環族異氰酸酯、六亞甲基二異氰酸酯等脂肪族異氰酸酯等。Isocyanate crosslinking agents refer to compounds having two or more isocyanate groups in one molecule (including isocyanate regeneration functional groups formed by temporarily protecting isocyanate groups by blocking agents or molecularization). Examples of isocyanate crosslinking agents include aromatic isocyanates such as toluene diisocyanate and xylene diisocyanate, alicyclic isocyanates such as isophorone diisocyanate, and aliphatic isocyanates such as hexamethylene diisocyanate.
更具體而言，例如可列舉：伸丁基二異氰酸酯、六亞甲基二異氰酸酯等低級脂肪族聚異氰酸酯類、伸環戊基二異氰酸酯、伸環己基二異氰酸酯、異佛爾酮二異氰酸酯等脂環族異氰酸酯類、2,4-甲苯二異氰酸酯、4,4'-二苯甲烷二異氰酸酯、二甲苯二異氰酸酯、聚亞甲基聚苯異氰酸酯等芳香族二異氰酸酯類、三羥甲基丙烷/甲苯二異氰酸酯三聚物加成物(Nippon Polyurethane Industry股份有限公司製造、製品名「Coronate L」)、三羥甲基丙烷/六亞甲基二異氰酸酯三聚物加成物(Nippon Polyurethane Industry股份有限公司製造、製品名「Coronate HL」)、六亞甲基二異氰酸酯之異氰尿酸酯體(Nippon Polyurethane Industry股份有限公司製造、製品名「Coronate HX」)等異氰酸酯加成物、二甲苯二異氰酸酯之三羥甲基丙烷加成物(三井化學股份有限公司製造、製品名「D110N」)、六亞甲基二異氰酸酯之三羥甲基丙烷加成物(三井化學股份有限公司製造、製品名「D160N」)；聚醚聚異氰酸酯、聚酯聚異氰酸酯、以及該等與各種多元醇之加成物、利用異氰尿酸酯鍵、縮二脲鍵、脲基甲酸酯鍵等進行多官能化而成之聚異氰酸酯等。其中，作為構成第1黏著劑層之黏著劑之交聯劑，適宜使用三羥甲基丙烷甲苯二異氰酸酯，作為構成第2黏著劑層之黏著劑之交聯劑，適宜使用三羥甲基丙烷二甲苯二異氰酸酯，適宜使用三羥甲基丙烷二甲苯二異氰酸酯。More specifically, for example, low-order aliphatic polyisocyanates such as butyl diisocyanate and hexamethylene diisocyanate, alicyclic isocyanates such as cyclopentyl diisocyanate, cyclohexyl diisocyanate, and isophorone diisocyanate, aromatic diisocyanates such as 2,4-toluene diisocyanate, 4,4'-diphenylmethane diisocyanate, xylene diisocyanate, and polymethylene polyphenylene isocyanate, trihydroxymethylpropane/toluene diisocyanate trimer adduct (manufactured by Nippon Polyurethane Industry Co., Ltd., product name "Coronate L"), trihydroxymethylpropane/hexamethylene diisocyanate trimer adduct (manufactured by Nippon Polyurethane Industry Co., Ltd., product name "Coronate Isocyanate adducts such as isocyanurate of hexamethylene diisocyanate (manufactured by Nippon Polyurethane Industry Co., Ltd., product name "Coronate HX"), trihydroxymethylpropane adduct of xylene diisocyanate (manufactured by Mitsui Chemicals Co., Ltd., product name "D110N"), trihydroxymethylpropane adduct of hexamethylene diisocyanate (manufactured by Mitsui Chemicals Co., Ltd., product name "D160N"); polyether polyisocyanates, polyester polyisocyanates, and adducts of these with various polyols, polyisocyanates obtained by multifunctionalization using isocyanurate bonds, biuret bonds, allophanate bonds, etc. Among them, trihydroxymethylpropane toluene diisocyanate is preferably used as a crosslinking agent for the adhesive constituting the first adhesive layer, trihydroxymethylpropane xylene diisocyanate is preferably used as a crosslinking agent for the adhesive constituting the second adhesive layer, and trihydroxymethylpropane xylene diisocyanate is preferably used.
D-3.紫外線吸收劑 作為紫外線吸收劑，可使用任意適當之紫外線吸收劑。紫外線吸收劑較佳為於分子結構中具有0個～3個羥基。具體而言，可列舉：三𠯤系紫外線吸收劑、苯并***系紫外線吸收劑、二苯甲酮系紫外線吸收劑、氧基二苯甲酮系紫外線吸收劑、水楊酸酯系紫外線吸收劑、氰基丙烯酸酯系紫外線吸收劑等，該等可單獨使用1種或將2種以上組合而使用。該等之中，較佳為三𠯤系紫外線吸收劑、苯并***系紫外線吸收劑，若為選自由1分子中具有2個以下之羥基之三𠯤系紫外線吸收劑、及1分子中具有1個苯并***骨架之苯并***系紫外線吸收劑所組成之群中之至少1種紫外線吸收劑，則於形成丙烯酸系黏著劑組合物所使用之單體中之溶解性良好，且波長380 nm附近之紫外線吸收能力較高，故而較佳。紫外線吸收劑可單獨使用，又，亦可將2種以上混合而使用。 D-3. Ultraviolet absorber As the ultraviolet absorber, any appropriate ultraviolet absorber can be used. The ultraviolet absorber preferably has 0 to 3 hydroxyl groups in the molecular structure. Specifically, there can be listed: trioxane ultraviolet absorbers, benzotriazole ultraviolet absorbers, benzophenone ultraviolet absorbers, oxybenzophenone ultraviolet absorbers, salicylic acid ester ultraviolet absorbers, cyanoacrylate ultraviolet absorbers, etc. These can be used alone or in combination of two or more. Among them, trioxane-based ultraviolet absorbers and benzotriazole-based ultraviolet absorbers are preferred. At least one ultraviolet absorber selected from the group consisting of trioxane-based ultraviolet absorbers having two or less hydroxyl groups in one molecule and benzotriazole-based ultraviolet absorbers having one benzotriazole skeleton in one molecule is preferred because it has good solubility in the monomer used to form the acrylic adhesive composition and has a higher ability to absorb ultraviolet light around a wavelength of 380 nm. The ultraviolet absorber can be used alone or in combination of two or more.
