TWI781855B - Optical film having improved optical properties and display apparatus comprising the same - Google Patents

Optical film having improved optical properties and display apparatus comprising the same Download PDF

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TWI781855B
TWI781855B TW110147176A TW110147176A TWI781855B TW I781855 B TWI781855 B TW I781855B TW 110147176 A TW110147176 A TW 110147176A TW 110147176 A TW110147176 A TW 110147176A TW I781855 B TWI781855 B TW I781855B
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optical film
chlorine
present disclosure
compound
optical
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TW202239831A (en
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崔民熙
朴曉準
鄭鶴基
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南韓商可隆股份有限公司
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1039—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors comprising halogen-containing substituents
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/14—Polyamide-imides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/04—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of organic materials, e.g. plastics
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
    • C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors

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Abstract

Disclosed are an optical film having a color difference (△E) of 3.5 or less before and after heat treatment at 150℃ for 30 minutes and exposure to visible light for 150 hours and a display device comprising the same. Disclosed is also a display device including the optical film. Here, the color difference (△E) is calculated using the following Equation 1 based on values measured in the CIE 1976 L*a*b* color space.
[Equation 1] △E=[(△L*)2+(△a*)2+(△b*)2]1/2 wherein △L*, △a* and △b* are the differences in L*, a* and b*, respectively, of the optical film according to the CIE 1976 L*a*b* color space before and after the optical film is heat-treated at a temperature of 150℃ for 30 minutes and exposed to visible light for 150 hours.

Description

具有改良的光學特性之光學膜以及包括其之顯 示元件 Optical film with improved optical properties and display including same display element

本揭露是有關於一種具有優異的光學特性的光學膜以及一種包括所述光學膜的顯示元件，更具體而言，是有關於一種具有小色差(△E)的光學膜以及一種包括其的顯示元件。 The present disclosure relates to an optical film having excellent optical characteristics and a display element including the same, and more particularly, to an optical film having small chromatic aberration (ΔE) and a display including the same element.

最近，出於減小顯示元件的厚度及重量並增加顯示元件的可撓性的目標，已經考慮使用光學膜代替玻璃作為顯示元件的覆蓋窗(cover window)。為使光學膜可用作顯示元件的覆蓋窗，光學膜需要具有優異的光學特性及機械特性。具體而言，需要開發即使在外部環境中長時間段使用之後仍能夠維持光學特性的光學膜。 Recently, with the aim of reducing the thickness and weight of the display element and increasing the flexibility of the display element, it has been considered to use an optical film instead of glass as a cover window of the display element. In order for the optical film to be useful as a cover window of a display element, the optical film needs to have excellent optical and mechanical properties. In particular, there is a need to develop an optical film capable of maintaining optical characteristics even after being used in an external environment for a long period of time.

因此，鑒於以上問題作出了本揭露，且本揭露的一個目的是提供一種具有優異的光學特性的光學膜。 Therefore, the present disclosure has been made in view of the above problems, and an object of the present disclosure is to provide an optical film having excellent optical characteristics.

本揭露的另一目的是提供一種光學膜，即使當在熱處理之後長時間暴露於可見光時，所述光學膜在熱處理及曝光處理之前及之後亦具有小色差(△E)。 Another object of the present disclosure is to provide an optical film having a small color difference (ΔE) before and after heat treatment and exposure treatment even when exposed to visible light for a long time after heat treatment.

本揭露的另一目的是提供一種光學膜，藉由控制所述膜中的氯(Cl)濃度，所述光學膜即使在長時間使用之後亦能夠維持光學特性。 Another object of the present disclosure is to provide an optical film capable of maintaining optical characteristics even after being used for a long time by controlling chlorine (Cl) concentration in the film.

本揭露的另一目的是提供一種用於製造具有優異的光學特性及光學穩定性的光學膜的方法，所述方法是藉由在製造所述光學膜的製程期間控制氯(Cl)受體及觸媒的含量及添加方法來達成。 Another object of the present disclosure is to provide a method for manufacturing an optical film having excellent optical characteristics and optical stability by controlling chlorine (Cl) acceptors and Catalyst content and adding method to achieve.

本揭露的另一目的是提供一種包括如上所述的光學膜的顯示元件。 Another object of the present disclosure is to provide a display element including the above optical film.

根據本揭露，以上及其他目的可藉由提供一種光學膜來達成，所述光學膜在150℃下進行熱處理達30分鐘以及暴露於可見光達150小時之前及之後具有3.5或小於3.5的色差(△E)，其中色差(△E)是基於在國際照明委員會(Commission Internationale de l′Eclairage，CIE)1976 L*a*b*顏色空間中量測的值而使用以下方程式1來計算：[方程式1] △E=[(△L*)2+(△a*)2+(△b*)2]1/2 According to the present disclosure, the above and other objects can be achieved by providing an optical film having a color difference (Δ) of 3.5 or less before and after heat treatment at 150° C. for 30 minutes and exposure to visible light for 150 hours. E), where the color difference (ΔE) is calculated based on values measured in the International Commission on Illumination (Commission Internationale de l'Eclairage, CIE) 1976 L*a*b* color space using Equation 1 below: [Equation 1 ] △E=[(△L*) 2 +(△a*) 2 +(△b*) 2 ] 1/2

其中△L*、△a*及△b*分別是根據CIE 1976 L*a*b*顏色空間的所述光學膜的L*、a*及b*在所述光學膜經歷在150℃的溫度下進行熱處理達30分鐘以及暴露於可見光達150小時之前及之後的差，其中L*a*b*是使用CIE標準光源D65而量測，且所述暴露於可見光是藉由在平均溫度為25℃及平均相對濕度為30%的環境條件下使用氙燈以0.8瓦/平方公尺的光劑量、420奈米的中心波長向所述光學膜照射可見光達150小時來執行。 where ΔL*, Δa*, and Δb* are L*, a*, and b* of the optical film according to the CIE 1976 L*a*b* color space, respectively, when the optical film experiences a temperature of 150° C. The difference before and after heat treatment for 30 minutes and exposure to visible light for 150 hours, where L*a*b* is measured using CIE standard illuminant D65, and the exposure to visible light is measured by °C and an average relative humidity of 30% using a xenon lamp to irradiate visible light to the optical film for 150 hours with a light dose of 0.8 W/m2 and a central wavelength of 420 nm.

所述光學膜可具有3.2或小於3.2的色差(△E)。 The optical film may have a color difference (ΔE) of 3.2 or less.

按重量計，所述光學膜可包含120百萬分點(parts per million，ppm)(0.012重量%)或小於120ppm(0.012重量%)的氯(Cl)。 The optical film may include 120 parts per million (ppm) (0.012 wt %) or less than 120 ppm (0.012 wt %) of chlorine (Cl) by weight.

按重量計，所述光學膜可包含50ppm(0.005重量%)或小於50ppm(0.005重量%)的氯(Cl)。 The optical film may include 50 ppm (0.005 wt %) or less of chlorine (Cl) by weight.

基於50微米的厚度，所述光學膜可具有3或小於3的黃度指標(yellowness index，Y.I.)。 The optical film may have a yellowness index (Y.I.) of 3 or less based on a thickness of 50 micrometers.

基於50微米的厚度，所述光學膜可具有1.0%或小於1.0%的霧度(haze)。 The optical film may have a haze of 1.0% or less based on a thickness of 50 micrometers.

基於50微米的厚度，所述光學膜可具有88%或大於88%的光透射率(light transmittance)。 The optical film may have a light transmittance of 88% or more based on a thickness of 50 micrometers.

所述光學膜可包含醯亞胺重複單元及醯胺重複單元中的至少一者。 The optical film may include at least one of an imide repeating unit and an amide repeating unit.

按重量計，所述光學膜可包含30ppm(0.003重量%)或小於30ppm(0.003重量%)的環狀醚化合物。 The optical film may include 30 ppm (0.003% by weight) or less of the cyclic ether compound by weight.

根據本揭露的另一態樣，提供一種顯示元件，所述顯示元件包括顯示面板以及設置於所述顯示面板上的所述光學膜。 According to another aspect of the present disclosure, a display element is provided, and the display element includes a display panel and the optical film disposed on the display panel.

根據本揭露實施例的所述光學膜即使當長時間暴露於可見光時亦不會發生顏色變化，且由於其小的色差(△E)而維持優異的透明度。 The optical film according to an embodiment of the present disclosure does not undergo color change even when exposed to visible light for a long time, and maintains excellent transparency due to its small color difference (ΔE).

相較於曝光之前而言，根據本揭露實施例的所述光學膜即使在暴露於外部光之後亦具有低的氯(Cl)濃度及非常小的色差。因此，根據本揭露實施例的所述光學膜具有優異的光學穩定性。 The optical film according to an embodiment of the present disclosure has a low chlorine (Cl) concentration and very little color difference even after being exposed to external light, compared to before exposure. Therefore, the optical film according to an embodiment of the present disclosure has excellent optical stability.

根據本揭露的實施例，藉由可生產一種具有優異的光學特性及光學穩定性的光學膜，所述生產所述光學膜是藉由在製造所述光學膜的製程中控制氯(Cl)受體及醯亞胺化觸媒的含量及添加方法來達成。 According to the embodiments of the present disclosure, an optical film having excellent optical characteristics and optical stability can be produced by controlling the influence of chlorine (Cl) in the process of manufacturing the optical film. The content and addition method of the body and imidization catalyst can be achieved.

根據本揭露實施例的包括光學膜的所述顯示元件具有優異的顯示品質，且即使在長時間使用之後亦能夠維持所述優異的顯示品質。 The display element including the optical film according to an embodiment of the present disclosure has excellent display quality and can maintain the excellent display quality even after being used for a long time.

100:光學膜 100: Optical film

200:顯示元件 200: display components

501:顯示面板 501: display panel

510:基板 510: Substrate

520:半導體層 520: semiconductor layer

530:閘極電極 530: gate electrode

535:閘極絕緣層 535: gate insulation layer

541:源極電極 541: source electrode

542:汲極電極 542: Drain electrode

551:層間絕緣層 551: interlayer insulating layer

552:平坦化層 552: Planarization layer

570:有機發光元件 570: Organic Light Emitting Components

571:第一電極 571: first electrode

572:有機發光層 572: Organic light-emitting layer

573:第二電極 573: second electrode

580:堤層 580: embankment layer

590:薄膜包封層 590: film encapsulation layer

P:部分 P: part

TFT:薄膜電晶體 TFT: thin film transistor

圖1是示出根據本揭露實施例的顯示元件的剖視圖。 FIG. 1 is a cross-sectional view illustrating a display element according to an embodiment of the present disclosure.

圖2是示出圖1所示部分「P」的放大剖視圖。 FIG. 2 is an enlarged sectional view showing a portion "P" shown in FIG. 1 .

在下文中，將參照附圖詳細地闡述本揭露的實施例。然而，例示性地提供以下實施例僅是為清楚地理解本揭露，且並不限制本揭露的範圍。 Hereinafter, embodiments of the present disclosure will be explained in detail with reference to the accompanying drawings. However, the following examples are provided merely for a clear understanding of the present disclosure, and do not limit the scope of the present disclosure.

在圖式中揭露的用於闡述本揭露的實施例的形狀、大小、比率、角度及數目僅為實例，且本揭露不限於所示細節。在本說明書通篇中，相同的參考編號指代相同的部件。在以下說明中，當確定對相關眾所習知功能或配置的詳細說明不必要地使本揭露的要點模糊不清時，將省略所述詳細說明。 The shapes, sizes, ratios, angles and numbers disclosed in the drawings to illustrate the embodiments of the disclosure are examples only, and the disclosure is not limited to the details shown. Throughout this specification, the same reference numerals refer to the same parts. In the following description, when it is determined that a detailed description of a related well-known function or configuration unnecessarily obscures the gist of the present disclosure, the detailed description will be omitted.

在本說明書中使用例如「包括」、「具有」或「包含」等用語的情形中，除非使用「僅」，否則亦可存在另一部分。除非另有相反表述，否則單數形式的用語可包含複數含義。此外，在解釋部件時，即使不存在對其的明確說明，所述部件亦應被解釋為包括誤差範圍。 Where terms such as "comprises", "has" or "comprises" are used in this specification, another part may also be present unless "only" is used. Terms in the singular may include plural meanings unless otherwise stated to the contrary. Furthermore, when explaining a component, the component should be construed as including a range of error even if there is no explicit description thereof.

在闡述位置關係時，舉例而言，當位置關係被闡述為「在...上」、「上方」、「下方」或「靠近」時，除非使用「恰好(just)」或「直接」，否則可包括其間並無接觸的情形。 When describing a positional relationship, for example, when a positional relationship is stated as "on," "above," "below," or "near," unless "just" or "directly" is used, Otherwise, situations where there is no contact can be included.

例如「下方」、「之下」、「下部」、「上方」及「上部」等空間相對用語在本文中可用於闡述如圖中所示的元件或部件與另一元件或部件之間的關係。應理解，除圖中繪示的定向之外，空間 相對用語亦旨在囊括在元件的使用或操作期間所述元件的不同定向。舉例而言，若所述圖中的一個圖中的元件上下顛倒，則被闡述為在其他部件「下方」或在其他部件「之下」的部件此時將被定位成位於其他部件「上方」。因此，示例性用語「下方」或「之下」可囊括「下方」及「上方」兩種含義。同樣地，示例性用語「上方」或「上部」可囊括「上方」及「下方」兩種含義。 Spatially relative terms such as "below," "under," "lower," "above" and "upper" may be used herein to describe a relationship between an element or component as shown in the figures and another element or component. . It should be understood that in addition to the orientations depicted in the figures, spatial Relative terms are also intended to encompass different orientations of the elements during use or operation of the elements. For example, if an element in one of the figures is turned upside down, elements described as being "below" or "beneath" the other elements would then be oriented "above" the other elements . Thus, the exemplary terms "below" or "under" can encompass both "below" and "above". Likewise, the exemplary terms "above" or "upper" can encompass both "above" and "below".

