TW201824298A - Transparent conductive film attached with carrier film and touch panel using the same capable of preventing a resistance value of the transparent conductive film from becoming abnormal by controlling a moisture content of a protective film - Google Patents
Transparent conductive film attached with carrier film and touch panel using the same capable of preventing a resistance value of the transparent conductive film from becoming abnormal by controlling a moisture content of a protective film Download PDFInfo
- Publication number
- TW201824298A TW201824298A TW105141598A TW105141598A TW201824298A TW 201824298 A TW201824298 A TW 201824298A TW 105141598 A TW105141598 A TW 105141598A TW 105141598 A TW105141598 A TW 105141598A TW 201824298 A TW201824298 A TW 201824298A
- Authority
- TW
- Taiwan
- Prior art keywords
- film
- transparent conductive
- conductive film
- resin
- transparent
- Prior art date
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Abstract
Description
本發明關於包含透明導電性薄膜與載體薄膜的附載體薄膜之透明導電性薄膜及使用其之觸控面板，為尤其防止電阻值異常及膜剝離之有用技術。The present invention relates to a transparent conductive film with a carrier film including a transparent conductive film and a carrier film, and a touch panel using the same, and is a useful technique for particularly preventing abnormal resistance values and film peeling.
背景技術 於觸控面板等之領域中，近年來日益追求其薄型化，伴隨於此亦希望透明導電性薄膜本身之薄型化。作為一般的觸控面板之方式，可列舉電阻膜方式、靜電容方式等。近年來，觸控面板大多採用之靜電容方式，廣泛使用聚對苯二甲酸乙二酯(PET)作為透明導電性薄膜之基材薄膜，因為具有可撓性、加工性優異，且耐衝擊性優異、為輕量等優點。BACKGROUND ART In the field of touch panels and the like, thickness reduction has been increasingly pursued in recent years, and along with this, the thickness reduction of the transparent conductive film itself is also desired. Examples of a general touch panel method include a resistive film method and a capacitive method. In recent years, the capacitive method of most touch panels is widely used. Polyethylene terephthalate (PET) is widely used as the base film of transparent conductive films, because of its flexibility, excellent processability, and impact resistance. Excellent and lightweight.
隨著基材薄膜之薄型化，為了確保製造步驟階段中之基材薄膜之處理性，在基材薄膜之與透明導電層相反之面側經由黏著劑層貼合之表面保護薄膜之必要性提高。一般而言，表面保護薄膜與基材薄膜相同，廣泛使用PET。With the thinning of the substrate film, in order to ensure the rationality of the substrate film in the manufacturing step stage, the necessity of a surface protective film bonded via an adhesive layer on the side of the substrate film opposite to the transparent conductive layer has increased. . In general, the surface protection film is the same as the base film, and PET is widely used.
於專利文獻1中揭示有一種非晶質透明導電性積層體，其於以PET作為基材之透明導電性薄膜上，在未形成透明導電層之面側利用黏著劑層貼合並積層以PET作為基材之保護薄膜。Patent Document 1 discloses an amorphous transparent conductive laminated body, which is laminated on a transparent conductive film using PET as a substrate, and an adhesive layer is laminated on the surface side where the transparent conductive layer is not formed, and the laminated layer is made of PET. Protective film for substrate.
另一方面，用於靜電容方式之觸控面板電極用之ITO(銦錫複合氧化物)，為形成高感度、高解析度之圖案，需要較低的表面電阻值。於專利文獻2中揭示有一種積層體，其於以PET作為薄膜基材之透明導電性薄膜上積層有保護薄膜。使用ITO作為透明導電體層時，雖然藉由利用加熱使ITO結晶化而使之低電阻化，但於該專利文獻2中進一步沈積四價金屬元素之氧化物之比例較大之銦系複合氧化物，沈積氧化銦或四價金屬元素之氧化物之比例較小之銦系複合氧化物，使ITO膜低電阻化。On the other hand, ITO (Indium Tin Composite Oxide) for touch panel electrodes of the electrostatic capacitance method requires a low surface resistance value in order to form a pattern with high sensitivity and high resolution. Patent Document 2 discloses a laminated body in which a protective film is laminated on a transparent conductive film using PET as a film substrate. When ITO is used as a transparent conductor layer, although ITO is crystallized by heating to reduce its resistance, in Patent Document 2 is further deposited an indium-based composite oxide having a large proportion of an oxide of a tetravalent metal element. Indium-based composite oxides with a small proportion of indium oxide or oxides of tetravalent metal elements are deposited to reduce the resistance of the ITO film.