D-4.色素化合物 色素化合物較佳為吸收光譜之最大吸收波長存在於380 nm～430 nm之波長區域。藉由將此種色素化合物與紫外線吸收劑組合而使用，可充分地吸收不會對有機EL元件之發光造成影響之區域(波長380 nm～430 nm)之光，且可充分地透過有機EL元件之發光區域(較430 nm長之波長側)。 D-4. Pigment compound The pigment compound preferably has a maximum absorption wavelength in the wavelength region of 380 nm to 430 nm in the absorption spectrum. By using such a pigment compound in combination with a UV absorber, it is possible to fully absorb light in the region (wavelength 380 nm to 430 nm) that does not affect the luminescence of the organic EL element, and to fully transmit the light emitting region of the organic EL element (the wavelength side longer than 430 nm).
色素化合物之半值寬較佳為80 nm以下，更佳為5 nm～70 nm，進而較佳為10 nm～60 nm。藉此，可充分地吸收不會對有機EL元件之發光造成影響之區域之光，並且可使較430 nm長之波長側之光充分地透過。The half-value width of the pigment compound is preferably 80 nm or less, more preferably 5 nm to 70 nm, and further preferably 10 nm to 60 nm. This allows sufficient absorption of light in a region that does not affect the luminescence of the organic EL element, and sufficient transmission of light at a wavelength longer than 430 nm.
D-5.其他成分 黏著劑組合物可視需要包含矽烷偶合劑、抗氧化劑、防老化劑、塑化劑等其他成分。作為抗氧化劑，例如可列舉酚系、磷系、硫系、胺系抗氧化劑。作為矽烷偶合劑，例如可列舉：3-縮水甘油氧基丙基三甲氧基矽烷等含環氧基矽烷偶合劑、3-胺基丙基三甲氧基矽烷等含胺基矽烷偶合劑、3-丙烯醯氧基丙基三甲氧基矽烷等含(甲基)丙烯酸基矽烷偶合劑、3-異氰酸基丙基三乙氧基矽烷等含異氰酸基矽烷偶合劑、含乙醯乙醯基矽烷偶合劑。 D-5. Other ingredients The adhesive composition may contain other ingredients such as silane coupling agents, antioxidants, anti-aging agents, plasticizers, etc. as needed. Examples of antioxidants include phenolic, phosphorus, sulfur, and amine antioxidants. Examples of silane coupling agents include epoxy-containing silane coupling agents such as 3-glycidyloxypropyltrimethoxysilane, amino-containing silane coupling agents such as 3-aminopropyltrimethoxysilane, (meth)acrylic-containing silane coupling agents such as 3-acryloxypropyltrimethoxysilane, isocyanate-containing silane coupling agents such as 3-isocyanatopropyltriethoxysilane, and acetoacetyl-containing silane coupling agents.
E.表面保護膜 如上所述，附相位差層之偏光板亦可於偏光板之視認側進而具有表面保護膜。代表性而言，表面保護膜包含基材及黏著劑層。表面保護膜之基材及黏著劑層可採用業界眾所周知之構成，故而省略詳細之說明。 E. Surface protection film As described above, the polarizing plate with a phase difference layer may also have a surface protection film on the visual side of the polarizing plate. Typically, the surface protection film includes a substrate and an adhesive layer. The substrate and adhesive layer of the surface protection film may adopt a structure well known in the industry, so a detailed description is omitted.
表面保護膜之厚度(基材與黏著劑層之合計厚度)較佳為40 μm～90 μm，更佳為60 μm～90 μm。若表面保護膜之厚度為此種範圍，則可獲得不易產生劃痕之附相位差層之偏光板。The thickness of the surface protection film (the total thickness of the substrate and the adhesive layer) is preferably 40 μm to 90 μm, more preferably 60 μm to 90 μm. If the thickness of the surface protection film is within this range, a polarizing plate with a phase difference layer that is not prone to scratches can be obtained.
F.有機EL顯示裝置 上述A至D項所記載之附相位差層之偏光板可用於圖像顯示裝置。因此，本發明亦包含使用此種光學積層體之圖像顯示裝置。作為圖像顯示裝置之代表例，可列舉液晶顯示裝置、有機電致發光(EL)顯示裝置。本發明之實施形態之圖像顯示裝置(有機EL顯示裝置)具備上述A項至D項所記載之光學積層體。 實施例 F. Organic EL display device The polarizing plate with phase difference layer described in items A to D above can be used in an image display device. Therefore, the present invention also includes an image display device using such an optical multilayer body. As representative examples of image display devices, liquid crystal display devices and organic electroluminescent (EL) display devices can be cited. The image display device (organic EL display device) of the embodiment of the present invention has the optical multilayer body described in items A to D above. Example
以下，藉由實施例具體地說明本發明，但本發明並不限定於該等實施例。再者，各特性之測定方法如下所述。 (1)厚度 使用干渉膜厚計(大塚電子股份有限公司製造、MCPD2000)測定相位差層之厚度。又，使用數位式測微計(Anritsu股份有限公司製造、KC-351C)測定相位差層以外之層之厚度。 (2)相位差值 藉由自動雙折射測定裝置(王子計測機器股份有限公司製造，自動雙折射計KOBRA-WPR)對相位差層之折射率nx、ny及nz進行計測，並算出面內相位差Re及厚度方向相位差Rth。 (3)黏著劑層之彈性模數 關於實施例及比較例中使用之黏著劑，藉由動態黏彈性測定裝置(商品名：ARES、Rheometrics公司製造)測定儲存模數G´之溫度依存性，並將25℃時之測定值G´(25℃)設為彈性模數。 Hereinafter, the present invention will be specifically described by way of examples, but the present invention is not limited to such examples. In addition, the measuring methods of the various characteristics are as follows. (1) Thickness The thickness of the phase difference layer was measured using an interference film thickness meter (manufactured by Otsuka Electronics Co., Ltd., MCPD2000). In addition, the thickness of layers other than the phase difference layer was measured using a digital micrometer (manufactured by Anritsu Co., Ltd., KC-351C). (2) Phase difference value The refractive indices nx, ny, and nz of the phase difference layer were measured using an automatic birefringence measuring device (manufactured by Oji Testing Instruments Co., Ltd., automatic birefractometer KOBRA-WPR), and the in-plane phase difference Re and the thickness direction phase difference Rth were calculated. (3) Elastic modulus of adhesive layer Regarding the adhesive used in the embodiment and the comparative example, the temperature dependence of the storage modulus G' was measured by a dynamic viscoelasticity measuring device (trade name: ARES, manufactured by Rheometrics), and the measured value G'(25°C) at 25°C was set as the elastic modulus.