在闡述時間關係時，舉例而言，當使用「之後」、「隨後」、「接下來」或「之前」闡述時間次序時，除非使用「恰好」或「直接」，否則可包括非連續關係的情形。 When describing temporal relationships, for example, when using "after", "later", "next" or "before" to describe temporal order, non-sequential relationships may be included unless "exactly" or "directly" are used situation.

應理解，儘管在本文中可能使用用語「第一(first)」、「第二(second)」等來闡述各種部件，然而該些部件不受該些用語限制。該些用語僅用於區分一個部件與另一部件。因此，在本揭露的技術思想內，第一部件可被稱為第二部件。 It should be understood that although the terms "first", "second", etc. may be used herein to describe various components, these components are not limited by these terms. These terms are only used to distinguish one component from another. Therefore, the first component may be referred to as the second component within the technical idea of the present disclosure.

應理解，用語「至少一者」包括與一或多個項相關的所有組合。舉例而言，「第一部件、第二部件及第三部件中的至少一者」可包括選自第一部件、第二部件及第三部件中的二或更多個部件、以及第一部件、第二部件及第三部件中的每一者的所有組合。 It should be understood that the term "at least one" includes all combinations in which one or more items are associated. For example, "at least one of the first component, the second component, and the third component" may include two or more components selected from the first component, the second component, and the third component, and the first component , all combinations of each of the second component and the third component.

本揭露的各種實施例的特徵可局部地或完全地彼此耦合或組合，並且可以不同方式彼此相互操作及在技術上驅動。 Features of various embodiments of the present disclosure may be partially or completely coupled or combined with each other, and may interoperate with each other and be technically driven in different ways.

本揭露的實施例提供一種光學膜。根據本揭露實施例的所述光學膜包含聚合物樹脂。 Embodiments of the present disclosure provide an optical film. The optical film according to an embodiment of the present disclosure includes a polymer resin.

根據本揭露實施例的所述光學膜可包含醯亞胺重複單 元及醯胺重複單元中的至少一者。 The optical film according to an embodiment of the present disclosure may include an imide repeating unit At least one of element and amide repeating unit.

根據本揭露實施例的所述光學膜可包含由二胺化合物及二酐化合物形成的醯亞胺重複單元。 The optical film according to an embodiment of the present disclosure may include an imide repeating unit formed of a diamine compound and a dianhydride compound.

根據本揭露實施例的所述光學膜可包含由二胺化合物及二羰基化合物形成的醯胺重複單元。 The optical film according to an embodiment of the present disclosure may include an amide repeating unit formed of a diamine compound and a dicarbonyl compound.

根據本揭露實施例的所述光學膜可包含由二胺化合物、二酐化合物及二羰基化合物形成的醯胺重複單元與醯亞胺重複單元二者。 The optical film according to an embodiment of the present disclosure may include both an amide repeating unit and an imide repeating unit formed of a diamine compound, a dianhydride compound, and a dicarbonyl compound.

據以，根據本揭露實施例的所述光學膜可包含聚醯亞胺樹脂、聚醯胺樹脂及聚醯胺-醯亞胺樹脂中的至少一者。根據本揭露實施例的所述光學膜可包含聚醯亞胺系聚合物、聚醯胺系聚合物及聚醯胺-醯亞胺系聚合物中的至少一者。 Accordingly, the optical film according to an embodiment of the present disclosure may include at least one of polyimide resin, polyamide resin and polyamide-imide resin. The optical film according to an embodiment of the present disclosure may include at least one of a polyimide-based polymer, a polyamide-based polymer, and a polyamide-imide-based polymer.

根據本揭露的實施例，所述光學膜可為聚醯亞胺系膜、聚醯胺系膜及聚醯胺-醯亞胺系膜中的任一者，但本揭露的實施例不限於此。根據本揭露的實施例，具有光透射率的任何膜均可用作所述光學膜。 According to the embodiments of the present disclosure, the optical film may be any one of polyimide-based films, polyamide-based films and polyamide-imide-based films, but the embodiments of the present disclosure are not limited thereto . According to an embodiment of the present disclosure, any film having light transmittance may be used as the optical film.

根據本揭露的實施例，二胺系化合物可由以下式1表示：[式1] H2N-A1-NH2 According to an embodiment of the present disclosure, the diamine compound can be represented by the following formula 1: [Formula 1] H 2 NA 1 -NH 2

其中A1表示二價基團。舉例而言，A1可包括具有4至40個碳原子的二價有機基團。式1中的有機基團中的氫原子可經鹵素元素、烴基或經鹵素元素取代的烴基取代。此處，烴基或經鹵 素元素取代的烴基可具有1至8個碳原子。舉例而言，A1中的氫可經-F、-CH3、-CF3或類似物取代。 wherein A 1 represents a divalent group. For example, A 1 may include a divalent organic group having 4 to 40 carbon atoms. The hydrogen atom in the organic group in Formula 1 may be substituted by a halogen element, a hydrocarbon group, or a hydrocarbon group substituted by a halogen element. Here, the hydrocarbon group or the hydrocarbon group substituted with a halogen element may have 1 to 8 carbon atoms. For example, the hydrogen in A 1 can be substituted with -F, -CH 3 , -CF 3 or the like.

使用其中氫原子經由氟取代的烴基取代的二胺化合物生產的光學膜可被賦予優異的光透射率及優異的可加工性(workability)。 An optical film produced using a diamine compound in which hydrogen atoms are substituted through a fluorine-substituted hydrocarbon group can be imparted with excellent light transmittance and excellent workability.

在根據本揭露實施例的所述光學膜的製造中所使用的二胺系化合物可例如包括脂族二胺、芳族二胺或其混合物。 The diamine-based compound used in the manufacture of the optical film according to the embodiments of the present disclosure may, for example, include aliphatic diamine, aromatic diamine or a mixture thereof.

在本揭露的實施例中，用語「芳族二胺」是指其中胺基直接鍵結至芳環的二胺，且可包括脂族基團或其他取代基作為其結構的一部分。芳環可為單環、包括藉由雜原子而直接與其連結的單環的稠環、或縮合環。芳環的實例可包括但不限於苯環、聯苯環、萘環、蒽環及芴環。 In embodiments of the present disclosure, the term "aromatic diamine" refers to a diamine in which an amine group is directly bonded to an aromatic ring, and may include aliphatic groups or other substituents as part of its structure. The aryl ring can be a monocyclic ring, a fused ring including a monocyclic ring directly attached thereto through a heteroatom, or a condensed ring. Examples of aromatic rings may include, but are not limited to, benzene rings, biphenyl rings, naphthalene rings, anthracene rings, and fluorene rings.

在本揭露的實施例中，用語「脂族二胺」是指其中胺基直接鍵結至脂族基團的二胺，且可包括芳環或其他取代基作為其結構的一部分。脂族二胺可包括環狀脂族二胺及非環狀脂族二胺。 In embodiments of the present disclosure, the term "aliphatic diamine" refers to a diamine in which an amine group is directly bonded to an aliphatic group, and may include aromatic rings or other substituents as part of its structure. Aliphatic diamines may include cyclic aliphatic diamines and acyclic aliphatic diamines.

式1中的A1可例如包括由以下式中的任一者表示的結構。 A 1 in Formula 1 may, for example, include a structure represented by any of the following formulae.

Figure 110147176-A0305-02-0010-1
Figure 110147176-A0305-02-0010-1

在上式中，*表示鍵結位置。在上式中，X可獨立地是單鍵、O、S、SO2、CO、CH2、C(CH3)2及C(CF3)2中的任一者。儘管 X在每一環上的鍵結位置並無特別限制，然而X的鍵結位置可為例如每一環上的間位或對位。 In the above formula, * represents a bonding position. In the above formula, X may independently be any one of a single bond, O, S, SO 2 , CO, CH 2 , C(CH 3 ) 2 and C(CF 3 ) 2 . Although the bonding position of X on each ring is not particularly limited, the bonding position of X may be, for example, a meta-position or a para-position on each ring.

根據本揭露的實施例，二酐系化合物可由以下式2表示：

Figure 110147176-A0305-02-0011-3
According to an embodiment of the present disclosure, the dianhydride compound can be represented by the following formula 2:
Figure 110147176-A0305-02-0011-3

其中A2表示四價基團。舉例而言，A2可包括具有4至40個碳原子的四價有機基團。式2中的有機基團中的氫原子可經鹵素元素、烴基或經鹵素元素取代的烴基取代。此處，烴基或經鹵素元素取代的烴基可具有1至8個碳原子。 Wherein A 2 represents a tetravalent group. For example, A 2 may include a tetravalent organic group having 4 to 40 carbon atoms. The hydrogen atom in the organic group in Formula 2 may be substituted by a halogen element, a hydrocarbon group, or a hydrocarbon group substituted by a halogen element. Here, the hydrocarbon group or the hydrocarbon group substituted with a halogen element may have 1 to 8 carbon atoms.

式2中的A2可例如包括由以下式中的任一者表示的結構。 A 2 in Formula 2 may, for example, include a structure represented by any of the following formulae.

Figure 110147176-A0305-02-0011-4
Figure 110147176-A0305-02-0011-4

在上式中，*表示鍵結位置。在上式中，X可獨立地為單鍵、O、S、SO2、CO、(CH2)n、(C(CH3)2)n及(C(CF3)2)n中的任一者，且n可為1至5的整數。儘管X在每一環上的鍵結位置並無特別 限制，然而X的鍵結位置可為例如每一環上的間位或對位。 In the above formula, * represents a bonding position. In the above formula, X can independently be any of single bond, O, S, SO 2 , CO, (CH 2 ) n , (C(CH 3 ) 2 ) n and (C(CF 3 ) 2 ) n One, and n can be an integer from 1 to 5. Although the bonding position of X on each ring is not particularly limited, the bonding position of X may be, for example, a meta-position or a para-position on each ring.

在根據本揭露實施例的所述光學膜的製造中所使用的單體可包括例如多種二酐化合物。 Monomers used in the manufacture of the optical film according to embodiments of the present disclosure may include, for example, various dianhydride compounds.

使用其中氫原子經由氟取代的烴基取代的二酐化合物產生的光學膜可被賦予優異的光透射率及優異的可加工性。 An optical film produced using a dianhydride compound in which hydrogen atoms are substituted through a fluorine-substituted hydrocarbon group can be imparted with excellent light transmittance and excellent processability.

根據本揭露的實施例，二羰基化合物可由以下式3表示：

Figure 110147176-A0305-02-0012-5
According to an embodiment of the present disclosure, the dicarbonyl compound may be represented by the following formula 3:
Figure 110147176-A0305-02-0012-5

其中A3表示二價基團。舉例而言，A3可包括具有4至40個碳原子的二價有機基團。另外，A3可表示碳原子、氮原子或氧原子。式3中的有機基團中的氫原子可經鹵素元素、烴基或經氟取代的烴基取代。此處，烴基或經氟取代的烴基可具有1至8個碳原子。 Wherein A 3 represents a divalent group. For example, A 3 may include a divalent organic group having 4 to 40 carbon atoms. In addition, A3 may represent a carbon atom, a nitrogen atom or an oxygen atom. The hydrogen atom in the organic group in Formula 3 may be substituted with a halogen element, a hydrocarbon group, or a fluorine-substituted hydrocarbon group. Here, the hydrocarbon group or the fluorine-substituted hydrocarbon group may have 1 to 8 carbon atoms.

在根據本揭露實施例的所述光學膜的製造中所使用的二酐化合物及二羰基化合物的含量並無特別限制。舉例而言，由式2表示的二酐化合物對由式3表示的二羰基化合物的莫耳比(二酐化合物：二羰基化合物)可在(20至60)：(80至40)的範圍內進行調節。 The contents of the dianhydride compound and the dicarbonyl compound used in the manufacture of the optical film according to the embodiments of the present disclosure are not particularly limited. For example, the molar ratio of the dianhydride compound represented by Formula 2 to the dicarbonyl compound represented by Formula 3 (dianhydride compound: dicarbonyl compound) may be in the range of (20 to 60): (80 to 40) Make adjustments.

根據本揭露實施例的所述光學膜可包含由以下式4表示的醯亞胺重複單元：[式4]

Figure 110147176-A0305-02-0013-6
The optical film according to an embodiment of the present disclosure may include an imide repeating unit represented by the following Formula 4: [Formula 4]
Figure 110147176-A0305-02-0013-6

其中A1及A2如上所述。 Wherein A1 and A2 are as above.

根據本揭露實施例的所述光學膜可包含由以下式5表示的醯胺重複單元。 The optical film according to an embodiment of the present disclosure may include an amide repeating unit represented by Formula 5 below.

Figure 110147176-A0305-02-0013-7
Figure 110147176-A0305-02-0013-7

其中A1及A3如上所述。 Wherein A1 and A3 are as above.

根據本揭露的實施例，具有醯亞胺重複單元的所述光學膜可為例如聚醯亞胺系膜。具有醯胺重複單元的所述光學膜可為例如聚醯胺系膜。具有醯亞胺重複單元及醯胺重複單元的所述光學膜可為例如聚醯胺-醯亞胺系膜。 According to an embodiment of the present disclosure, the optical film having imide repeating units may be, for example, a polyimide-based film. The optical film having an amide repeating unit may be, for example, a polyamide-based film. The optical film having amide repeating units and amide repeating units may be, for example, a polyamide-imide based film.

根據本揭露的實施例，所述光學膜可為光透射性的及可撓性的。舉例而言，根據本揭露實施例的所述光學膜可為可彎曲的、可折疊的或可捲曲的。 According to an embodiment of the present disclosure, the optical film may be light transmissive and flexible. For example, the optical film according to embodiments of the present disclosure may be bendable, foldable or rollable.