先行技術文獻 專利文獻 專利文獻1：WO2008-108255號公報 專利文獻2：日本特開2012-112031號公報Prior technical documents Patent documents Patent document 1: WO2008-108255 Patent document 2: Japanese Patent Laid-Open No. 2012-112031
發明概要 發明欲解決之問題 然而，PET薄膜由於在基材本身含有較多水分，受到該水分的影響，而無法充分地進行透明導電膜之結晶化。即，由於受到該水分的影響阻礙透明導電膜之結晶成長，不僅結晶化速度變慢，且電阻值上升或變動，發生透明導電性薄膜之電阻值異常、或透明導電膜與基材之密接性降低，於界面發生膜剝離。本發明者們進行研究發現：如此之薄膜水分量的影響，不僅來自於透明導電性薄膜之基材，在透明導電性薄膜結合有保護薄膜之形態中，來自於保護薄膜尤其大。SUMMARY OF THE INVENTION Problems to be Solved by the Invention However, since the PET film contains a large amount of water in the base material, and is affected by the water, the transparent conductive film cannot be sufficiently crystallized. In other words, the crystalline growth of the transparent conductive film is hindered by the influence of the moisture, which not only slows down the crystallization rate, but also increases or changes the resistance value, causing abnormalities in the resistance value of the transparent conductive film or the adhesion between the transparent conductive film and the substrate Lowered, and film peeling occurred at the interface. The present inventors conducted research and found that the influence of the moisture content of such a film is not only from the base material of the transparent conductive film, but also from the protective film in the form where the transparent conductive film is combined with the protective film.
因此，本發明之目的在於提供一種附載體薄膜之透明導電性薄膜及使用其之觸控面板，其藉由控制附載體薄膜之透明導電性薄膜之保護薄膜之含水量，而防止透明導電性薄膜之電阻值異常，並且提高透明導電膜與基材之密接性，防止膜剝離。Therefore, an object of the present invention is to provide a transparent conductive film with a carrier film and a touch panel using the same, which can prevent the transparent conductive film by controlling the moisture content of the protective film of the transparent conductive film with a carrier film. The resistance value is abnormal, and the adhesion between the transparent conductive film and the substrate is improved to prevent the film from peeling.
用以解決問題之方法 本發明者們為解決上述問題而致力於研究，結果發現藉由採用下述構成可達成上述目的，終完成本發明。Means for Solving the Problems The present inventors have been working hard to solve the above problems, and as a result, have found that the above-mentioned objects can be achieved by adopting the following constitutions, and the present invention has finally been completed.
即，本發明之附載體薄膜之透明導電性薄膜，其特徵在於包含：透明導電性薄膜，包含透明樹脂薄膜及透明導電膜；以及載體薄膜，包含配置於前述透明導電性薄膜之形成有前述透明樹脂薄膜之面側之黏著劑層及保護薄膜；前述透明導電膜為銦錫複合氧化物，前述保護薄膜之含水量每10mm×10mm為1.0×10-3 g以下。再者，於不特別說明時，本發明中之各種物性值為利用實施例等中採用之方法所測定之值。That is, the transparent conductive film with a carrier film of the present invention includes a transparent conductive film including a transparent resin film and a transparent conductive film; and a carrier film including the transparent film formed on the transparent conductive film. The adhesive layer and the protective film on the front side of the resin film; the transparent conductive film is an indium tin composite oxide, and the moisture content of the protective film is 1.0 × 10 -3 g or less per 10mm × 10mm. In addition, unless otherwise specified, various physical property values in the present invention are values measured by a method used in the examples and the like.