＜製造例1＞ (偏光板之製作) 藉由輥延伸機將厚度30 μm之聚乙烯醇膜(Kuraray製造，製品名「PE3000」)之長條輥以於長條方向成為5.9倍之方式沿長條方向單軸延伸並且同時實施膨潤、染色、交聯、洗淨處理，最後實施乾燥處理，藉此製作厚度12 μm之偏光元件。 具體而言，膨潤處理係一面利用20℃之純水進行處理一面延伸至2.2倍。繼而，染色處理係一面以所製作之偏光膜之透過率成為45.0%之方式於碘濃度經調整之碘與碘化鉀之重量比為1：7之30℃之水溶液中進行處理一面延伸至1.4倍。進而，交聯處理係採用2階段之交聯處理，第1階段之交聯處理係一面於40℃之溶解有硼酸及碘化鉀之水溶液中進行處理一面延伸至1.2倍。第1階段之交聯處理之水溶液之硼酸含量係設為5.0重量%，碘化鉀含量係設為3.0重量%。第2階段之交聯處理係一面於65℃之溶解有硼酸及碘化鉀之水溶液中進行處理一面延伸至1.6倍。第2階段之交聯處理之水溶液之硼酸含量係設為4.3重量%，碘化鉀含量係設為5.0重量%。又，洗淨處理係利用20℃之碘化鉀水溶液進行處理。洗淨處理之水溶液之碘化鉀含量係設為2.6重量%。最後，乾燥處理係於70℃乾燥5分鐘而獲得偏光元件。 於所獲得之偏光元件之兩面分別經由聚乙烯醇系接著劑貼合Konica Minolta股份有限公司製造之TAC膜(製品名：KC2UA，厚度：25 μm)，且於該TAC膜之單面貼合具有HC層之HC-TAC膜(厚度：32 μm)而獲得於偏光元件之兩面貼合有保護膜之偏光板1。 <Production Example 1> (Production of polarizing plate) A 30 μm thick polyvinyl alcohol film (manufactured by Kuraray, product name "PE3000") was stretched uniaxially in the longitudinal direction by a roll stretching machine in a manner that the film was stretched 5.9 times in the longitudinal direction, and swelling, dyeing, crosslinking, washing, and finally drying were performed to produce a polarizing element with a thickness of 12 μm. Specifically, the swelling treatment was performed while stretching the film to 2.2 times using pure water at 20°C. Subsequently, the dyeing treatment was performed while stretching the film to 1.4 times in a 30°C aqueous solution in which the weight ratio of iodine to potassium iodide was adjusted to 1:7 in a manner that the transmittance of the produced polarizing film was 45.0%. Furthermore, the crosslinking treatment adopts a two-stage crosslinking treatment. The first stage of the crosslinking treatment is to extend the crosslinking treatment to 1.2 times while being treated in an aqueous solution containing boric acid and potassium iodide at 40°C. The boric acid content of the aqueous solution in the first stage of the crosslinking treatment is set to 5.0% by weight, and the potassium iodide content is set to 3.0% by weight. The second stage of the crosslinking treatment is to extend the crosslinking treatment to 1.6 times while being treated in an aqueous solution containing boric acid and potassium iodide at 65°C. The boric acid content of the aqueous solution in the second stage of the crosslinking treatment is set to 4.3% by weight, and the potassium iodide content is set to 5.0% by weight. In addition, the washing treatment is carried out using a potassium iodide aqueous solution at 20°C. The potassium iodide content of the aqueous solution in the washing treatment is set to 2.6% by weight. Finally, the polarizing element was obtained by drying at 70°C for 5 minutes. TAC films (product name: KC2UA, thickness: 25 μm) manufactured by Konica Minolta Co., Ltd. were bonded to both sides of the obtained polarizing element via a polyvinyl alcohol-based adhesive, and an HC-TAC film (thickness: 32 μm) having an HC layer was bonded to one side of the TAC film to obtain a polarizing plate 1 with protective films bonded to both sides of the polarizing element.
＜製造例2＞ (相位差層A之製作) 將顯示向列型液晶相之聚合性液晶(BASF公司製造、商品名「Paliocolor LC242」、由下式表示)10 g、及針對該聚合性液晶化合物之光聚合起始劑(Ciba Specialty Chemicals公司製造、商品名「Irgacure907」)3 g溶解於甲苯40 g而製備液晶組合物(塗敷液)。 [化2] 使用磨擦布磨擦聚對苯二甲酸乙二酯(PET)膜(厚度38 μm)之表面而實施配向處理。關於配向處理之條件，磨擦次數(磨擦輥個數)為1，磨擦輥半徑r為76.89 mm，磨擦輥轉速nr為1500 rpm，膜搬送速度v為83 mm/sec，磨擦強度RS及壓入量M係如表1所示之5種條件(a)～(e)。 <Production Example 2> (Production of Phase Difference Layer A) 10 g of polymerizable liquid crystal showing a nematic liquid crystal phase (manufactured by BASF, trade name "Paliocolor LC242", represented by the following formula) and 3 g of a photopolymerization initiator for the polymerizable liquid crystal compound (manufactured by Ciba Specialty Chemicals, trade name "Irgacure907") were dissolved in 40 g of toluene to prepare a liquid crystal composition (coating liquid). [Chemistry 2] The surface of a polyethylene terephthalate (PET) film (thickness 38 μm) was rubbed with a rubbing cloth to perform an alignment treatment. Regarding the conditions for the alignment treatment, the number of rubbing times (number of rubbing rollers) was 1, the radius of the rubbing roller r was 76.89 mm, the rotation speed of the rubbing roller nr was 1500 rpm, the film transport speed v was 83 mm/sec, and the friction strength RS and the pressure M were the five conditions (a) to (e) shown in Table 1.