根據本揭露的實施例，所述光學膜即使在長時間暴露於可見光之後亦不會改變顏色。 According to an embodiment of the present disclosure, the optical film does not change color even after prolonged exposure to visible light.

根據本揭露的實施例，即使當所述光學膜在150℃下進行熱處理達30分鐘且然後暴露於可見光達150小時時，所述光學 膜在熱處理及暴露於可見光之前及之後的色差(△E)為3.5或小於3.5。根據本揭露的實施例，向所述光學膜照射可見光亦被稱為「曝光」。 According to an embodiment of the present disclosure, even when the optical film is heat-treated at 150° C. for 30 minutes and then exposed to visible light for 150 hours, the optical film The film had a color difference (ΔE) of 3.5 or less before and after heat treatment and exposure to visible light. According to an embodiment of the present disclosure, irradiating visible light to the optical film is also referred to as “exposure”.

根據本揭露的實施例，色差被表達為自兩種顏色獲得的顏色值之間的差。 According to an embodiment of the present disclosure, a color difference is expressed as a difference between color values obtained from two colors.

根據本揭露實施例的所述光學膜的色差被表達為「△E」，且是基於在CIE 1976 L*a*b*顏色空間中量測的值而使用以下方程式1來計算：[方程式1] △E=[(△L*)2+(△a*)2+(△b*)2]1/2 The chromatic aberration of the optical film according to an embodiment of the present disclosure is expressed as "ΔE" and is calculated using the following Equation 1 based on values measured in the CIE 1976 L*a*b* color space: [Equation 1 ] △E=[(△L*) 2 +(△a*) 2 +(△b*) 2 ] 1/2

其中△L*、△a*及△b*分別是根據CIE 1976 L*a*b*顏色空間的所述光學膜的L*、a*及b*在所述光學膜在150℃的溫度下進行熱處理達30分鐘以及暴露於可見光達150小時之前及之後的差。 where ΔL*, Δa* and Δb* are L*, a* and b* of the optical film according to the CIE 1976 L*a*b* color space, respectively, at the temperature of the optical film at 150°C The difference before and after heat treatment for 30 minutes and exposure to visible light for 150 hours.

L*a*b*是使用CIE標準光源D65而量測。 L*a*b* is measured using CIE standard illuminant D65.

具體而言，△L*、△a*及△b*可分別使用以下方程式2、方程式3及方程式4來計算：[方程式2] △L*=L*2-L*1 Specifically, △L*, △a*, and △b* can be calculated using the following Equation 2, Equation 3, and Equation 4, respectively: [Equation 2] △L*=L*2-L*1

其中L*2表示在對所述光學膜進行熱處理及將所述光學膜曝光之後的L*，且L*1表示在對所述光學膜進行熱處理及將所述光學膜曝光之前的L*： [方程式3] △a*=a*2-a*1 Wherein L*2 represents L* after heat-treating and exposing the optical film to the optical film, and L*1 represents L* before heat-treating the optical film and exposing the optical film: [Equation 3] △a*=a*2-a*1

其中a*2表示在對所述光學膜進行熱處理及將所述光學膜曝光之後的a*，且a*1表示在對所述光學膜進行熱處理及將所述光學膜曝光之前的a*：[方程式4] △b*=b*2-b*1 Where a*2 represents a* after heat-treating the optical film and exposing the optical film, and a*1 represents a* before heat-treating the optical film and exposing the optical film: [Equation 4] △b*=b*2-b*1

其中b*2表示在對所述光學膜進行熱處理及將所述光學膜曝光之後的b*，且b*1表示在對所述光學膜進行熱處理及將所述光學膜曝光之前的b*。 Wherein b*2 represents b* after heat-treating the optical film and exposing the optical film, and b*1 represents b* before heat-treating the optical film and exposing the optical film.

所述熱處理是藉由在150℃下利用熱對所述光學膜進行處理達30分鐘來執行。舉例而言，所述熱處理可藉由將所述光學膜放置於150℃的烘箱中達30分鐘來執行。 The heat treatment was performed by treating the optical film with heat at 150° C. for 30 minutes. For example, the heat treatment can be performed by placing the optical film in an oven at 150° C. for 30 minutes.

所述暴露於可見光是藉由在平均溫度為25℃及平均相對濕度為30%的環境條件下使用氙燈以0.8瓦/平方公尺的光劑量、420奈米的中心波長向所述光學膜照射可見光達150小時來執行。 The exposure to visible light is performed by using a xenon lamp to irradiate the optical film with a light dose of 0.8 watts/square meter and a central wavelength of 420 nm under the environmental conditions of an average temperature of 25° C. and an average relative humidity of 30%. Visible light up to 150 hours to perform.

當所述光學膜在熱處理及暴露於可見光之前及之後的色差(△E)為3.5或小於3.5時，即使所述光學膜在外部環境中長時間使用，亦存在很少或不存在使用者所可察覺的色差。作為結果，即使在苛刻的條件下，所述光學膜的光學特性亦會長時間得到維持，因此所述光學膜可表現出優異的光學穩定性。 When the color difference (ΔE) of the optical film before and after heat treatment and exposure to visible light is 3.5 or less, there is little or no user concern even if the optical film is used in an external environment for a long time. Perceptible color difference. As a result, even under severe conditions, the optical characteristics of the optical film are maintained for a long time, and thus the optical film may exhibit excellent optical stability.

根據本揭露實施例的所述光學膜可在熱處理及曝光之 前及之後具有3.5或小於3.5的色差(△E)、3.2或小於3.2的色差(△E)或者3.0或小於3.0的色差(△E)。 The optical film according to an embodiment of the present disclosure can be processed after heat treatment and exposure The front and back have a color difference (ΔE) of 3.5 or less, a color difference (ΔE) of 3.2 or less, or a color difference (ΔE) of 3.0 or less.

根據本揭露的實施例，在使所述光學膜中所產生的色差(△E)最小化的方法中，舉例而言，可使所述光學膜中的氯(Cl)的含量最小化。 According to an embodiment of the present disclosure, in the method of minimizing chromatic aberration (ΔE) generated in the optical film, for example, chlorine (Cl) content in the optical film may be minimized.

根據本揭露的實施例，可使所述光學膜中的氯(Cl)的含量最小化。當氯(Cl)的含量被最小化時，可抑制所述光學膜中出現色差(△E)。 According to embodiments of the present disclosure, the content of chlorine (Cl) in the optical film can be minimized. When the content of chlorine (Cl) is minimized, occurrence of chromatic aberration (ΔE) in the optical film can be suppressed.

本發明者已發現，當氯(Cl)原子保留於所述光學膜中時，在所述光學膜中出現色差(△E)的可能性增加。 The present inventors have found that when chlorine (Cl) atoms remain in the optical film, the possibility of chromatic aberration (ΔE) occurring in the optical film increases.

具體而言，當在製造所述光學膜的製程中，在聚合物(例如聚醯胺-醯亞胺聚合物)的聚合期間產生的鹽酸(HCl)未被充分移除且因此存在於用於製造所述光學膜的反應溶液(例如，聚醯胺-醯胺酸溶液)中時，所述反應溶液的酸度可能增加，反應性可能劣化，且聚合物可能降解。另外，在製造所述光學膜的製程中的化學醯亞胺化或熱醯亞胺化期間，鹽酸(HCl)與水(H2O)進行反應，從而引起例如產生水合氫離子(H3O+)及氯離子(Cl-)等副反應。作為結果，所述膜的光學特性可能劣化。 Specifically, when in the process of manufacturing the optical film, hydrochloric acid (HCl) generated during polymerization of polymers such as polyamide-imide polymers is not sufficiently removed and thus exists in the When in a reaction solution (for example, a polyamide-amic acid solution) for manufacturing the optical film, the acidity of the reaction solution may increase, reactivity may deteriorate, and polymers may degrade. In addition, during chemical imidization or thermal imidization in the process of manufacturing the optical film, hydrochloric acid (HCl) reacts with water (H 2 O), causing, for example, generation of hydronium ions (H 3 O + ) and chloride ion (Cl - ) and other side reactions. As a result, the optical characteristics of the film may deteriorate.

另外，當熱及光被施加至包含氯(Cl)原子的光學膜時，構成所述光學膜的聚合物的降解或劣化可能由於氯(Cl)原子而加速，或者聚合物樹脂的化學結構可能改變。因此，當構成所述光學膜的聚合物樹脂的化學結構由於因熱處理及曝光引起的分解或降 解而改變時，在所述光學膜中可能會出現色差△E。 In addition, when heat and light are applied to an optical film containing chlorine (Cl) atoms, degradation or deterioration of polymers constituting the optical film may be accelerated due to chlorine (Cl) atoms, or the chemical structure of the polymer resin may Change. Therefore, when the chemical structure of the polymer resin constituting the optical film is decomposed or degraded due to heat treatment and exposure, When the solution is changed, a chromatic aberration ΔE may occur in the optical film.

以重量計，根據本揭露實施例的所述光學膜可包含120ppm或小於120ppm的氯(Cl)。根據本揭露的實施例，120ppm可對應於0.012重量%。以重量計，當所述光學膜包含120ppm或小於120ppm的氯(Cl)時，可使由氯(Cl)引起的所述光學膜的色差(△E)最小化或防止所述色差(△E)。根據本揭露的實施例，「氯(Cl)」旨在包括氯原子及氯離子(Cl-)。另外，根據本揭露的實施例，氯(Cl)可鍵結至其他原子以形成分子，且根據本揭露的實施例，氯(Cl)中包括存在於分子中的氯原子。氯的含量可表達為氯的濃度。 The optical film according to an embodiment of the present disclosure may include 120 ppm or less of chlorine (Cl) by weight. According to an embodiment of the present disclosure, 120 ppm may correspond to 0.012% by weight. When the optical film contains chlorine (Cl) at 120 ppm or less by weight, the chromatic aberration (ΔE) of the optical film caused by chlorine (Cl) can be minimized or prevented. ). According to an embodiment of the present disclosure, "chlorine (Cl)" is intended to include chlorine atoms and chloride ions (Cl − ). In addition, according to an embodiment of the present disclosure, chlorine (Cl) may be bonded to other atoms to form a molecule, and according to an embodiment of the present disclosure, chlorine (Cl) includes chlorine atoms present in the molecule. The content of chlorine can be expressed as the concentration of chlorine.

根據本揭露實施例的所述光學膜可包含量為1ppm至120ppm(0.0001重量%至0.012重量%)的氯(Cl)。另外，以重量計，根據本揭露實施例的所述光學膜可包含50ppm(0.005重量%)或小於50ppm(0.005重量%)、較佳為10ppm(0.001重量%)或小於10ppm(0.001重量%)的氯(Cl)。根據本揭露實施例的所述光學膜可包含2ppm至120ppm、2ppm至50ppm、1ppm至10ppm或2ppm至10ppm的氯。 The optical film according to an embodiment of the present disclosure may include chlorine (Cl) in an amount of 1 ppm to 120 ppm (0.0001 wt % to 0.012 wt %). In addition, on a weight basis, the optical film according to an embodiment of the present disclosure may contain 50 ppm (0.005 wt %) or less than 50 ppm (0.005 wt %), preferably 10 ppm (0.001 wt %) or less than 10 ppm (0.001 wt %) Chlorine (Cl). The optical film according to an embodiment of the present disclosure may include 2 ppm to 120 ppm, 2 ppm to 50 ppm, 1 ppm to 10 ppm, or 2 ppm to 10 ppm of chlorine.

如上所述，在製造所述光學膜的製程中可能產生鹽酸(HCl)。當在製造所述光學膜的製程中產生的鹽酸未被移除時，氯(Cl)可能保留於所得的光學膜中。因此，根據本揭露的實施例，為使保留於所述光學膜中的氯(Cl)的量最小化，使用用於移除在製造所述光學膜的製程中產生的鹽酸的氯(Cl)受體。 As described above, hydrochloric acid (HCl) may be generated during the process of manufacturing the optical film. When hydrochloric acid generated during the process of manufacturing the optical film is not removed, chlorine (Cl) may remain in the resulting optical film. Therefore, according to an embodiment of the present disclosure, in order to minimize the amount of chlorine (Cl) remaining in the optical film, chlorine (Cl) for removing hydrochloric acid generated in the process of manufacturing the optical film is used. receptor.

在製造所述光學膜的製程中，氯(Cl)受體藉由與鹽酸(HCl)進行反應而轉化為氯(Cl)化合物，且然後被移除。然而，氯(Cl)受體的一部分可能不與鹽酸反應，且可能不會在製造所述光學膜的製程中被移除。因此，根據本揭露實施例的所述光學膜可包含痕量的氯(Cl)受體。 During the process of manufacturing the optical film, chlorine (Cl) acceptors are converted into chlorine (Cl) compounds by reacting with hydrochloric acid (HCl), and then removed. However, a portion of the chlorine (Cl) acceptor may not react with hydrochloric acid and may not be removed during the process of making the optical film. Therefore, the optical film according to an embodiment of the present disclosure may contain a trace amount of chlorine (Cl) acceptors.

在本揭露的一個實施例中，氯(Cl)受體是能夠與鹽酸(HCl)或氯離子(Cl-)進行反應的物質。氯(Cl)受體可選自在製造所述光學膜的製程中在與鹽酸(HCl)或氯離子(Cl-)進行反應之後可在後續製程中移除的物質。 In one embodiment of the present disclosure, the chlorine (Cl) acceptor is a substance capable of reacting with hydrochloric acid (HCl) or chloride ions (Cl − ). Chlorine (Cl) acceptors may be selected from substances that can be removed in subsequent processes after reacting with hydrochloric acid (HCl) or chloride ions (Cl − ) in the process of manufacturing the optical film.