藉由本發明之附載體薄膜之透明導電性薄膜，可防止透明導電性薄膜之電阻值異常，並且提高透明導電膜與基材之密接性，防止膜剝離。電阻值異常及膜剝離之機制雖然尚不明確，但認為原因如下。關於電阻值異常，認為尤其是受到保護薄膜之含水量的影響。其理由為，利用濺鍍透明導電膜之前的退火、除氣過程而進行基材的除氣，因此以水分、釋氣較少之狀態構成透明樹脂薄膜，相對於此，於後續步驟貼合之保護薄膜之水分直接影響製作完成之透明導電膜。進而，若保護薄膜含有較多水分，不但透明導電膜之結晶化無法充分進行、無法獲得所期望之電阻值，亦使面內電阻值之不均惡化。認為其原因為，由於基材所吸附之水分或接觸電漿等時所產生之氣體等作為雜質而作用，阻礙結晶成長。關於膜剝離(密接性)，推測為於透明導電膜與基材(透明樹脂薄膜等)之界面進行氧化反應，藉此於界面附近局部地產生結晶性變形(晶格常數改變)，因此密接性降低、發生膜剝離。即，認為因水分的影響，於透明導電膜與基材之界面進行氧化，因此密接性降低、發生膜剝離。The transparent conductive film with a carrier film according to the present invention can prevent abnormal resistance values of the transparent conductive film, improve the adhesion between the transparent conductive film and the substrate, and prevent film peeling. Although the mechanism of abnormal resistance value and film peeling is not clear, the reason is thought to be as follows. Regarding the abnormal resistance value, it is thought that it is particularly affected by the moisture content of the protective film. The reason is that the substrate is degassed by the annealing and degassing process before the transparent conductive film is sputtered. Therefore, a transparent resin film is formed in a state of less moisture and outgassing. The moisture of the protective film directly affects the completed transparent conductive film. Furthermore, if the protective film contains a large amount of water, not only does the crystallization of the transparent conductive film not proceed sufficiently, the desired resistance value cannot be obtained, but also unevenness in the in-plane resistance value is deteriorated. This is considered to be because the moisture adsorbed on the base material or the gas generated when contacting the plasma etc. acts as an impurity and hinders crystal growth. Regarding film peeling (adhesiveness), it is presumed that an oxidation reaction occurs at the interface between the transparent conductive film and the substrate (transparent resin film, etc.), thereby locally causing crystalline deformation (change in lattice constant) in the vicinity of the interface. Reduction and film peeling. That is, it is considered that due to the influence of moisture, the interface between the transparent conductive film and the substrate is oxidized, so that the adhesiveness is reduced and film peeling occurs.
本發明中之透明樹脂薄膜宜具有：第1硬化樹脂層，設置於前述透明導電膜之面側；及第2硬化樹脂層，設置於與前述透明導電膜相反之面側。由於在透明樹脂薄膜之兩面形成有硬化樹脂層，故在形成透明導電膜及圖案化或朝電子機器之搭載等各步驟中不易受損傷。The transparent resin film in the present invention preferably includes: a first hardened resin layer provided on a surface side of the transparent conductive film; and a second hardened resin layer provided on a surface side opposite to the transparent conductive film. Since the hardened resin layers are formed on both sides of the transparent resin film, it is difficult to be damaged in each step of forming a transparent conductive film, patterning, or mounting on an electronic device.
本發明之附載體薄膜之透明導電性薄膜宜於第1硬化樹脂層與前述透明導電膜之間進而具備一層以上之光學調整層。由於藉由光學調整層可控制折射率，故即使在將ITO膜圖案化時亦可減低圖案形成部與圖案開口部之反射率差，不易看見透明導電膜圖案，於觸控面板等顯示裝置中之視認性變得良好。The transparent conductive film with a carrier film of the present invention is preferably provided with one or more optical adjustment layers between the first cured resin layer and the transparent conductive film. Since the refractive index can be controlled by the optical adjustment layer, even when the ITO film is patterned, the difference in reflectance between the pattern forming portion and the pattern opening portion can be reduced, and it is difficult to see the transparent conductive film pattern. In a display device such as a touch panel The visibility becomes good.
本發明中之保護薄膜之厚度宜為1μm~150μm。由於保護薄膜之厚度越薄，越可進而抑制保護薄膜之含水量，充分進行透明導電膜之結晶化，故可更確實地防止透明導電性薄膜之電阻值異常，且可更提高透明導電膜與基材之密接性，防止膜剝離。又，藉由設為前述範圍，可提高捲對捲製法之易搬送性。The thickness of the protective film in the present invention is preferably 1 μm to 150 μm. As the thickness of the protective film is thinner, the moisture content of the protective film can be further suppressed, and the transparent conductive film can be fully crystallized, so that the abnormal resistance value of the transparent conductive film can be prevented more reliably, and the transparent conductive film and the The adhesiveness of the substrate prevents the film from peeling. Moreover, by setting it as the said range, the easy conveyance property of a roll-to-roll method can be improved.