[表1]
配向處理之方向係於與偏光板貼附時相對於偏光元件之吸收軸之方向自視認側觀察為-75°方向。利用棒式塗佈機將上述塗敷液塗敷至該配向處理表面並於90℃下加熱乾燥2分鐘，藉此使液晶化合物配向。於條件(a)～(c)下，液晶化合物之配向狀態非常良好。於條件(d)及(e)下，液晶化合物之配向出現少許混亂，但為實際使用中沒有問題之程度。使用金屬鹵化物燈向以此方式形成之液晶層照射1 mJ/cm 2之光使該液晶層硬化，藉此於PET膜上形成相位差層A。相位差層A之厚度為2 μm，面內相位差Re為270 nm。進而，相位差層A具有nx＞ny＝nz之折射率分佈。將相位差層A設為第1相位差層。 The direction of the alignment treatment is -75° relative to the direction of the absorption axis of the polarizing element when attached to the polarizing plate, as viewed from the viewing side. The above-mentioned coating liquid is applied to the alignment-treated surface using a rod coater and dried at 90°C for 2 minutes to align the liquid crystal compound. Under conditions (a) to (c), the alignment state of the liquid crystal compound is very good. Under conditions (d) and (e), the alignment of the liquid crystal compound is slightly disordered, but it is to a degree that there is no problem in actual use. A metal halide lamp is used to irradiate the liquid crystal layer formed in this way with 1 mJ/ cm2 of light to harden the liquid crystal layer, thereby forming a phase difference layer A on the PET film. The thickness of the phase difference layer A is 2 μm, and the in-plane phase difference Re is 270 nm. Furthermore, the phase difference layer A has a refractive index distribution of nx>ny=nz. The phase difference layer A is set as the first phase difference layer.
＜製造例3＞ (相位差層B之製作) 使用磨擦布磨擦聚對苯二甲酸乙二酯(PET)膜(厚度38 μm)表面而實施配向處理。配向處理之方向係於與偏光板貼附時相對於偏光元件之吸收軸之方向自視認側觀察為-15°方向。向該配向處理表面塗敷與上文相同之液晶塗敷液，並以與上文相同之方式使液晶配向及硬化，從而於PET膜上形成相位差層B。相位差層B之厚度為1.2 μm，面內相位差Re為140 nm。進而，相位差層B具有nx＞ny＝nz之折射率分佈。將相位差層B設為第2相位差層。 <Production Example 3> (Production of Phase Difference Layer B) The surface of a polyethylene terephthalate (PET) film (thickness 38 μm) was rubbed with a rubbing cloth to perform an alignment treatment. The direction of the alignment treatment is -15° relative to the direction of the absorption axis of the polarizing element when attached to the polarizing plate. The same liquid crystal coating liquid as above was applied to the alignment-treated surface, and the liquid crystal was aligned and cured in the same manner as above, thereby forming a phase difference layer B on the PET film. The thickness of the phase difference layer B is 1.2 μm, and the in-plane phase difference Re is 140 nm. Furthermore, the phase difference layer B has a refractive index distribution of nx＞ny＝nz. The phase difference layer B is set as the second phase difference layer.
＜製造例4＞ (黏著劑A之製作) 向具備冷卻管、氮導入管、溫度計及攪拌裝置之反應容器中，與乙酸乙酯一併添加丙烯酸丁酯94.9份、丙烯酸5份、丙烯酸2-羥基乙酯0.1份、及相對於單體(固形物成分)100份為0.3份之過氧化二苯甲醯，於氮氣氣流下於60℃反應7小時之後，向該反應液添加乙酸乙酯而獲得含有重量平均分子量220萬之丙烯酸系聚合物之溶液(固形物成分濃度30重量%)。相對於上述丙烯酸系聚合物溶液之固形物成分100份調配0.6份之三羥甲基丙烷甲苯二異氰酸酯(Nippon Polyurethane股份有限公司製造、製品名「Coronate L」)、及0.075份之γ-縮水甘油氧基丙基甲氧基矽烷(信越化學工業股份有限公司製造、製品名「KBM-403」)而獲得黏著劑組合物(溶液)。 將上述黏著劑組合物塗敷至包含利用聚矽氧系剝離劑進行過表面處理之聚酯膜之隔離件，並於155℃加熱處理3分鐘而獲得特定厚度之黏著劑A。黏著劑A於25℃下之彈性模數為1.4×10 5Pa。 <Production Example 4> (Production of Adhesive A) Into a reaction container equipped with a cooling tube, a nitrogen inlet tube, a thermometer and a stirring device, 94.9 parts of butyl acrylate, 5 parts of acrylic acid, 0.1 parts of 2-hydroxyethyl acrylate, and 0.3 parts of dibenzoyl peroxide relative to 100 parts of monomers (solid content) were added together with ethyl acetate, and the mixture was reacted at 60°C for 7 hours under a nitrogen flow. Ethyl acetate was then added to the reaction solution to obtain a solution containing an acrylic polymer having a weight average molecular weight of 2.2 million (solid content concentration 30% by weight). An adhesive composition (solution) was obtained by mixing 0.6 parts of trihydroxymethylpropane toluene diisocyanate (manufactured by Nippon Polyurethane Co., Ltd., product name "Coronate L") and 0.075 parts of γ-glycidyloxypropyl methoxysilane (manufactured by Shin-Etsu Chemical Co., Ltd., product name "KBM-403") with respect to 100 parts of the solid content of the acrylic polymer solution. The adhesive composition was applied to a separator including a polyester film surface-treated with a silicone-based release agent and heat-treated at 155°C for 3 minutes to obtain an adhesive A of a specific thickness. The elastic modulus of the adhesive A at 25°C was 1.4×10 5 Pa.