氯(Cl)受體可例如與鹽酸進行反應以形成鹽或鹵醇化合物，藉此用於移除在聚合期間產生的鹽酸。 Chlorine (Cl) acceptors can be reacted, for example, with hydrochloric acid to form salts or halohydrin compounds, thereby serving to remove hydrochloric acid generated during polymerization.

在本揭露的實施例中，環狀醚化合物可用作氯(Cl)受體。環狀醚化合物可例如包括環氧化合物、氧雜環丁烷化合物、四氫呋喃(tetrahydrofuran，THF)化合物及四氫吡喃化合物中的至少一者。 In embodiments of the present disclosure, cyclic ether compounds can be used as chlorine (Cl) acceptors. The cyclic ether compound may, for example, include at least one of an epoxy compound, an oxetane compound, a tetrahydrofuran (THF) compound, and a tetrahydropyran compound.

按重量計，根據本揭露實施例的所述光學膜可包含30ppm(0.003重量%)或小於30ppm(0.003重量%)的環狀醚化合物。按重量計，根據本揭露實施例的所述光學膜可包含0.1ppm至30ppm的環狀醚化合物。按重量計，根據本揭露實施例的所述光學膜可包含0.1ppm至12ppm的環狀醚化合物。 The optical film according to an embodiment of the present disclosure may include 30 ppm (0.003 wt %) or less of the cyclic ether compound by weight. The optical film according to an embodiment of the present disclosure may include 0.1 ppm to 30 ppm of the cyclic ether compound by weight. The optical film according to an embodiment of the present disclosure may include 0.1 ppm to 12 ppm of the cyclic ether compound by weight.

根據本揭露的實施例，由以下式6表示的環氧化合物可用作氯(Cl)受體。 According to an embodiment of the present disclosure, an epoxy compound represented by Formula 6 below may be used as a chlorine (Cl) acceptor.

Figure 110147176-A0305-02-0019-8
Figure 110147176-A0305-02-0019-8

其中R1、R2、R3及R4各自獨立地是氫或者具有1至20個碳原子的有機基團。更具體而言，R1、R2、R3及R4可各自獨立地是氫或者具有1至20個碳原子的經取代或未經取代的烴基。根據本揭露的實施例，R1、R2、R3及R4可各自獨立地是氫或者具有1至10個碳原子的烷基。 wherein R 1 , R 2 , R 3 and R 4 are each independently hydrogen or an organic group having 1 to 20 carbon atoms. More specifically, R 1 , R 2 , R 3 and R 4 may each independently be hydrogen or a substituted or unsubstituted hydrocarbon group having 1 to 20 carbon atoms. According to an embodiment of the present disclosure, R 1 , R 2 , R 3 and R 4 may each independently be hydrogen or an alkyl group having 1 to 10 carbon atoms.

根據本揭露的實施例，在由式6表示的環氧化合物中，環氧丙烷(propylene oxide，PO)可用作氯(Cl)受體。 According to an embodiment of the present disclosure, among the epoxy compounds represented by Formula 6, propylene oxide (PO) may be used as a chlorine (Cl) acceptor.

用作氯(Cl)受體的環氧化合物可根據以下反應方案1與鹽酸(HCl)或氯(Cl)進行反應。 Epoxy compounds serving as chlorine (Cl) acceptors can be reacted with hydrochloric acid (HCl) or chlorine (Cl) according to Reaction Scheme 1 below.

Figure 110147176-A0305-02-0019-9
Figure 110147176-A0305-02-0019-9

在本揭露的一個實施例中，氯(Cl)受體與鹽酸(HCl)的反應產物在製造所述光學膜的製程中被移除。作為結果，氯(Cl) 可被移除。然而，氯(Cl)受體的反應產物以及氯(Cl)可能保留於所述光學膜中而不被移除。據以，根據本揭露實施例的所述光學膜可包含痕量的氯(Cl)受體與鹽酸(HCl)的反應產物或者氯(Cl)。 In one embodiment of the present disclosure, the reaction product of chlorine (Cl) acceptors and hydrochloric acid (HCl) is removed during the process of manufacturing the optical film. As a result, chlorine (Cl) can be removed. However, reaction products of chlorine (Cl) acceptors and chlorine (Cl) may remain in the optical film without being removed. Accordingly, the optical film according to an embodiment of the present disclosure may contain a trace amount of a reaction product of a chlorine (Cl) acceptor and hydrochloric acid (HCl) or chlorine (Cl).

當環氧丙烷(PO)用作氯(Cl)受體時，所述氯受體可根據以下反應方案2與鹽酸(HCl)進行反應：

Figure 110147176-A0305-02-0020-10
When propylene oxide (PO) is used as the chlorine (Cl) acceptor, the chlorine acceptor can be reacted with hydrochloric acid (HCl) according to the following reaction scheme 2:
Figure 110147176-A0305-02-0020-10

基於50微米的厚度，根據本揭露實施例的所述光學膜可具有3或小於3的黃度指標。另外，基於50微米的厚度，根據本揭露實施例的所述光學膜可具有2或小於2的黃度指標、或者1或小於1的黃度指標。 The optical film according to an embodiment of the present disclosure may have a yellowness index of 3 or less based on a thickness of 50 micrometers. In addition, the optical film according to an embodiment of the present disclosure may have a yellowness index of 2 or less, or a yellowness index of 1 or less based on a thickness of 50 micrometers.

基於50微米的厚度，根據本揭露實施例的所述光學膜可具有88%或大於88%的光透射率。另外，基於50微米的厚度，根據本揭露實施例的所述光學膜可具有90%或大於90%的光透射率、或91%或大於91%的光透射率。 Based on a thickness of 50 micrometers, the optical film according to an embodiment of the present disclosure may have a light transmittance of 88% or more. In addition, the optical film according to an embodiment of the present disclosure may have a light transmittance of 90% or more, or a light transmittance of 91% or more based on a thickness of 50 micrometers.

可根據美國材料試驗協會(American Society for Testing Material，ASTM)E313標準使用分光光度計在360奈米至740奈米的波長範圍中量測黃度指標及光透射率。本文中所使用的分光 光度計為例如由柯尼卡美能達(KONICA MINOLTA)製造的CM-3700D。 According to American Society for Testing Materials (ASTM) E313 standard, a spectrophotometer can be used to measure the yellowness index and light transmittance in the wavelength range of 360 nm to 740 nm. spectroscopic used in this paper The photometer is, for example, CM-3700D manufactured by KONICA MINOLTA.

基於50微米的厚度，根據本揭露實施例的所述光學膜可具有1.0%或小於1.0%的霧度。 The optical film according to an embodiment of the present disclosure may have a haze of 1.0% or less based on a thickness of 50 micrometers.

霧度可根據ASTM D1003使用霧度計來量測。具有50毫米×50毫米的大小的光學膜樣品可用於霧度量測。所述樣品的霧度可取藉由執行五次量測而獲得的五個霧度值的平均值。在本揭露的實施例中，由村上顏色研究實驗室(Murakami Color Research Laboratory)生產的HM-150可用作霧度計。 Haze can be measured using a haze meter according to ASTM D1003. Optical film samples having a size of 50 mm x 50 mm can be used for haze measurement. The haze of the sample may take an average value of five haze values obtained by performing five measurements. In an embodiment of the present disclosure, HM-150 manufactured by Murakami Color Research Laboratory may be used as a haze meter.

根據本揭露實施例的所述光學膜可應用於顯示元件，以保護顯示面板的顯示表面。根據本揭露實施例的所述光學膜可具有足以保護顯示面板的厚度。舉例而言，所述光學膜可具有10微米至100微米的厚度。 The optical film according to an embodiment of the present disclosure can be applied to a display element to protect a display surface of a display panel. The optical film according to an embodiment of the present disclosure may have a thickness sufficient to protect a display panel. For example, the optical film may have a thickness of 10 microns to 100 microns.

在下文中，將參照圖1及圖2對根據本揭露示例性實施例的包括所述光學膜的顯示元件進行闡述。 Hereinafter, a display element including the optical film according to an exemplary embodiment of the present disclosure will be described with reference to FIGS. 1 and 2 .

圖1是示出根據另一實施例的顯示元件200的一部分的剖視圖，且圖2是圖1中的部分「P」的放大剖視圖。 FIG. 1 is a cross-sectional view illustrating a part of a display element 200 according to another embodiment, and FIG. 2 is an enlarged cross-sectional view of a portion 'P' in FIG. 1 .

參照圖1，根據本揭露另一實施例的顯示元件200包括顯示面板501及位於顯示面板501上的光學膜100。 Referring to FIG. 1 , a display device 200 according to another embodiment of the present disclosure includes a display panel 501 and an optical film 100 on the display panel 501 .

參照圖1及圖2，顯示面板501包括基板510、位於基板510上的薄膜電晶體TFT、以及連接至薄膜電晶體TFT的有機發光元件570。有機發光元件570包括第一電極571、位於第一電 極571上的有機發光層572及位於有機發光層572上的第二電極573。圖1及圖2中所示的顯示元件200是有機發光顯示元件。 1 and 2, the display panel 501 includes a substrate 510, a thin film transistor TFT on the substrate 510, and an organic light emitting element 570 connected to the thin film transistor TFT. The organic light emitting element 570 includes a first electrode 571, located at the first electrode The organic light emitting layer 572 on the electrode 571 and the second electrode 573 on the organic light emitting layer 572 . The display element 200 shown in FIGS. 1 and 2 is an organic light emitting display element.

基板510可由玻璃或塑膠形成。具體而言，基板510可由塑膠(例如，聚醯亞胺系樹脂)形成。儘管未示出，然而可在基板510上設置緩衝層。 The substrate 510 may be formed of glass or plastic. Specifically, the substrate 510 may be formed of plastic (eg, polyimide resin). Although not shown, a buffer layer may be disposed on the substrate 510 .

薄膜電晶體TFT設置於基板510上。薄膜電晶體TFT包括半導體層520、與半導體層520絕緣且與半導體層520至少局部地交疊的閘極電極530、連接至半導體層520的源極電極541、以及與源極電極541間隔開且連接至半導體層520的汲極電極542。 The thin film transistor TFT is disposed on the substrate 510 . The thin film transistor TFT includes a semiconductor layer 520, a gate electrode 530 insulated from the semiconductor layer 520 and at least partially overlapping the semiconductor layer 520, a source electrode 541 connected to the semiconductor layer 520, and a source electrode 541 spaced apart from the source electrode 541 and Connected to the drain electrode 542 of the semiconductor layer 520 .

參照圖2，在閘極電極530與半導體層520之間設置閘極絕緣層535。可在閘極電極530上設置層間絕緣層551，且源極電極541及汲極電極542可設置於層間絕緣層551上。 Referring to FIG. 2 , a gate insulating layer 535 is disposed between the gate electrode 530 and the semiconductor layer 520 . An interlayer insulating layer 551 may be disposed on the gate electrode 530 , and a source electrode 541 and a drain electrode 542 may be disposed on the interlayer insulating layer 551 .

在薄膜電晶體TFT上設置平坦化層552，以將薄膜電晶體TFT的頂部平坦化。 A planarization layer 552 is provided on the thin film transistor TFT to planarize the top of the thin film transistor TFT.

第一電極571設置於平坦化層552上。第一電極571藉由設置於平坦化層552中的接觸孔連接至薄膜電晶體TFT。 The first electrode 571 is disposed on the planarization layer 552 . The first electrode 571 is connected to the thin film transistor TFT through a contact hole disposed in the planarization layer 552 .

在平坦化層552上在第一電極571的一部分中設置堤層(bank layer)580，以界定畫素區域或發光區域。舉例而言，堤層580以矩陣的形式設置於多個畫素之間的邊界處，以界定相應的畫素區。 A bank layer 580 is disposed in a part of the first electrode 571 on the planarization layer 552 to define a pixel area or a light emitting area. For example, the bank layer 580 is arranged in a matrix form at the boundary between a plurality of pixels to define corresponding pixel areas.

有機發光層572設置於第一電極571上。有機發光層572亦可設置於堤層580上。有機發光層572可包括一個發光層或 在垂直方向上堆疊的二或更多個發光層。可自有機發光層572發射具有紅色、綠色及藍色中的任一種顏色的光，且可自有機發光層572發射白光。 The organic light emitting layer 572 is disposed on the first electrode 571 . The organic light emitting layer 572 can also be disposed on the bank layer 580 . The organic light-emitting layer 572 may include a light-emitting layer or Two or more light-emitting layers stacked in the vertical direction. Light having any one of red, green, and blue colors may be emitted from the organic light emitting layer 572 , and white light may be emitted from the organic light emitting layer 572 .

第二電極573設置於有機發光層572上。 The second electrode 573 is disposed on the organic light emitting layer 572 .

可對第一電極571、有機發光層572及第二電極573進行堆疊以構成有機發光元件570。 The first electrode 571 , the organic light emitting layer 572 and the second electrode 573 can be stacked to form the organic light emitting element 570 .

儘管未示出，然而當有機發光層572發射白光時，每一畫素可包括用於基於特定波長對自有機發光層572發射的白光進行過濾的彩色濾光片(color filter)。所述彩色濾光片形成於光路徑中。 Although not shown, when the organic light emitting layer 572 emits white light, each pixel may include a color filter for filtering white light emitted from the organic light emitting layer 572 based on a specific wavelength. The color filter is formed in the light path.

可在第二電極573上設置薄膜包封層590。薄膜包封層590可包括至少一個有機層及至少一個無機層，且所述至少一個有機層與所述至少一個無機層可交替地設置。 A thin film encapsulation layer 590 may be disposed on the second electrode 573 . The thin film encapsulation layer 590 may include at least one organic layer and at least one inorganic layer, and the at least one organic layer and the at least one inorganic layer may be arranged alternately.