本發明中之保護薄膜宜由環烯烴系樹脂或聚碳酸酯系樹脂構成。藉此，由於可使用含水率較低之樹脂，可進一步控制保護薄膜之含水量，充分進行透明導電膜之結晶化，故可更確實地防止透明導電性薄膜之電阻值異常，且可更提高透明導電膜與基材之密接性，防止膜剝離。The protective film in the present invention is preferably composed of a cycloolefin-based resin or a polycarbonate-based resin. As a result, a resin with a lower moisture content can be used, the moisture content of the protective film can be further controlled, and the transparent conductive film can be fully crystallized. Therefore, the abnormal resistance value of the transparent conductive film can be prevented more reliably, and the resistance can be further improved. The adhesion between the transparent conductive film and the substrate prevents the film from peeling.
本發明中之保護薄膜之水分率宜為0.50重量%以下。藉此，由於可使用含水率較低之保護薄膜，可進一步控制保護薄膜之含水量，充分進行透明導電膜之結晶化，故可更確實地防止透明導電性薄膜之電阻值異常，且可更提高透明導電膜與基材之密接性，防止膜剝離。The moisture content of the protective film in the present invention is preferably 0.50% by weight or less. As a result, a protective film with a lower moisture content can be used, the moisture content of the protective film can be further controlled, and the transparent conductive film can be fully crystallized, so that the abnormal resistance value of the transparent conductive film can be prevented more reliably, and Improve the adhesion between the transparent conductive film and the substrate, and prevent the film from peeling.
於本發明中，宜於保護薄膜之與形成有前述黏著劑層之面成相反之面側進一步具備導電層。藉此，可抗靜電，可抑制不必要電氣之影響。In the present invention, it is preferable that the protective film further includes a conductive layer on a surface side opposite to the surface on which the adhesive layer is formed. This makes it possible to resist static electricity and suppress unnecessary electrical influences.
本發明之觸控面板宜包含前述附載體薄膜之透明導電性薄膜。藉此，由於可更確實地防止透明導電性薄膜之電阻值異常，且可提高透明導電膜與基材之密接性，防止膜剝離，故可形成穩定之高感度、高解析度之圖案，且使觸控面板之顯示裝置之視認性等品質提高。The touch panel of the present invention preferably includes the aforementioned transparent conductive film with a carrier film. As a result, the abnormal resistance value of the transparent conductive film can be prevented more reliably, the adhesion between the transparent conductive film and the substrate can be improved, and the film can be prevented from peeling off. Therefore, a stable high-sensitivity and high-resolution pattern can be formed, and The quality of visibility of the display device of the touch panel is improved.
用以實施發明之形態 一面參照圖式一面如下說明本發明之附載體薄膜之透明導電性薄膜之實施形態。其中，於一部分圖或全部圖中省略不需說明之部分，且為了容易說明，存在有放大或縮小等而進行圖示之部分。表示上下等位置關係之用語，僅為了容易說明而使用，並不意圖限定本發明之構成。Embodiments for Carrying Out the Invention Embodiments of the transparent conductive film with a carrier film of the present invention will be described below with reference to the drawings. Among them, parts that do not need explanation are omitted in some or all of the figures, and for ease of explanation, there are parts that are shown enlarged or reduced. The terms indicating the positional relationship between the upper and lower sides are used for ease of explanation, and are not intended to limit the structure of the present invention.
＜附載體薄膜之透明導電性薄膜＞ 圖1是模式地顯示本發明之附載體薄膜之透明導電性薄膜之一實施形態之剖面圖，圖2是本發明之另一實施形態之附載體薄膜之透明導電性薄膜之模式性剖面圖。本發明之附載體薄膜之透明導電性薄膜，如圖1所示包含：透明導電性薄膜20，包含透明樹脂薄膜3及透明導電膜4；以及載體薄膜10，包含配置於透明導電性薄膜20之形成有透明樹脂薄膜3之面側之黏著劑層2及保護薄膜1。再者，可於保護薄膜1之與形成有前述黏著劑層2之面成相反之面側進一步具備導電層。<Transparent conductive film with a carrier film> FIG. 1 is a cross-sectional view schematically showing one embodiment of the transparent conductive film with a carrier film of the present invention, and FIG. 2 is a schematic view of another embodiment of the present invention with a carrier film. A schematic cross-sectional view of a transparent conductive film. As shown in FIG. 1, the transparent conductive film with a carrier film according to the present invention includes: a transparent conductive film 20 including a transparent resin film 3 and a transparent conductive film 4; and a carrier film 10 including a transparent conductive film 20 An adhesive layer 2 and a protective film 1 on the front side of the transparent resin film 3 are formed. Furthermore, a conductive layer may be further provided on the side of the protective film 1 opposite to the side where the adhesive layer 2 is formed.