＜製造例5＞ (黏著劑B之製作) 向具備冷卻管、氮導入管、溫度計及攪拌裝置之反應容器中，與乙酸乙酯一併添加丙烯酸丁酯99份、丙烯酸4-羥基丁酯1.0份及2,2'-偶氮二異丁腈0.3份，於氮氣氣流下於60℃反應4小時之後，向該反應液添加乙酸乙酯而獲得含有重量平均分子量165萬之丙烯酸系聚合物之溶液(固形物成分濃度30%)。相對於上述丙烯酸系聚合物溶液之固形物成分100份調配0.15份之過氧化二苯甲醯(日本油脂股份有限公司製造、製品名「Nyper BO-Y」)、0.1份之三羥甲基丙烷二甲苯二異氰酸酯(Mitsuitakeda chemicals股份有限公司、製品名「Takenate D110N」)、及0.2份之矽烷偶合劑(綜研化學股份有限公司製造、製品名「A-100」、含乙醯乙醯基矽烷偶合劑)而獲得黏著劑組合物(溶液)。 將上述黏著劑組合物塗敷至包含利用聚矽氧系剝離劑進行過表面處理之聚酯膜之隔離件，並於155℃加熱處理3分鐘而獲得特定厚度之黏著劑B。黏著劑B於25℃下之彈性模數為8.1×10 4Pa。 <Production Example 5> (Production of Adhesive B) Into a reaction container equipped with a cooling tube, a nitrogen inlet tube, a thermometer and a stirring device, 99 parts of butyl acrylate, 1.0 part of 4-hydroxybutyl acrylate and 0.3 part of 2,2'-azobisisobutyronitrile were added together with ethyl acetate, and the mixture was reacted at 60°C for 4 hours under a nitrogen flow. Ethyl acetate was then added to the reaction solution to obtain a solution containing an acrylic polymer having a weight average molecular weight of 1.65 million (solid content concentration 30%). An adhesive composition (solution) was obtained by mixing 0.15 parts of dibenzoyl peroxide (manufactured by NOF Corporation, product name "Nyper BO-Y"), 0.1 parts of trihydroxymethyl propane xylene diisocyanate (manufactured by Mitsuitakeda Chemicals Co., Ltd., product name "Takenate D110N"), and 0.2 parts of a silane coupling agent (manufactured by Soken Chemical Co., Ltd., product name "A-100", containing acetyl acetyl silane coupling agent) with respect to 100 parts of the solid content of the acrylic polymer solution. The adhesive composition was applied to a separator including a polyester film surface-treated with a silicone-based release agent and heat-treated at 155°C for 3 minutes to obtain an adhesive B having a specific thickness. The elastic modulus of adhesive B at 25°C is 8.1×10 4 Pa.
[實施例1] 以偏光元件之吸收軸與第1相位差層之遲相軸之角度成為75°之方式，經由紫外線硬化型接著劑貼合上述偏光板之TAC膜面及第1相位差層。其次，以偏光板之吸收軸與第2相位差層之遲相軸之角度成為15°之方式，經由厚度5 μm之黏著劑A(第1黏著劑層)貼合第1相位差層及第2相位差層。進而，將厚度10 μm之黏著劑A(第2黏著劑層)貼合於第2相位差層之表面，進而於偏光板之視認側貼合表面保護膜(日東電工公司製造、E-MASK RP109F、基材(PET)之厚度38 μm、黏著劑層之厚度10 μm)，從而獲得附相位差層之偏光板1。 [Example 1] The TAC film surface of the polarizing plate and the first phase difference layer are bonded together via a UV curable adhesive in such a manner that the angle between the absorption axis of the polarizing element and the retarded axis of the first phase difference layer is 75°. Next, the first phase difference layer and the second phase difference layer are bonded together via an adhesive A (first adhesive layer) having a thickness of 5 μm in such a manner that the angle between the absorption axis of the polarizing plate and the retarded axis of the second phase difference layer is 15°. Then, an adhesive A (second adhesive layer) with a thickness of 10 μm was bonded to the surface of the second phase difference layer, and a surface protection film (E-MASK RP109F manufactured by Nitto Denko Corporation, with a base material (PET) thickness of 38 μm and an adhesive layer thickness of 10 μm) was bonded to the viewing side of the polarizing plate, thereby obtaining a polarizing plate 1 with a phase difference layer.
[實施例2] 將厚度15 μm之黏著劑B(第2黏著劑層)貼合於第2相位差層之表面，除此以外，以與實施例1相同之方法獲得附相位差層之偏光板2。 [Example 2] A 15 μm thick adhesive B (second adhesive layer) was bonded to the surface of the second phase difference layer. The polarizing plate 2 with a phase difference layer was obtained in the same manner as in Example 1.
[實施例3] 將厚度15 μm之黏著劑A(第2黏著劑層)貼合於第2相位差層之表面，除此以外，以與實施例1相同之方法獲得附相位差層之偏光板3。 [Example 3] A 15 μm thick adhesive A (second adhesive layer) was bonded to the surface of the second phase difference layer. The polarizing plate 3 with a phase difference layer was obtained in the same manner as in Example 1 except that the adhesive A (second adhesive layer) was bonded to the surface of the second phase difference layer.
[實施例4] 將厚度20 μm之黏著劑B(第2黏著劑層)貼合於第2相位差層之表面，除此以外，以與實施例1相同之方法獲得附相位差層之偏光板4。 [Example 4] A 20 μm thick adhesive B (second adhesive layer) was bonded to the surface of the second phase difference layer. The polarizing plate 4 with a phase difference layer was obtained in the same manner as in Example 1.
[實施例5] 將厚度20 μm之黏著劑A(第2黏著劑層)貼合於第2相位差層之表面，除此以外，以與實施例1相同之方法獲得附相位差層之偏光板5。 [Example 5] A 20 μm thick adhesive A (second adhesive layer) was bonded to the surface of the second phase difference layer. The polarizing plate 5 with a phase difference layer was obtained in the same manner as in Example 1 except that the adhesive A (second adhesive layer) was bonded to the surface of the second phase difference layer.