光學膜100設置於具有上述堆疊結構的顯示面板501上。 The optical film 100 is disposed on the display panel 501 having the above stacked structure.

在下文中，將對根據本揭露實施例的製造光學膜的方法進行闡述。 Hereinafter, a method of manufacturing an optical film according to an embodiment of the present disclosure will be described.

根據本揭露實施例的製造光學膜的方法包括：使用二胺化合物、二酐化合物、第一二羰基化合物及第一氯(Cl)受體形成第一反應溶液；向第一反應溶液添加第二二羰基化合物及第二氯(Cl)受體，且容許其間的反應以形成第二反應溶液；向第二反應溶液添加脫水劑及醯亞胺化觸媒，且容許其間的反應以形成第三反應溶液；對第三反應溶液進行處理以製備固相的聚合物樹脂；將 固相聚合物樹脂溶解以製備聚合物樹脂溶液；以及對聚合物樹脂溶液進行鑄製。在下文中，將詳細闡述每一步驟。 The method for manufacturing an optical film according to an embodiment of the present disclosure includes: forming a first reaction solution using a diamine compound, a dianhydride compound, a first dicarbonyl compound, and a first chlorine (Cl) acceptor; adding a second reaction solution to the first reaction solution; A dicarbonyl compound and a second chlorine (Cl) acceptor, and allowing a reaction therebetween to form a second reaction solution; adding a dehydrating agent and an imidization catalyst to the second reaction solution, and allowing a reaction therebetween to form a third reaction solution Reaction solution; The third reaction solution is processed to prepare the polymer resin of solid phase; dissolving the solid phase polymer resin to prepare a polymer resin solution; and casting the polymer resin solution. Hereinafter, each step will be explained in detail.

首先，使用二胺化合物、二酐化合物、第一二羰基化合物及第一氯(Cl)受體形成第一反應溶液。 First, a first reaction solution is formed using a diamine compound, a dianhydride compound, a first dicarbonyl compound, and a first chlorine (Cl) acceptor.

用於製備第一反應溶液的溶劑可為例如極性非質子溶劑，如N,N-二甲基乙醯胺(N,N-dimethylacetamide，DMAc)、N,N-二甲基甲醯胺(N,N-dimethylformamide，DMF)、1-甲基-2-吡咯啶酮(1-methyl-2-pyrrolidinone，NMP)、間甲酚、四氫呋喃(THF)、氯仿、甲基乙基酮(methyl ethyl ketone，MEK)或其混合物。然而，根據本揭露實施例的溶劑不限於此，且可使用其他溶劑。 The solvent used to prepare the first reaction solution can be, for example, a polar aprotic solvent, such as N,N-dimethylacetamide (N,N-dimethylacetamide, DMAc), N,N-dimethylformamide (N , N-dimethylformamide, DMF), 1-methyl-2-pyrrolidinone (1-methyl-2-pyrrolidinone, NMP), m-cresol, tetrahydrofuran (THF), chloroform, methyl ethyl ketone (methyl ethyl ketone , MEK) or mixtures thereof. However, the solvent according to an embodiment of the present disclosure is not limited thereto, and other solvents may be used.

上述式1的化合物可用作二胺化合物，且上述式2的化合物可用作二酐化合物。由上述式3表示的二羰基化合物可用作第一二羰基化合物。 The compound of Formula 1 above can be used as the diamine compound, and the compound of Formula 2 above can be used as the dianhydride compound. The dicarbonyl compound represented by Formula 3 above may be used as the first dicarbonyl compound.

舉例而言，二胺化合物可為對苯二胺、間苯二胺、4,4'-二胺基二苯醚、3,4'-二胺基二苯醚、3,3'-二胺基二苯醚、4,4'-二胺基二苯碸、3,4'-二胺基二苯碸、3,3'-二胺基二苯碸、2,2'-雙(三氟甲基)聯苯胺(2,2'-bis(trifluoromethyl)benzidine，TFDB)或類似物。 For example, the diamine compound can be p-phenylenediamine, m-phenylenediamine, 4,4'-diaminodiphenyl ether, 3,4'-diaminodiphenyl ether, 3,3'-diamine Diphenyl ether, 4,4'-diaminodiphenyl, 3,4'-diaminodiphenyl, 3,3'-diaminodiphenyl, 2,2'-bis(trifluoro Methyl)benzidine (2,2'-bis(trifluoromethyl)benzidine, TFDB) or the like.

二酐化合物可為環丁烷-1,2,3,4-四羧酸二酐(cyclobutane-1,2,3,4-tetracarboxylic dianhydride，CBDA)、3,3',4,4'-聯苯四羧酸二酐(3,3',4,4'-biphenyltetracarboxylic dianhydride，BPDA)、4,4'-(六氟伸異丙基)二鄰苯二甲酸二酐(4,4'-(hexafluoroisopropylidene)diphthalic dianhydride，6FDA)或類似 物。 The dianhydride compound can be cyclobutane-1,2,3,4-tetracarboxylic dianhydride (cyclobutane-1,2,3,4-tetracarboxylic dianhydride, CBDA), 3,3',4,4'-linked Benzene tetracarboxylic dianhydride (3,3',4,4'-biphenyltetracarboxylic dianhydride, BPDA), 4,4'-(hexafluoroisopropyl) diphthalic dianhydride (4,4'-( hexafluoroisopropylidene) diphthalic dianhydride, 6FDA) or similar thing.

二羰基化合物可為對苯二甲醯二氯(terephthaloyl dichloride，TPC)、間苯二甲醯二氯(isophthaloyl chloride，IPC)、萘二甲酸二氯、4,4'-聯苯二甲酸二氯、3,3'-聯苯二甲酸二氯或類似物。 The dicarbonyl compound can be terephthaloyl dichloride (TPC), isophthaloyl chloride (IPC), naphthalene dichloride, 4,4'-biphenyl dichloride , 3,3'-biphenyl dicarboxylic acid dichloride or the like.

二胺化合物、二酐化合物及第一二羰基化合物可單獨使用或以其中的二或更多者的組合使用。 The diamine compound, the dianhydride compound, and the first dicarbonyl compound may be used alone or in combination of two or more thereof.

根據本揭露的實施例，以100莫耳份(parts by mole)的二胺化合物計，二酐化合物可以20莫耳份至60莫耳份的量來使用。 According to an embodiment of the present disclosure, based on 100 parts by mole of the diamine compound, the dianhydride compound may be used in an amount of 20 parts by mole to 60 parts by mole.

在二胺化合物與第一二羰基化合物之間的反應期間可能產生氯(Cl)化合物。為移除氯化合物，根據本揭露的實施例，在第一反應溶液的形成中使用第一氯(Cl)受體。 A chlorine (Cl) compound may be generated during the reaction between the diamine compound and the first dicarbonyl compound. To remove chlorine compounds, according to embodiments of the present disclosure, a first chlorine (Cl) acceptor is used in the formation of the first reaction solution.

根據本揭露的實施例，作為第一氯(Cl)受體，可使用環狀醚化合物。環狀醚化合物可例如包括環氧化合物、氧雜環丁烷化合物、四氫呋喃化合物及四氫吡喃化合物中的至少一者。 According to an embodiment of the present disclosure, as the first chlorine (Cl) acceptor, a cyclic ether compound may be used. The cyclic ether compound may, for example, include at least one of an epoxy compound, an oxetane compound, a tetrahydrofuran compound, and a tetrahydropyran compound.

根據本揭露的實施例，由式6表示的環氧化合物可用作第一氯(Cl)受體：

Figure 110147176-A0305-02-0025-12
According to an embodiment of the present disclosure, an epoxy compound represented by Formula 6 may be used as the first chlorine (Cl) acceptor:
Figure 110147176-A0305-02-0025-12

其中R1、R2、R3及R4可各自獨立地是氫或者具有1至20個碳原子的有機基團。更具體而言，R1、R2、R3及R4可各自獨立地是氫或者具有1至20個碳原子的經取代或未經取代的烴基。根據本揭露的實施例，R1、R2、R3及R4可各自獨立地是氫或者具有1至10個碳原子的烷基。 Wherein R 1 , R 2 , R 3 and R 4 may each independently be hydrogen or an organic group having 1 to 20 carbon atoms. More specifically, R 1 , R 2 , R 3 and R 4 may each independently be hydrogen or a substituted or unsubstituted hydrocarbon group having 1 to 20 carbon atoms. According to an embodiment of the present disclosure, R 1 , R 2 , R 3 and R 4 may each independently be hydrogen or an alkyl group having 1 to 10 carbon atoms.

用作第一氯(Cl)受體的環氧化合物可根據以下反應方案1與鹽酸(HCl)進行反應。作為結果，可自第一反應溶液移除鹽酸(HCl)。 The epoxy compound used as the first chlorine (Cl) acceptor can be reacted with hydrochloric acid (HCl) according to Reaction Scheme 1 below. As a result, hydrochloric acid (HCl) can be removed from the first reaction solution.

Figure 110147176-A0305-02-0026-13
Figure 110147176-A0305-02-0026-13

根據本揭露的實施例，在環氧化合物中，環氧丙烷(PO)可用作第一氯(Cl)受體。 According to an embodiment of the present disclosure, among epoxy compounds, propylene oxide (PO) may be used as the first chlorine (Cl) acceptor.

當環氧丙烷(PO)用作第一氯(Cl)受體時，可根據以下反應方案2自第一反應溶液移除鹽酸(HCl)：[反應方案2]

Figure 110147176-A0305-02-0027-14
When propylene oxide (PO) is used as the first chlorine (Cl) acceptor, hydrochloric acid (HCl) can be removed from the first reaction solution according to the following Reaction Scheme 2: [Reaction Scheme 2]
Figure 110147176-A0305-02-0027-14

根據本揭露的實施例，以莫耳數計，第一氯(Cl)受體的含量可為第一二羰基化合物的含量的4倍至7倍。慮及二胺與第一羰基化合物之間的反應方案，理論上，當第一氯(Cl)受體的含量是第一二羰基化合物的含量的兩倍時，由二胺與第一二羰基化合物之間的反應產生的鹽酸(HCl)可藉由第一氯受體而被移除。然而，本發明者發現，當第一氯(Cl)受體的莫耳含量小於第一二羰基化合物的莫耳含量的4倍時，氯(Cl)移除效率由於第一氯(Cl)受體與鹽酸(HCl)之間的不充分反應而降低。另外，當第一氯(Cl)受體的莫耳數高於二羰基化合物的莫耳數的7倍時，聚合度由於過量的氯(Cl)受體而降低。因此，根據本揭露的實施例，以莫耳數計，將第一氯(Cl)受體的含量調節至第一二羰基化合物的含量的4倍至7倍。 According to an embodiment of the present disclosure, the content of the first chlorine (Cl) acceptor may be 4 times to 7 times the content of the first dicarbonyl compound in terms of moles. Considering the reaction scheme between the diamine and the first carbonyl compound, in theory, when the content of the first chlorine (Cl) acceptor is twice the content of the first dicarbonyl compound, the diamine and the first dicarbonyl The hydrochloric acid (HCl) produced by the reaction between the compounds can be removed by the first chlorine acceptor. However, the present inventors have found that when the molar content of the first chlorine (Cl) acceptor is less than 4 times the molar content of the first dicarbonyl compound, the chlorine (Cl) removal efficiency is lower than that of the first chlorine (Cl) acceptor. reduced due to insufficient reaction between the body and hydrochloric acid (HCl). In addition, when the molar number of the first chlorine (Cl) acceptor is higher than 7 times that of the dicarbonyl compound, the degree of polymerization decreases due to the excess chlorine (Cl) acceptor. Therefore, according to an embodiment of the present disclosure, the content of the first chlorine (Cl) acceptor is adjusted to be 4 times to 7 times the content of the first dicarbonyl compound in terms of moles.

根據本揭露的實施例，第一反應溶液包含聚醯胺酸及聚醯胺重複單元。 According to an embodiment of the present disclosure, the first reaction solution includes polyamide acid and polyamide repeating units.

接著，向第一反應溶液添加第二二羰基化合物及第二氯(Cl)受體並使其與第一反應溶液進行反應，以形成第二反應溶液。舉例而言，在形成第一反應溶液之後1至24小時，可向第一反應 溶液添加第二二羰基化合物及第二氯(Cl)受體。更具體而言，在形成第一反應溶液之後1至20小時，可向第一反應溶液添加第二二羰基化合物及第二氯(Cl)受體。 Next, a second dicarbonyl compound and a second chlorine (Cl) acceptor are added to the first reaction solution and reacted with the first reaction solution to form a second reaction solution. For example, 1 to 24 hours after the formation of the first reaction solution, the first reaction The solution adds a second dicarbonyl compound and a second chlorine (Cl) acceptor. More specifically, the second dicarbonyl compound and the second chlorine (Cl) acceptor may be added to the first reaction solution 1 to 20 hours after the first reaction solution is formed.

根據本揭露的實施例，當第二二羰基化合物及第二氯(Cl)受體被添加至第一反應溶液時，所述反應溶液被稱為第二反應溶液。 According to an embodiment of the present disclosure, when a second dicarbonyl compound and a second chlorine (Cl) acceptor are added to the first reaction solution, the reaction solution is referred to as a second reaction solution.

根據本揭露的實施例，第一二羰基化合物與第二二羰基化合物可為相同的材料。然而，本揭露的實施例不限於此，且第一二羰基化合物與第二二羰基化合物可為不同的材料。第一二羰基化合物與第二二羰基化合物統稱為二羰基化合物。 According to an embodiment of the present disclosure, the first dicarbonyl compound and the second dicarbonyl compound may be the same material. However, the embodiments of the present disclosure are not limited thereto, and the first dicarbonyl compound and the second dicarbonyl compound may be different materials. The first dicarbonyl compound and the second dicarbonyl compound are collectively referred to as dicarbonyl compounds.