又，如圖2所示，透明樹脂薄膜3可具有設置於前述透明導電膜4之面側之第1硬化樹脂層6、及設置於與前述透明導電膜4相反之面側之第2硬化樹脂層5，但亦可僅於單面具有任一者之硬化樹脂層。再者，第1硬化樹脂層6與第2硬化樹脂層5包含作為抗黏著層或硬塗層而起作用之層。可於第1硬化樹脂層6與透明導電膜4之間進而具備一層之光學調整層7，亦可具備二層以上之光學調整層7。再者，於圖2中雖然透明導電性薄膜20依序具有第2硬化樹脂層5、透明樹脂薄膜3、第1硬化樹脂層6、光學調整層7、及透明導電膜4，但例如亦可為依序具有第2硬化樹脂層5、透明樹脂薄膜3、第1硬化樹脂層6及透明導電膜4之透明導電性薄膜20，或依序具有透明樹脂薄膜3、光學調整層7及透明導電膜4之透明導電性薄膜20，可為任意之組合。As shown in FIG. 2, the transparent resin film 3 may include a first hardened resin layer 6 provided on a surface side of the transparent conductive film 4 and a second hardened resin provided on a surface side opposite to the transparent conductive film 4. The layer 5 may have any one of the hardened resin layers only on one side. The first cured resin layer 6 and the second cured resin layer 5 include a layer that functions as an anti-adhesion layer or a hard coat layer. An optical adjustment layer 7 may be further provided between the first hardened resin layer 6 and the transparent conductive film 4, or two or more optical adjustment layers 7 may be provided. In addition, although the transparent conductive film 20 has the second cured resin layer 5, the transparent resin film 3, the first cured resin layer 6, the optical adjustment layer 7, and the transparent conductive film 4 in this order in FIG. 2, for example, it may be A transparent conductive film 20 having a second hardened resin layer 5, a transparent resin film 3, a first hardened resin layer 6, and a transparent conductive film 4 in this order, or a transparent resin film 3, an optical adjustment layer 7, and a transparent conductive member in this order. The transparent conductive thin film 20 of the film 4 may be any combination.
附載體薄膜之透明導電性薄膜之自非晶質朝結晶質之結晶化完成時之到達電阻值(表面電阻值)宜為100~130Ω/□、較佳為100~120Ω/□、更佳為100~110Ω/□。藉此，可形成穩定之高感度、高解析度之圖案。The arrival resistance value (surface resistance value) of the transparent conductive film with a carrier film when the crystallization from amorphous to crystalline is completed is preferably 100 to 130 Ω / □, preferably 100 to 120 Ω / □, and more preferably 100 ~ 110Ω / □. Thereby, a pattern with stable high sensitivity and high resolution can be formed.
附載體薄膜之透明導電性薄膜之自非晶質朝結晶質之結晶化完成時之到達電阻值(表面電阻值)之標準偏差宜為30Ω/□以下、較佳為20Ω/□以下、更佳為10Ω/□以下。藉此，可形成穩定之高感度、高解析度之圖案。The standard deviation of the arrival resistance value (surface resistance value) of the transparent conductive film with a carrier film when the crystallization from amorphous to crystalline is completed is preferably 30 Ω / □ or less, preferably 20 Ω / □ or less, and more preferably It is 10Ω / □ or less. Thereby, a pattern with stable high sensitivity and high resolution can be formed.