[實施例6] 經由厚度8 μm之黏著劑A(第1黏著劑層)貼合第1相位差層及第2相位差層，且將厚度20 μm之黏著劑B(第2黏著劑層)貼合於第2相位差層之表面，除此以外，以與實施例1相同之方法獲得附相位差層之偏光板6。 [Example 6] The first phase difference layer and the second phase difference layer are bonded via an adhesive A (first adhesive layer) having a thickness of 8 μm, and an adhesive B (second adhesive layer) having a thickness of 20 μm is bonded to the surface of the second phase difference layer. A polarizing plate 6 with a phase difference layer is obtained in the same manner as in Example 1.
[實施例7] 經由厚度10 μm之黏著劑A(第1黏著劑層)貼合第1相位差層及第2相位差層，且將厚度20 μm之黏著劑B(第2黏著劑層)貼合於第2相位差層之表面，除此以外，以與實施例1相同之方法獲得附相位差層之偏光板7。 [Example 7] The first phase difference layer and the second phase difference layer are bonded via an adhesive A (first adhesive layer) having a thickness of 10 μm, and an adhesive B (second adhesive layer) having a thickness of 20 μm is bonded to the surface of the second phase difference layer. A polarizing plate 7 with a phase difference layer is obtained in the same manner as in Example 1.
[實施例8] 經由厚度12 μm之黏著劑A(第1黏著劑層)貼合第1相位差層及第2相位差層，且將厚度20 μm之黏著劑B(第2黏著劑層)貼合於第2相位差層之表面，除此以外，以與實施例1相同之方法獲得附相位差層之偏光板8。 [Example 8] The first phase difference layer and the second phase difference layer are bonded via an adhesive A (first adhesive layer) having a thickness of 12 μm, and an adhesive B (second adhesive layer) having a thickness of 20 μm is bonded to the surface of the second phase difference layer. A polarizing plate 8 with a phase difference layer is obtained in the same manner as in Example 1.
[實施例9] 經由厚度20 μm之黏著劑A(第1黏著劑層)貼合第1相位差層及第2相位差層，除此以外，以與實施例1相同之方法獲得附相位差層之偏光板9。 [Example 9] The first phase difference layer and the second phase difference layer are bonded together via an adhesive A (first adhesive layer) having a thickness of 20 μm. In addition, a polarizing plate 9 with a phase difference layer is obtained in the same manner as in Example 1.
[實施例10] 經由厚度20 μm之黏著劑A(第1黏著劑層)貼合第1相位差層及第2相位差層，且將厚度15 μm之黏著劑B(第2黏著劑層)貼合於第2相位差層之表面，除此以外，以與實施例1相同之方法獲得附相位差層之偏光板10。 [Example 10] The first phase difference layer and the second phase difference layer are bonded via an adhesive A (first adhesive layer) having a thickness of 20 μm, and an adhesive B (second adhesive layer) having a thickness of 15 μm is bonded to the surface of the second phase difference layer. A polarizing plate 10 with a phase difference layer is obtained in the same manner as in Example 1.
[實施例11] 經由厚度20 μm之黏著劑A(第1黏著劑層)貼合第1相位差層及第2相位差層，且將厚度15 μm之黏著劑A(第2黏著劑層)貼合於第2相位差層之表面，除此以外，以與實施例1相同之方法獲得附相位差層之偏光板11。 [Example 11] The first phase difference layer and the second phase difference layer are bonded via an adhesive A (first adhesive layer) having a thickness of 20 μm, and an adhesive A (second adhesive layer) having a thickness of 15 μm is bonded to the surface of the second phase difference layer. A polarizing plate 11 with a phase difference layer is obtained in the same manner as in Example 1.
[實施例12] 經由厚度20 μm之黏著劑A(第1黏著劑層)貼合第1相位差層及第2相位差層，且將厚度20 μm之黏著劑B(第2黏著劑層)貼合於第2相位差層之表面，除此以外，以與實施例1相同之方法獲得附相位差層之偏光板12。 [Example 12] The first phase difference layer and the second phase difference layer are bonded via an adhesive A (first adhesive layer) having a thickness of 20 μm, and an adhesive B (second adhesive layer) having a thickness of 20 μm is bonded to the surface of the second phase difference layer. A polarizing plate 12 with a phase difference layer is obtained in the same manner as in Example 1.
[實施例13] 經由厚度20 μm之黏著劑A(第1黏著劑層)貼合第1相位差層及第2相位差層，且將厚度20 μm之黏著劑A(第2黏著劑層)貼合於第2相位差層之表面，除此以外，以與實施例1相同之方法獲得附相位差層之偏光板13。 [Example 13] The first phase difference layer and the second phase difference layer are bonded via an adhesive A (first adhesive layer) having a thickness of 20 μm, and an adhesive A (second adhesive layer) having a thickness of 20 μm is bonded to the surface of the second phase difference layer. A polarizing plate 13 with a phase difference layer is obtained in the same manner as in Example 1.
[實施例14] 使用與日本專利第6258681號之實施例1相同之方法獲得將基材(PET)之厚度設為75 μm且將黏著劑層之厚度設為10 μm之表面保護膜。 經由厚度20 μm之黏著劑A(第1黏著劑層)貼合第1相位差層及第2相位差層，將厚度20 μm之黏著劑B(第2黏著劑層)貼合於第2相位差層之表面，且使用上述表面保護膜，除此以外，以與實施例1相同之方法獲得附相位差層之偏光板14。 [Example 14] Using the same method as Example 1 of Japanese Patent No. 6258681, a surface protective film with a base material (PET) having a thickness of 75 μm and an adhesive layer having a thickness of 10 μm was obtained. The first phase difference layer and the second phase difference layer were bonded via an adhesive A (first adhesive layer) having a thickness of 20 μm, and an adhesive B (second adhesive layer) having a thickness of 20 μm was bonded to the surface of the second phase difference layer, and the above-mentioned surface protective film was used. In addition, a polarizing plate 14 with a phase difference layer was obtained in the same method as Example 1.