根據本揭露的實施例，第一氯(Cl)受體與第二氯(Cl)受體可為相同的材料。然而，本揭露的實施例不限於此，且第一氯(Cl)受體與第二氯(Cl)受體可為不同的材料。第一氯(Cl)受體與第二氯(Cl)受體統稱為氯(Cl)受體。 According to an embodiment of the present disclosure, the first chlorine (Cl) acceptor and the second chlorine (Cl) acceptor may be the same material. However, embodiments of the present disclosure are not limited thereto, and the first chlorine (Cl) acceptor and the second chlorine (Cl) acceptor may be different materials. The first chlorine (Cl) acceptor and the second chlorine (Cl) acceptor are collectively referred to as the chlorine (Cl) acceptor.

根據本揭露的實施例，第二氯(Cl)受體可包括環狀醚化合物。用作第二氯(Cl)受體的環狀醚化合物可為環氧化合物、氧雜環丁烷化合物、四氫呋喃化合物或四氫吡喃化合物。環狀醚化合物可包括環氧丙烷化合物。 According to an embodiment of the present disclosure, the second chlorine (Cl) acceptor may include a cyclic ether compound. The cyclic ether compound used as the second chlorine (Cl) acceptor may be an epoxy compound, an oxetane compound, a tetrahydrofuran compound, or a tetrahydropyran compound. The cyclic ether compound may include a propylene oxide compound.

可藉由改變第二二羰基化合物及第二氯(Cl)受體的量來對反應溶液的黏度進行調節。根據本揭露的實施例，在形成第二反應溶液期間，可添加第二二羰基化合物及第二氯(Cl)受體，直至第二反應溶液的表觀黏度(apparent viscosity)達到250±30帕 秒(Ps)為止。根據本揭露的實施例，藉由將第二反應溶液分份至100毫升消泡杯(defoaming cup)中以製備反應溶液樣品以及使用黏度計(布魯克菲爾德(Brookfield)，DV2TRV)的第六心軸以20轉/分鐘(revolutions per minute，rpm)對反應溶液樣品進行量測來對所述表觀黏度進行量測。在量測完成之後，將經分份的反應溶液樣品注射至容納所述第二反應溶液的反應罐中，且然後執行後續處理。 The viscosity of the reaction solution can be adjusted by changing the amount of the second dicarbonyl compound and the second chlorine (Cl) acceptor. According to an embodiment of the present disclosure, during the formation of the second reaction solution, a second dicarbonyl compound and a second chlorine (Cl) acceptor may be added until the apparent viscosity of the second reaction solution reaches 250±30 Pa seconds (Ps). According to an embodiment of the present disclosure, the reaction solution samples were prepared by aliquoting the second reaction solution into 100 ml defoaming cups and using the sixth spindle of a viscometer (Brookfield, DV2TRV) The apparent viscosity is measured by measuring the reaction solution sample at 20 revolutions per minute (rpm). After the measurement is completed, the portioned reaction solution sample is injected into the reaction tank containing the second reaction solution, and then subsequent processing is performed.

根據本揭露的實施例，以莫耳數計，第二氯(Cl)受體的含量可為第二二羰基化合物的含量的4倍至7倍。 According to an embodiment of the present disclosure, the content of the second chlorine (Cl) acceptor may be 4 times to 7 times the content of the second dicarbonyl compound in terms of moles.

根據本揭露的實施例，以100莫耳份的二胺化合物計，第一二羰基化合物與第二二羰基化合物的總含量可為40莫耳份至80莫耳份。具體而言，以100莫耳份的二胺化合物計，第一二羰基化合物的含量可為35莫耳份至79莫耳份，且第二二羰基化合物的含量可為1莫耳份至5莫耳份。 According to an embodiment of the present disclosure, based on 100 mole parts of the diamine compound, the total content of the first dicarbonyl compound and the second dicarbonyl compound may be 40 mole parts to 80 mole parts. Specifically, based on 100 mole parts of the diamine compound, the content of the first dicarbonyl compound may be 35 mole parts to 79 mole parts, and the content of the second dicarbonyl compound may be 1 mole part to 5 mole parts. Mole portion.

更具體而言，以100莫耳份的二胺化合物計，第一二羰基化合物的含量可為37莫耳份至79莫耳份。以100莫耳份的二胺化合物計，第二二羰基化合物的含量可為1莫耳份至3莫耳份。 More specifically, based on 100 mole parts of the diamine compound, the content of the first dicarbonyl compound may be 37 to 79 mole parts. Based on 100 mole parts of the diamine compound, the content of the second dicarbonyl compound may be 1 to 3 mole parts.

接著，向第二反應溶液添加脫水劑及醯亞胺化觸媒並使其與第二反應溶液進行反應，以形成第三反應溶液。 Next, a dehydrating agent and an imidization catalyst are added to the second reaction solution to react with the second reaction solution to form a third reaction solution.

在形成第三反應溶液期間，醯胺酸的一部分可被醯亞胺化以形成醯亞胺重複單元。 During formation of the third reaction solution, a portion of the amide acid may be imidized to form an amide repeating unit.

根據本揭露的實施例，向第二反應溶液添加脫水劑及醯 亞胺化觸媒，隨後在60℃至80℃的溫度下進行迴流達30分鐘至2小時。作為結果，可形成第三反應溶液。 According to an embodiment of the present disclosure, adding a dehydrating agent and an acyl to the second reaction solution The catalyst is imidized, followed by reflux at a temperature of 60° C. to 80° C. for 30 minutes to 2 hours. As a result, a third reaction solution may be formed.

作為脫水劑，可使用例如乙酸酐(acetic anhydride，AA)、丙酸酐、異丁酸酐、特戊酸酐、丁酸酐或異戊酸酐等酸酐。 As the dehydrating agent, for example, an acid anhydride such as acetic anhydride (AA), propionic anhydride, isobutyric anhydride, pivalic anhydride, butyric anhydride, or isovaleric anhydride can be used.

作為醯亞胺化觸媒，可使用例如異喹啉、β-甲基吡啶或吡啶(pyridine，Py)等三級胺。 As the imidization catalyst, for example, tertiary amines such as isoquinoline, β-picoline, or pyridine (pyridine, Py) can be used.

可藉由第一氯(Cl)受體、第二氯(Cl)受體及醯亞胺化觸媒來對第三反應溶液的pH進行調節。根據本揭露的實施例，第三反應溶液可具有8或大於8的pH。 The pH of the third reaction solution can be adjusted by the first chlorine (Cl) acceptor, the second chlorine (Cl) acceptor and the imidization catalyst. According to an embodiment of the present disclosure, the third reaction solution may have a pH of 8 or greater.

根據本揭露的實施例，可將為形成第二反應溶液而添加的第二氯(Cl)受體的含量調節成使得第三反應溶液的pH為8至9。根據本揭露的實施例，第三反應溶液具有8至9的pH。 According to an embodiment of the present disclosure, the content of the second chlorine (Cl) acceptor added for forming the second reaction solution may be adjusted such that the pH of the third reaction solution is 8-9. According to an embodiment of the present disclosure, the third reaction solution has a pH of 8-9.

當第三反應溶液具有8至9的弱鹼性pH時，在形成第一反應溶液及第二反應溶液期間產生的鹽酸(HCl)中的所有者或大部分與氯(Cl)受體進行反應。 When the third reaction solution has a weak alkaline pH of 8 to 9, all or most of hydrochloric acid (HCl) generated during the formation of the first reaction solution and the second reaction solution reacts with the chlorine (Cl) acceptor .

當第三反應溶液的pH小於8時，在形成第一反應溶液及第二反應溶液期間產生的鹽酸(HCl)將很有可能不會被充分移除，且氯(Cl)及衍生自保留下來的鹽酸(HCl)的氯化合物將保留於聚醯胺-醯亞胺系膜中。 When the pH of the third reaction solution is less than 8, hydrochloric acid (HCl) generated during the formation of the first reaction solution and the second reaction solution will most likely not be sufficiently removed, and chlorine (Cl) and derivatives thereof remain. Chlorine compounds of hydrochloric acid (HCl) will remain in the polyamide-imide film.

慮及第三反應溶液的pH，醯亞胺化觸媒可以二酐化合物的莫耳量的2倍至7倍的莫耳量來使用。 In consideration of the pH of the third reaction solution, the imidization catalyst may be used in a molar amount of 2 to 7 times the molar amount of the dianhydride compound.

接著，對第三反應溶液進行處理以製備固相的聚合物樹 脂。 Next, the third reaction solution is processed to prepare a solid-phase polymer tree fat.

為製備固相聚合物樹脂，可向第三反應溶液添加溶劑。溶劑可為例如乙醇、甲醇、己烷或類似物。溶劑可單獨使用或以二或更多種溶劑的混合物使用。 To prepare a solid-phase polymer resin, a solvent may be added to the third reaction solution. The solvent can be, for example, ethanol, methanol, hexane or the like. The solvents may be used alone or as a mixture of two or more solvents.

當向第三反應溶液添加具有低極性且能夠與聚合溶劑徹底混合的溶劑時，粉末相的固體聚合物樹脂沈澱。藉由對沈澱物進行過濾及乾燥，可獲得高純度的固體聚合物樹脂。當在對沈澱物進行過濾的製程中移除液體組分時，未反應的單體、寡聚物、添加劑及反應副產物(例如鹽酸(HCl)與氯(Cl)受體的反應產物)被移除。因此而獲得的固體聚合物樹脂不包含氯(Cl)，或僅包含痕量的氯(Cl)。聚合物樹脂可包含醯亞胺重複單元及醯胺重複單元。聚合物樹脂可為例如聚醯胺-醯亞胺樹脂。 When a solvent having low polarity and capable of being thoroughly mixed with a polymerization solvent is added to the third reaction solution, a solid polymer resin of a powder phase precipitates. By filtering and drying the precipitate, a high-purity solid polymer resin can be obtained. Unreacted monomers, oligomers, additives, and reaction by-products (such as reaction products of hydrochloric acid (HCl) and chlorine (Cl) acceptors) are removed when the liquid components are removed during the process of filtering the precipitate. remove. The solid polymer resin thus obtained contains no chlorine (Cl), or only traces of chlorine (Cl). The polymeric resin may comprise imide repeat units and amide repeat units. The polymer resin may be, for example, polyamide-imide resin.

接著，將固相聚合物樹脂溶解以製備聚合物樹脂溶液。藉由將固相聚合物樹脂溶解於溶劑中，可製備聚合物樹脂溶液。此步驟亦被稱為「再溶解(re-dissolution)」。 Next, the solid-phase polymer resin is dissolved to prepare a polymer resin solution. A polymer resin solution can be prepared by dissolving a solid phase polymer resin in a solvent. This step is also called "re-dissolution".

用於將固相聚合物樹脂溶解的溶劑可與聚合中所使用的溶劑中的任一者相同。可用於將固相聚合物樹脂溶解的溶劑可為例如極性非質子溶劑，例如N,N-二甲基乙醯胺(DMAc)、N,N-二甲基甲醯胺(DMF)、1-甲基-2-吡咯啶酮(NMP)、間甲酚、四氫呋喃(THF)、氯仿、甲基乙基酮(MEK)或其混合物。然而，根據本揭露的溶劑不限於此，且亦可使用其他眾所習知的溶劑。 The solvent used to dissolve the solid-phase polymer resin may be the same as any of the solvents used in polymerization. Solvents that can be used to dissolve the solid-phase polymer resin can be, for example, polar aprotic solvents such as N,N-dimethylacetamide (DMAc), N,N-dimethylformamide (DMF), 1- Methyl-2-pyrrolidone (NMP), m-cresol, tetrahydrofuran (THF), chloroform, methyl ethyl ketone (MEK) or mixtures thereof. However, the solvent according to the present disclosure is not limited thereto, and other well-known solvents may also be used.

根據本揭露的實施例，經再溶解的聚合物樹脂溶液可具 有6至7的pH。根據本揭露的實施例，聚醯胺-醯亞胺樹脂溶液可具有弱酸性或接近於中性的弱酸性。第三反應溶液是以8至9的弱鹼性pH而製備，使得聚合物樹脂溶液可被賦予6至7的弱酸性pH。 According to an embodiment of the present disclosure, the redissolved polymer resin solution may have Has a pH of 6 to 7. According to an embodiment of the present disclosure, the polyamide-imide resin solution may have a weak acidity or a weak acidity close to neutral. The third reaction solution is prepared with a weakly basic pH of 8-9, so that the polymer resin solution can be given a weakly acidic pH of 6-7.

接著，對聚合物樹脂溶液進行鑄製。 Next, the polymer resin solution is cast.

鑄製基板用於進行鑄製。對於鑄製基板的類型並無特別限制。鑄製基板可為玻璃基板、不鏽(鋼用不鏽鋼(Steel Use Stainless，SUS))基板、特氟隆(Teflon)基板或類似物。根據本揭露的實施例，鑄製基板可為例如玻璃基板。 Casting substrates are used for casting. There is no particular limitation on the type of cast substrate. The cast substrate may be a glass substrate, a stainless (Steel Use Stainless (SUS)) substrate, a Teflon substrate, or the like. According to an embodiment of the present disclosure, the cast substrate may be, for example, a glass substrate.

具體而言，藉由將聚合物樹脂溶液施加至鑄製基板來達成鑄製。塗佈機、刀片或類似物可用於進行鑄製。 Specifically, casting is achieved by applying a polymer resin solution to a casting substrate. A coater, blade or the like can be used for casting.