[比較例1] 經由厚度20 μm之黏著劑B(第1黏著劑層)貼合第1相位差層及第2相位差層，且將厚度20 μm之黏著劑B(第2黏著劑層)貼合於第2相位差層之表面，除此以外，以與實施例1相同之方法獲得附相位差層之偏光板15。 [Comparative Example 1] The first phase difference layer and the second phase difference layer are bonded via an adhesive B (first adhesive layer) having a thickness of 20 μm, and an adhesive B (second adhesive layer) having a thickness of 20 μm is bonded to the surface of the second phase difference layer. A polarizing plate 15 with a phase difference layer is obtained in the same manner as in Example 1.
[比較例2] 使用厚度1 μm之紫外線硬化型接著劑(25℃下之彈性模數：大於1.0×10 6Pa)代替黏著劑層C(第1黏著劑層)來貼合第1相位差層及第2相位差層，且將厚度20 μm之黏著劑B(第2黏著劑層)貼合於第2相位差層之表面，除此以外，以與實施例1相同之方法獲得附相位差層之偏光板16。 [Comparative Example 2] A polarizing plate 16 with a phase difference layer is obtained in the same manner as in Example 1 except that a 1 μm thick UV-curable adhesive (elastic modulus at 25°C: greater than 1.0×10 6 Pa) is used instead of adhesive layer C (first adhesive layer) to bond the first phase difference layer and the second phase difference layer, and an adhesive B (second adhesive layer) with a thickness of 20 μm is bonded to the surface of the second phase difference layer.
[參考例1] 將厚度20 μm之黏著劑B(第2黏著劑層)貼合於第2相位差層之表面，除此以外，以與實施例1相同之方法獲得附相位差層之偏光板17。進而，於下述劃痕試驗中，不積層表面保護膜地供於劃痕試驗。 [Reference Example 1] A polarizing plate 17 with a phase difference layer was obtained in the same manner as in Example 1 except that an adhesive B (second adhesive layer) with a thickness of 20 μm was attached to the surface of the second phase difference layer. Furthermore, in the following scratch test, the scratch test was performed without laminating a surface protective film.
[參考例2] 經由厚度20 μm之黏著劑A(第1黏著劑層)貼合第1相位差層及第2相位差層，且將厚度20 μm之黏著劑B(第2黏著劑層)貼合於第2相位差層之表面，除此以外，以與實施例1相同之方法獲得附相位差層之偏光板18。進而，於下述劃痕試驗中，不積層表面保護膜地供於劃痕試驗。 [Reference Example 2] The first phase difference layer and the second phase difference layer are bonded via an adhesive A (first adhesive layer) having a thickness of 20 μm, and an adhesive B (second adhesive layer) having a thickness of 20 μm is bonded to the surface of the second phase difference layer. A polarizing plate 18 with a phase difference layer is obtained in the same manner as in Example 1. Furthermore, in the following scratch test, the scratch test is performed without laminating a surface protective film.
[參考例3] 經由厚度20 μm之黏著劑B(第1黏著劑層)貼合第1相位差層及第2相位差層，且將厚度20 μm之黏著劑B(第2黏著劑層)貼合於第2相位差層之表面，除此以外，以與實施例1相同之方法獲得附相位差層之偏光板19。進而，於下述劃痕試驗中，不積層表面保護膜地供於劃痕試驗。 [Reference Example 3] The first phase difference layer and the second phase difference layer are bonded via an adhesive B (first adhesive layer) having a thickness of 20 μm, and an adhesive B (second adhesive layer) having a thickness of 20 μm is bonded to the surface of the second phase difference layer. A polarizing plate 19 with a phase difference layer is obtained in the same manner as in Example 1. Furthermore, in the following scratch test, the scratch test is performed without laminating a surface protective film.
(評價) 對實施例及比較例中所獲得之附相位差層之偏光板進行下述評價。將結果示於表2。 ＜劃痕試驗＞ 使用手壓輥將附相位差層之偏光板貼合於載玻片(S200423，65×165 mm，松浪硝子工業公司製造)上而製成試樣。將該試樣置於電子天平上。使用鉛筆劃痕值試驗用之鉛筆(三菱鉛筆公司製造)自偏光板表面施加負荷。使負荷變為150 g、300 g及500 g。評價係以n＝10進行。於背光裝置上觀察施加負荷後之上述試樣。將試驗所使用之圓偏光板之逆圓偏光板(NZD-UFQAMEGQ1773VDUHC)夾持於背光裝置與試樣之間並撤銷圓偏振光。由於在該狀態下成為正交狀態，故而將漏光之亮點設為劃痕而進行評價。將劃痕數量為0～3個者設為〇，將4個以上者設為×。 於負荷150 g下，所有附相位差層之偏光板之劃痕數量均為0～3個。於負荷300 g下，附相位差層之偏光板1～7、14及16～17之劃痕數量為0～3個，附相位差層之偏光板8～13、15及18～19之劃痕數量為4個以上。進而，於負荷500 g下，僅附相位差層之偏光板16之劃痕數量為0～3個，附相位差層之偏光板1～15及17～19之劃痕數量為4個以上。 ＜捲曲試驗＞ 於附相位差層之偏光板中，將表面保護膜及偏光板之保護層剝離。供於該試驗之偏光板之大小係設為120 mm×60 mm。將偏光板置於水平之面上，並使用鋼製金屬尺測定中央部距水平面之高度(捲曲值)。若捲曲值為10 mm以內則設為〇，若超過10 mm則設為×。 於附相位差層之偏光板16確認到捲曲之產生，但於附相位差層之偏光板1～15及17～19未確認到捲曲之產生。 ＜耐熱衝擊性＞ 將附相位差層之偏光板裁斷成120 mm×60 mm之尺寸，並經由最表面之黏著劑層B貼合於玻璃而製成試樣。將該試樣投入至熱衝擊試驗機進行熱衝擊試驗，即，於-40℃保持30分鐘之後於85℃保持30分鐘，將其重複進行100個循環，隨後利用光學顯微鏡確認相位差層中之龜裂之有無。 於附相位差層之偏光板15及19中，於相位差層確認到龜裂之產生，但於附相位差層之偏光板1～14及16～18中，未確認到相位差之龜裂。 ＜耐熱性＞ 將附相位差層之偏光板裁斷成120 mm×60 mm之尺寸，並經由最表面之黏著劑層B貼合於玻璃而製成試樣。將該試樣投入至85℃之烘箱保管500小時後，於置於反射板上之狀態下，利用目視確認不均之有無。 於附相位差層之偏光板16中，明顯視認到周邊顏色變紅之不均，對於附相位差層之偏光板1～15及17～19，未視認到不均。 (Evaluation) The polarizing plates with phase difference layers obtained in the embodiments and comparative examples were evaluated as follows. The results are shown in Table 2. <Scratch test> The polarizing plates with phase difference layers were bonded to a glass slide (S200423, 65×165 mm, manufactured by Matsunami Glass Industries) using a hand roller to prepare a sample. The sample was placed on an electronic balance. A load was applied to the surface of the polarizing plate using a pencil for pencil scratch value test (manufactured by Mitsubishi Pencil Co., Ltd.). The load was changed to 150 g, 300 g, and 500 g. The evaluation was performed with n=10. The above sample after the load was applied was observed on the backlight device. The reverse circular polarizer (NZD-UFQAMEGQ1773VDUHC) of the circular polarizer used in the test was clamped between the backlight device and the sample and the circular polarization was removed. Since the state is orthogonal, the bright spots of light leakage are set as scratches for evaluation. The number of scratches is set as 0 for 0 to 3, and 4 or more for ×. Under a load of 150 g, the number of scratches on all polarizers with phase difference layers is 0 to 3. Under a load of 300 g, the number of scratches on polarizers 1 to 7, 14, and 16 to 17 with phase difference layers is 0 to 3, and the number of scratches on polarizers 8 to 13, 15, and 18 to 19 with phase difference layers is 4 or more. Furthermore, under a load of 500 g, the number of scratches on the polarizing plate 16 with only a phase difference layer was 0 to 3, and the number of scratches on the polarizing plates 1 to 15 and 17 to 19 with a phase difference layer was 4 or more. <Curl test> In the polarizing plate with a phase difference layer, the surface protective film and the protective layer of the polarizing plate were peeled off. The size of the polarizing plate used in this test was set to 120 mm × 60 mm. The polarizing plate was placed on a horizontal surface, and the height of the center from the horizontal surface (curl value) was measured using a steel ruler. If the curl value is within 10 mm, it is set to 0, and if it exceeds 10 mm, it is set to ×. Curling was observed in polarizing plate 16 with phase difference layer, but no curling was observed in polarizing plates 1 to 15 and 17 to 19 with phase difference layer. <Heat shock resistance> The polarizing plate with phase difference layer was cut into a size of 120 mm × 60 mm and bonded to glass via the adhesive layer B on the outermost surface to prepare a sample. The sample was placed in a heat shock tester for a heat shock test, that is, 100 cycles of keeping at -40°C for 30 minutes and then keeping at 85°C for 30 minutes were repeated, and then the presence of cracks in the phase difference layer was confirmed using an optical microscope. In polarizing plates 15 and 19 with phase difference layers, cracks were observed in the phase difference layers, but in polarizing plates 1 to 14 and 16 to 18 with phase difference layers, cracks in the phase difference were not observed. <Heat resistance> The polarizing plates with phase difference layers were cut into a size of 120 mm × 60 mm and bonded to glass via the adhesive layer B on the outermost surface to prepare a sample. The sample was placed in an oven at 85°C for 500 hours, and then placed on a reflective plate to visually check for unevenness. In polarizing plate 16 with phase difference layers, unevenness in which the peripheral color turned red was clearly observed, but in polarizing plates 1 to 15 and 17 to 19 with phase difference layers, unevenness was not observed.
[表2]
由表2明確，實施例之附相位差層之偏光板不易產生劃痕，捲曲得到抑制，相位差層之龜裂得到抑制，且不均之產生得到抑制。進而可知，附相位差層之偏光板之第1黏著劑層之厚度越薄越不易產生劃痕，表面保護膜之厚度越厚越不易產生劃痕。 [產業上之可利用性] Table 2 clearly shows that the polarizing plate with phase difference layer of the embodiment is not easy to produce scratches, curling is suppressed, cracking of the phase difference layer is suppressed, and unevenness is suppressed. It can be further known that the thinner the thickness of the first adhesive layer of the polarizing plate with phase difference layer is, the less likely it is to produce scratches, and the thicker the thickness of the surface protective film is, the less likely it is to produce scratches. [Industrial Applicability]
本發明之光學積層體適宜用於有機EL顯示裝置等圖像顯示裝置。The optical multilayer body of the present invention is suitable for use in image display devices such as organic EL display devices.
10:偏光板 20:第1相位差層 30:黏著劑層 40:第2相位差層 50:黏著劑層 100:附相位差層之偏光板 10: Polarizing plate 20: First phase difference layer 30: Adhesive layer 40: Second phase difference layer 50: Adhesive layer 100: Polarizing plate with phase difference layer
圖1係本發明之一實施形態之附相位差層之偏光板之概略剖視圖。FIG. 1 is a schematic cross-sectional view of a polarizing plate with a phase difference layer according to an embodiment of the present invention.
10:偏光板 10: Polarizing plate
20:第1相位差層 20: 1st phase difference layer
30:黏著劑層 30: Adhesive layer
40:第2相位差層 40: Second phase difference layer
50:黏著劑層 50: Adhesive layer
100:附相位差層之偏光板 100: Polarizing plate with phase difference layer
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| Application Number | Priority Date | Filing Date | Title |
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| JP2018-081256 | 2018-04-20 | ||
| JP2019-061379 | 2019-03-27 |
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| TW202414002A true TW202414002A (en) | 2024-04-01 |
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