在鑄製之後，在以2℃/分鐘的速率將溫度昇高至80℃至120℃的同時對聚合物樹脂溶液進行乾燥，以生產聚合物樹脂的塗膜。以此方式生產的塗膜可被稱為所述光學膜的中間體。在將塗膜拉緊至針式拉幅機(pin-type tenter)並固定至所述針式拉幅機之後，在以3℃/分鐘的昇溫速率將溫度自120℃昇高至250℃至350℃的同時執行熱處理。當溫度達到最高塗膜形成溫度時，可在恆溫氣氛中執行額外的熱處理達10分鐘至30分鐘。作為結果，可製造出光學膜。 After casting, the polymer resin solution was dried while raising the temperature to 80° C. to 120° C. at a rate of 2° C./minute to produce a coating film of the polymer resin. The coating film produced in this way can be referred to as an intermediate of the optical film. After the coating film was tensioned to a pin-type tenter and fixed to the pin-type tenter, the temperature was raised from 120°C to 250°C at a temperature increase rate of 3°C/min. Heat treatment is performed at 350°C. When the temperature reaches the highest coating film forming temperature, additional heat treatment may be performed in a constant temperature atmosphere for 10 minutes to 30 minutes. As a result, an optical film can be manufactured.

在下文中，將參照示例性實例及比較例更詳細地對本揭露進行闡述。然而，實例及比較例不應被解釋為限制本揭露的範圍。 Hereinafter, the present disclosure will be explained in more detail with reference to illustrative examples and comparative examples. However, examples and comparative examples should not be construed as limiting the scope of the present disclosure.

<實例1> <Example 1>

在4頸雙夾套反應器(4-neck double-jacket reactor)中，將80.06克(250毫莫耳)的TFDB(二胺化合物)溶解於二甲基乙醯胺(DMAc)(溶劑)中。向其添加19.86克(68毫莫耳)的BPDA(二酐化合物)，隨後在將溫度維持在25℃的同時攪拌達2小時。在反應完成時，向其添加13.33克(30毫莫耳)的6FDA(二酐化合物)，隨後在25℃下攪拌達1小時。在反應器溫度降低至7℃或小於7℃之後，向其添加29.945克(148毫莫耳)的TPC(第一二羰基化合物)及環氧丙烷(PO)(38.55克，664毫莫耳，TPC的莫耳數的4.5倍)(第一氯受體)。將混合物在7℃下攪拌達1小時[第一反應溶液的形成]。 In a 4-neck double-jacket reactor, 80.06 g (250 mmol) of TFDB (diamine compound) was dissolved in dimethylacetamide (DMAc) (solvent) . 19.86 g (68 mmol) of BPDA (dianhydride compound) was added thereto, followed by stirring for 2 hours while maintaining the temperature at 25°C. When the reaction was completed, 13.33 g (30 mmol) of 6FDA (dianhydride compound) was added thereto, followed by stirring at 25° C. for 1 hour. After the reactor temperature was lowered to 7° C. or less than 7° C., 29.945 g (148 mmol) of TPC (the first dicarbonyl compound) and propylene oxide (PO) (38.55 g, 664 mmol, 4.5 times the molar number of TPC) (first chlorine acceptor). The mixture was stirred at 7° C. for 1 hour [formation of first reaction solution].

容許第一反應溶液在室溫下靜置達1小時，對第一反應溶液的黏度進行了量測，並向其進一步添加TPC(1.269克，6毫莫耳)(第二二羰基化合物)及環氧丙烷(PO)(1.63克，28毫莫耳，TPC的莫耳數的4.5倍)(第二氯受體)，直至第二反應溶液的表觀黏度達到250±30帕秒為止[第二反應溶液的形成]。 The first reaction solution was allowed to stand at room temperature for 1 hour, the viscosity of the first reaction solution was measured, and TPC (1.269 g, 6 mmol) (the second dicarbonyl compound) and Propylene oxide (PO) (1.63 g, 28 millimolar, 4.5 times the molar number of TPC) (second chlorine acceptor) until the apparent viscosity of the second reaction solution reaches 250 ± 30 Pas [No. Formation of the second reaction solution].

在聚合完成之後，向第二反應溶液進一步添加作為醯亞胺化觸媒的吡啶(Py)(16.97克，BPDA+6FDA的莫耳數的2.2倍)及作為脫水劑的乙酸酐(AA)(21.97克，BPDA+6FDA的莫耳數的2.2倍)，隨後將溫度昇高至80℃並攪拌達1小時[第三反應溶液的形成]。 After the polymerization was completed, pyridine (Py) (16.97 grams, 2.2 times the molar number of BPDA+6FDA) and acetic anhydride (AA) as a dehydrating agent were further added to the second reaction solution as an imidization catalyst ( 21.97 g, 2.2 times the number of moles of BPDA+6FDA), then the temperature was raised to 80° C. and stirred for 1 hour [formation of a third reaction solution].

將燒瓶冷卻至室溫，並將第三反應溶液倒入至甲醇 (3,000毫升)中以誘發沈澱。對沈澱物進行過濾以獲得作為白色固體的聚合物樹脂。所獲得的聚合物樹脂是固體粉末。在實例1中製備的聚合物樹脂是聚醯胺-醯亞胺聚合物樹脂。 The flask was cooled to room temperature, and the third reaction solution was poured into methanol (3,000 ml) to induce precipitation. The precipitate was filtered to obtain the polymer resin as a white solid. The obtained polymer resin is a solid powder. The polymer resin prepared in Example 1 was a polyamide-imide polymer resin.

將作為固體粉末獲得的聚合物樹脂以12.7重量%的濃度溶解於二甲基乙醯胺(DMAc)中，以製備聚合物樹脂溶液。 The polymer resin obtained as a solid powder was dissolved in dimethylacetamide (DMAc) at a concentration of 12.7% by weight to prepare a polymer resin solution.

在基板上鑄製所製備的聚合物樹脂溶液。具體而言，使用邁耶棒塗機(Mayer bar coater)將聚合物樹脂溶液施加至玻璃基板，並用80℃的熱空氣進行處理達10分鐘，以形成塗膜。 The prepared polymer resin solution was cast on a substrate. Specifically, the polymer resin solution was applied to a glass substrate using a Mayer bar coater, and treated with hot air at 80° C. for 10 minutes to form a coating film.

隨後，在將溫度自80℃昇高至120℃的同時，使塗膜經歷初步熱處理(primary heat treatment)達17分鐘。將所獲得的中間塗膜拉緊至針式拉幅機，將其固定於所述針式拉幅機上，並放置於烘箱中，且然後以3℃/分鐘的昇溫速率將溫度自120℃昇高至270℃。在達到270℃時，在恆溫氣氛中使塗膜經歷二次熱處理(secondary heat treatment)達10分鐘。 Subsequently, while raising the temperature from 80°C to 120°C, the coating film was subjected to primary heat treatment for 17 minutes. The obtained intermediate coating film was stretched to a pin tenter, fixed on the pin tenter, and placed in an oven, and then the temperature was raised from 120° C. at a temperature increase rate of 3° C./min. raised to 270°C. Upon reaching 270° C., the coating film was subjected to secondary heat treatment for 10 minutes in a constant temperature atmosphere.

為移除殘留的應力，將經二次熱處理的塗膜自拉幅機分離，且然後使所述經二次熱處理的塗膜在270℃下經歷第三熱處理(third heat treatment)達1分鐘。作為結果，製造出了具有50微米的厚度的光學膜。 In order to remove the residual stress, the secondary heat-treated coating film was separated from the tenter, and then the secondary heat-treated coating film was subjected to a third heat treatment at 270° C. for 1 minute. As a result, an optical film having a thickness of 50 micrometers was produced.

<實例2至實例5> <Example 2 to Example 5>

使用在實例1中揭露的方法在下表1中闡述的條件下製造出了根據實例2至實例5的光學膜。 Optical films according to Examples 2 to 5 were manufactured using the method disclosed in Example 1 under the conditions set forth in Table 1 below.

<比較例1至比較例3> <Comparative Example 1 to Comparative Example 3>

使用在實例1中揭露的方法在下表1中闡述的條件下製造出了根據比較例1至比較例3的光學膜。 The optical films according to Comparative Example 1 to Comparative Example 3 were manufactured using the method disclosed in Example 1 under the conditions set forth in Table 1 below.

Figure 110147176-A0305-02-0035-15
Figure 110147176-A0305-02-0035-15

在表1中，用語「莫耳份」是指以100莫耳的TFDB(其為二胺化合物)計的莫耳數。用於指示環氧丙烷(PO)的含量的用語「倍數」是指以TPC的莫耳數計的倍數，且用於指示吡啶(Py)及乙酸酐(AA)的含量的用語「倍數」是指以二酐的莫耳數計的倍數。 In Table 1, the term "parts by mole" refers to the number of moles based on 100 moles of TFDB (which is a diamine compound). The term "multiple" used to indicate the content of propylene oxide (PO) refers to a multiple in moles of TPC, and the term "multiple" used to indicate the content of pyridine (Py) and acetic anhydride (AA) is Refers to the multiple of moles of dianhydride.

在實例1至實例5以及比較例1至比較例3中製造的光學膜的物理特性被量測如下。 The physical properties of the optical films manufactured in Examples 1 to 5 and Comparative Examples 1 to 3 were measured as follows.

(1)L*a*b*量測 (1) L*a*b* measurement

使用CIE標準光源D65對CIE 1976顏色空間中的L*a*b*進行了量測。 L*a*b* in CIE 1976 color space was measured using CIE standard illuminant D65.

D65光源：D65標準光源是發射表示日光的光的光源，所述光具有被指派至溫度T68的為6504K的相關色溫。 D65 Illuminant: The D65 standard illuminant is a light source that emits light representing sunlight with a correlated color temperature of 6504K assigned to a temperature T68.

用於L*a*b*量測的設備是來自柯尼卡美能達的CM-3700D，且使得能夠在360奈米至740奈米的整個可見光波長範圍 內以10奈米的節距(pitch)進行量測。 The equipment used for L*a*b* measurements is the CM-3700D from Konica Minolta and enables the entire visible wavelength range from 360 nm to 740 nm Measured at a pitch of 10 nm.

(2)色差(△E)的量測 (2) Measurement of color difference (△E)

將所製造的光學膜(具有50微米的厚度)切割至50毫米×50毫米的大小以生產樣品，並使用以上(1)的方法對樣品的L*a*b*進行了量測。作為結果，獲得了L*1、a*1及b*1。 The produced optical film (having a thickness of 50 μm) was cut to a size of 50 mm×50 mm to produce a sample, and L*a*b* of the sample was measured using the method of (1) above. As a result, L*1, a*1, and b*1 are obtained.

接著，在150℃的烘箱中對樣品進行熱處理達30分鐘，且然後在維持25℃的平均溫度及30%的平均相對濕度的同時使用裝備有氙燈的齊桑(Q-Sun)裝置(桑泰斯特XXL+(Suntest XXL+))以0.8瓦/平方公尺的光劑量、以420奈米的中心波長將其曝光達150小時。 Next, the samples were heat-treated in an oven at 150°C for 30 minutes, and then maintained with an average temperature of 25°C and an average relative humidity of 30% using a Q-Sun apparatus (Santex) equipped with a xenon lamp. Suntest XXL+ (Suntest XXL+) was exposed for 150 hours at a light dose of 0.8 W/m2 at a central wavelength of 420 nm.

氙燈：使用了由亞伯奈科(Abnexo)(阿特拉斯(Atlas)的進口商)生產的氙燈(型號名稱：NXE 1700)，其為一種在相應波長處具有最相似於陽光的能量的燈。 Xenon lamp: A xenon lamp (model name: NXE 1700) produced by Abnexo (an importer of Atlas), which is a lamp having energy most similar to sunlight at the corresponding wavelength, was used. lamp.

在熱處理及曝光處理之後，使用在(1)中闡述的方法對樣品的L*a*b*進行了量測。作為結果，獲得了L*2、a*2及b*2。 After heat treatment and exposure treatment, L*a*b* of the samples were measured using the method described in (1). As a result, L*2, a*2, and b*2 are obtained.

計算出了在熱處理及曝光之前及之後L*的變化(即，△L*)、a*的變化(即，△a*)及b*的變化(即，△b*)，並根據以下方程式1計算出了色差(△E)。 The change in L* (i.e., ΔL*), the change in a* (i.e., Δa*) and the change in b* (i.e., Δb*) before and after heat treatment and exposure were calculated, and according to the following equation 1 The color difference (ΔE) was calculated.

[方程式1] △E=[(△L*)2+(△a*)2+(△b*)2]1/2 [Equation 1] △E=[(△L*) 2 +(△a*) 2 +(△b*) 2 ] 1/2

[方程式2] △L*=L*2-L*1 [Equation 2] △L*=L*2-L*1

[方程式3] △a*=a*2-a*1 [Equation 3] △a*=a*2-a*1

[方程式4] △b*=b*2-b*1 [Equation 4] △b*=b*2-b*1

(3)黃度指標(Y.I.)：根據ASTM E313標準使用分光光度計(CM-3700D，柯尼卡美能達)對黃度指標進行了量測。在熱處理及曝光處理之前，對具有50微米的厚度的光學膜的黃度指標進行了量測。 (3) Yellowness index (Y.I.): The yellowness index was measured using a spectrophotometer (CM-3700D, Konica Minolta) according to the ASTM E313 standard. The yellowness index of the optical film having a thickness of 50 micrometers was measured before heat treatment and exposure treatment.

(4)光透射率(TT)(%)：根據ASTM E313標準使用分光光度計(CM-3700D，柯尼卡美能達)對在360奈米至740奈米的波長下的平均光學透射率進行了量測。對具有50微米的厚度的光學膜在熱處理及曝光之前的光透射率進行了量測。 (4) Optical transmittance (TT) (%): The average optical transmittance at a wavelength of 360 nm to 740 nm was measured using a spectrophotometer (CM-3700D, Konica Minolta) according to ASTM E313 standard measured. The light transmittance of an optical film having a thickness of 50 micrometers before heat treatment and exposure was measured.

(5)霧度(%)：將所製造的光學膜切割至50毫米×50毫米的大小，使用由村上顏色研究實驗室生產的霧度計(型號名稱：HM-150)根據ASTM D1003將霧度量測了5次，並取霧度值的平均值作為霧度。對具有50微米的厚度的光學膜在熱處理及曝光之前的霧度進行了量測。 (5) Haze (%): The manufactured optical film was cut to a size of 50 mm × 50 mm, and the haze was measured according to ASTM D1003 using a haze meter (model name: HM-150) produced by Murakami Color Research Laboratory. The measurement was measured 5 times, and the average value of the haze value was taken as the haze. Haze was measured for optical films having a thickness of 50 micrometers before heat treatment and exposure.

(6)氯(Cl)含量(ppm) (6) Chlorine (Cl) content (ppm)

氯(Cl)的含量被表達為氯的濃度(ppm)。 The chlorine (Cl) content is expressed as chlorine concentration (ppm).

將50微米厚的光學膜切割成約0.5公分×0.5公分的片件，將其冷凍乾燥、製成粉末，且然後使用蒸餾水進行超聲萃取達2小時，以獲得氯(Cl)萃取物。藉由對氯萃取物執行離子層析分 析(ion chromatography analysis)並計算氯的濃度而對氯含量進行了量測。對於離子層析分析，將兩個管柱[艾恩派克AS18分析柱(IonPac AS18 Analytical)(4×250毫米)+AG18保護柱(AG18 Guard)(4×50毫米)]及溶析液[來自戴安(Dionex)的EGC-KOH III筒(EGC-KOH III Cartridge)]放置於來自戴安的ICS-2000離子層析系統中。 A 50 micron thick optical film was cut into approximately 0.5 cm x 0.5 cm pieces, freeze-dried, powdered, and then subjected to ultrasonic extraction using distilled water for 2 hours to obtain chlorine (Cl) extracts. By performing ion chromatography analysis on the chlorine extract Chlorine content was measured by ion chromatography analysis and calculation of chlorine concentration. For ion chromatography analysis, two columns [IonPac AS18 Analytical Column (IonPac AS18 Analytical) (4 × 250 mm) + AG18 Guard Column (AG18 Guard) (4 × 50 mm)] and eluent [from An EGC-KOH III Cartridge from Dionex] was placed in an ICS-2000 ion chromatography system from Dionex.

具體而言，氯(Cl)的含量被量測如下。 Specifically, the content of chlorine (Cl) was measured as follows.

量測裝置：在來自戴安的ICS-2000離子層析系統中，使用兩個管柱[艾恩派克AS18分析柱(4×250毫米)+AG18保護柱(4×50毫米)]及溶析液[來自戴安的EGC-KOH III筒]執行了離子層析分析。 Measuring device: In the ICS-2000 ion chromatography system from Diane, use two columns [Air Park AS18 analytical column (4 × 250 mm) + AG18 guard column (4 × 50 mm)] and elution Ion chromatography analysis was performed on the liquid [EGC-KOH III cartridge from Dionex].

量測方法：將在實例1至實例5以及比較例1至比較例3中製造的各所述50微米厚光學膜切割至約0.5公分×0.5公分的大小，隨後將其冷凍乾燥並粉碎，以製備光學膜粉末。然後，將所述光學膜粉末以5重量%的濃度與蒸餾水進行混合，且然後自光學膜萃取出氯(Cl)，特別是氯離子(Cl-)。具體而言，將0.2克光學膜粉末及3.8克水裝入20毫升小瓶中，並使用由必能信超聲(Branson Ultrasonics)生產的5510超聲浴(5510 ultrasonic bath)執行超聲萃取達2小時。作為結果，製備出了包含自光學膜萃取出的氯(Cl)的氯萃取混合物。藉由0.45微米耐綸過濾器對所製備的氯萃取混合物進行了過濾，以製備用於量測的樣品。將20微升用於量測的樣品注射至設定在30℃的管柱溫度(column temperature)及35℃的量測單元格溫度(measurement cell temperature)下的離子層析元件中，且然後對分離的離子波峰中對應於氯離子的波峰的面積進行了偵測。為計算氯離子含量，利用蒸餾水對來自賽默科學(Thermo Scientific)的戴安七種陰離子標準液(Dionex Seven Anion Standard)進行了稀釋，以製備濃度範圍為0.04ppm至1ppm(0.04ppm、0.06ppm、0.08ppm、0.1ppm及1.0ppm)的標準氯離子溶液，並以與針對用於量測的樣品的相同方式對所述標準氯離子溶液執行了離子層析分析。藉由對使用標準溶液而量測的對應於氯離子的波峰的面積進行偵測來繪製出校準曲線。 Measurement method: each of the 50-micrometer-thick optical films produced in Example 1 to Example 5 and Comparative Example 1 to Comparative Example 3 was cut to a size of about 0.5 cm×0.5 cm, then freeze-dried and pulverized to obtain Prepare optical film powder. Then, the optical film powder was mixed with distilled water at a concentration of 5% by weight, and then chlorine (Cl), particularly chloride ions (Cl − ), were extracted from the optical film. Specifically, 0.2 g of optical film powder and 3.8 g of water were charged into a 20 ml vial, and ultrasonic extraction was performed for 2 hours using a 5510 ultrasonic bath manufactured by Branson Ultrasonics. As a result, a chlorine extraction mixture containing chlorine (Cl) extracted from the optical film is prepared. The prepared chlorine extraction mixture was filtered through a 0.45 micron nylon filter to prepare a sample for measurement. 20 microliters of the sample for measurement was injected into an ion chromatography element set at a column temperature of 30°C and a measurement cell temperature of 35°C, and then the separation The area of the ion peak corresponding to the chloride ion was detected. To calculate the chloride ion content, Dionex Seven Anion Standard from Thermo Scientific was diluted with distilled water to prepare concentrations ranging from 0.04ppm to 1ppm (0.04ppm, 0.06ppm , 0.08 ppm, 0.1 ppm, and 1.0 ppm) of standard chloride ion solutions, and ion chromatography analysis was performed on the standard chloride ion solutions in the same manner as for the samples used for measurement. A calibration curve was drawn by detecting the area of the peak corresponding to chloride ions measured using standard solutions.

校準曲線被表達為以下方程式5中的一次函數：[方程式5] y=ax+b The calibration curve is expressed as a linear function in Equation 5 below: [Equation 5] y=ax+b

其中y是波峰面積，x是標準溶液的濃度，a是校準曲線的斜率，且b是校準曲線的y軸截距。藉由將在方程式5中獲得的校準曲線應用於用於量測的樣品的波峰面積(y)，可計算用於量測的樣品的氯濃度(x)。用於量測的樣品的氯濃度(x)可使用以下方程式6來獲得。 where y is the peak area, x is the concentration of the standard solution, a is the slope of the calibration curve, and b is the y-intercept of the calibration curve. By applying the calibration curve obtained in Equation 5 to the peak area (y) of the sample for measurement, the chlorine concentration (x) of the sample for measurement can be calculated. The chlorine concentration (x) of the sample used for measurement can be obtained using Equation 6 below.

[方程式6] x=(y-b)/a [Equation 6] x=(y-b)/a

接著，慮及應用於製備用於量測的樣品的稀釋比，計算光學膜中的氯含量。具體而言，應用於用於量測的樣品的光學膜的 重量比可使用以下方程式7來計算：[方程式7]光學膜在用於量測的樣品中的重量比=(光學膜的重量)/(光學膜的重量+蒸餾水的重量) Next, the chlorine content in the optical film was calculated in consideration of the dilution ratio applied to prepare samples for measurement. Specifically, the optical film applied to the sample used for measurement The weight ratio can be calculated using the following Equation 7: [Equation 7] Weight ratio of the optical film in the sample used for measurement = (weight of the optical film) / (weight of the optical film + weight of distilled water)

其中所述光學膜的重量是用於生產用於量測的樣品的光學膜的重量。 Wherein the weight of the optical film is the weight of the optical film used to produce the sample for measurement.

接著，使用光學膜相對於用於量測的樣品的重量比以及用於量測的樣品中的氯濃度，根據以下方程式8計算光學膜的氯濃度。 Next, using the weight ratio of the optical film to the sample for measurement and the chlorine concentration in the sample for measurement, the chlorine concentration of the optical film was calculated according to Equation 8 below.

[方程式8]光學膜的氯濃度=(用於量測的樣品中的氯濃度)/(光學膜對用於量測的樣品的重量比) [Equation 8] Chlorine concentration of optical film=(chlorine concentration in sample for measurement)/(weight ratio of optical film to sample for measurement)

量測結果示出於以下表2及表3中。 The measurement results are shown in Table 2 and Table 3 below.

Figure 110147176-A0305-02-0040-16
Figure 110147176-A0305-02-0040-16

Figure 110147176-A0305-02-0040-17
Figure 110147176-A0305-02-0040-17
Figure 110147176-A0305-02-0041-18
Figure 110147176-A0305-02-0041-18

如可自表2及表3中的量測結果看出，根據本揭露實施例的所述光學膜表現出低的色差(△E)、低的黃度指標、優異的光透射率、低的霧度及低的氯(Cl)含量。 As can be seen from the measurement results in Table 2 and Table 3, the optical film according to the disclosed embodiment exhibits low chromatic aberration (ΔE), low yellowness index, excellent light transmittance, low Haze and low chlorine (Cl) content.

100:光學膜 100: Optical film

200:顯示元件 200: display components

501:顯示面板 501: display panel

P:部分 P: part

Claims (10)

一種光學膜，在150℃下進行熱處理達30分鐘以及暴露於可見光達150小時之前及之後具有3.5或小於3.5的色差(△E)，其中所述色差(△E)是基於在國際照明委員會1976 L*a*b*顏色空間中量測的值而使用以下方程式1來計算：[方程式1] △E=[(△L*)2+(△a*)2+(△b*)2]1/2其中△L*、△a*及△b*分別是根據所述國際照明委員會1976 L*a*b*顏色空間的所述光學膜的L*、a*及b*在所述光學膜經歷在150℃的溫度下進行熱處理達30分鐘以及暴露於可見光達150小時之前及之後的差，其中L*a*b*是使用國際照明委員會標準光源D65而量測，且所述暴露於可見光是藉由在平均溫度為25℃及平均相對濕度為30%的環境條件下使用氙燈以0.8瓦/平方公尺的光劑量、420奈米的中心波長向所述光學膜照射可見光達150小時來執行。 An optical film having a color difference (ΔE) of 3.5 or less before and after heat treatment at 150°C for 30 minutes and exposure to visible light for 150 hours, wherein the color difference (ΔE) is based on the International Commission on Illumination 1976 The value measured in the L*a*b* color space is calculated using the following Equation 1: [Equation 1] △E=[(△L*) 2 +(△a*) 2 +(△b*) 2 ] 1/2 where △L*, △a* and △b* are L*, a* and b* of the optical film in the optical The difference before and after the film was subjected to heat treatment at a temperature of 150°C for 30 minutes and exposure to visible light for 150 hours, where L*a*b* was measured using the International Commission on Illumination standard illuminant D65, and the exposure to Visible light is obtained by irradiating visible light to the optical film for 150 hours at an average temperature of 25°C and an average relative humidity of 30% using a xenon lamp with a light dose of 0.8 watts/square meter and a central wavelength of 420 nm. to execute. 如請求項1所述的光學膜，其中所述光學膜具有3.2或小於3.2的所述色差(△E)。 The optical film according to claim 1, wherein the optical film has the chromatic aberration (ΔE) of 3.2 or less. 如請求項1所述的光學膜，其中按重量計，所述光學膜包含120ppm(0.012重量%)或小於120ppm(0.012重量%)的氯(Cl)。 The optical film according to claim 1, wherein the optical film contains 120 ppm (0.012% by weight) or less of chlorine (Cl) by weight. 如請求項1所述的光學膜，其中按重量計，所述光學 膜包含50ppm(0.005重量%)或小於50ppm(0.005重量%)的氯(Cl)。 The optical film as claimed in claim 1, wherein by weight, the optical The film contains 50 ppm (0.005% by weight) or less of chlorine (Cl). 如請求項1所述的光學膜，其中基於50微米的厚度，所述光學膜具有3或小於3的黃度指標。 The optical film of claim 1, wherein the optical film has a yellowness index of 3 or less based on a thickness of 50 micrometers. 如請求項1所述的光學膜，其中基於50微米的厚度，所述光學膜具有1.0%或小於1.0%的霧度。 The optical film of claim 1, wherein the optical film has a haze of 1.0% or less based on a thickness of 50 micrometers. 如請求項1所述的光學膜，其中基於50微米的厚度，所述光學膜具有88%或大於88%的光透射率。 The optical film of claim 1, wherein the optical film has a light transmittance of 88% or more based on a thickness of 50 micrometers. 如請求項1所述的光學膜，其中所述光學膜包含醯亞胺重複單元及醯胺重複單元中的至少一者。 The optical film according to claim 1, wherein the optical film comprises at least one of an amide repeating unit and an amide repeating unit. 如請求項1所述的光學膜，其中按重量計，所述光學膜包含30ppm(0.003重量%)或小於30ppm(0.003重量%)的環狀醚化合物。 The optical film according to claim 1, wherein the optical film contains 30 ppm (0.003% by weight) or less of the cyclic ether compound by weight. 一種顯示元件，包括：顯示面板；以及如請求項1至請求項9中任一項所述的光學膜，設置於所述顯示面板上。 A display element, comprising: a display panel; and the optical film according to any one of claim 1 to claim 9, disposed on the display panel.
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