＜透明導電性薄膜＞ 透明導電性薄膜具有透明樹脂薄膜及透明導電膜。透明導電性薄膜可具有如下透明樹脂薄膜，即該透明樹脂薄膜具有設置於前述透明導電膜之面側之第1硬化樹脂層、及設置於與前述透明導電膜相反之面側之第2硬化樹脂層。透明導電性薄膜亦可於第1硬化樹脂層與透明導電膜之間進而包含一層以上之光學調整層。<Transparent conductive film> The transparent conductive film includes a transparent resin film and a transparent conductive film. The transparent conductive film may include a transparent resin film having a first hardened resin layer provided on the surface side of the transparent conductive film and a second hardened resin provided on the surface side opposite to the transparent conductive film. Floor. The transparent conductive film may further include one or more optical adjustment layers between the first cured resin layer and the transparent conductive film.
透明導電性薄膜之厚度宜為20~150μm之範圍內、較佳為25~100μm之範圍內、更佳為30~80μm之範圍內。若透明導電性薄膜之厚度為未達上述範圍之下限，有機械強度不足、將薄膜基材以捲筒狀之形式連續地形成硬化樹脂層或透明導電膜之操作變得困難之情形。另一方面，若厚度超過上述範圍之上限，則有不能提升透明導電性薄膜等之耐擦傷性或作為觸控面板用之點擊特性之情形。The thickness of the transparent conductive film is preferably within a range of 20 to 150 μm, preferably within a range of 25 to 100 μm, and more preferably within a range of 30 to 80 μm. If the thickness of the transparent conductive film is less than the lower limit of the above range, the mechanical strength may be insufficient, and it may be difficult to continuously form a film substrate in a roll shape into a hardened resin layer or a transparent conductive film. On the other hand, if the thickness exceeds the upper limit of the above range, the scratch resistance of a transparent conductive film or the like or the click characteristics for a touch panel may not be improved.
(透明樹脂薄膜) 作為透明樹脂薄膜只要為於可見光區域中為透明者即可，並無特別限制，可使用具有透明性之各種塑膠薄膜。例如作為其材料可列舉：聚酯系樹脂、環烯烴系樹脂、聚碳酸酯系樹脂、乙酸酯系樹脂、聚醚碸系樹脂、聚醯胺系樹脂、聚醯亞胺系樹脂、聚烯烴系樹脂、(甲基)丙烯酸系樹脂、聚氯乙烯系樹脂、聚偏二氯乙烯系樹脂、聚苯乙烯系樹脂、聚乙烯醇系樹脂、聚丙烯酸系樹脂、聚芳酯系樹脂、聚苯硫系樹脂等。由視認性變得良好之方面來看，較佳為聚酯系樹脂、環烯烴系樹脂、聚碳酸酯系樹脂，但由高透明性、低吸水性、水分阻斷性、熱穩定性、等方性等觀點來看，尤佳為非晶性樹脂之環烯烴系樹脂或聚碳酸酯系樹脂。(Transparent resin film) The transparent resin film is not particularly limited as long as it is transparent in the visible light region, and various plastic films having transparency can be used. Examples of the material include polyester resins, cycloolefin resins, polycarbonate resins, acetate resins, polyether fluorene resins, polyamine resins, polyimide resins, and polyolefins. Resin, (meth) acrylic resin, polyvinyl chloride resin, polyvinylidene chloride resin, polystyrene resin, polyvinyl alcohol resin, polyacrylic resin, polyarylate resin, polybenzene Sulfur-based resin. From the standpoint of good visibility, polyester resins, cycloolefin resins, and polycarbonate resins are preferred, but from high transparency, low water absorption, moisture blocking properties, thermal stability, etc. From the viewpoints of squareness and the like, a cycloolefin-based resin or a polycarbonate-based resin of an amorphous resin is particularly preferred.
由機械特性或耐熱性之方面，聚酯系樹脂較佳為聚對苯二甲酸乙二酯系樹脂、聚萘二甲酸乙二酯系樹脂等。In terms of mechanical properties or heat resistance, the polyester resin is preferably a polyethylene terephthalate resin, a polyethylene naphthalate resin, or the like.
作為環烯烴系樹脂，只要為具有由環狀烯烴(環烯烴)構成之單體之單元的樹脂即可，並無特別限定。作為透明樹脂薄膜所使用之環烯烴系樹脂，可為環烯烴聚合物(COP)或環烯烴共聚物(COC)之任一者。所謂環烯烴共聚物指環狀烯烴與伸乙基等之烯烴之共聚物的非結晶性環狀烯烴系樹脂。The cycloolefin-based resin is not particularly limited as long as it is a resin having a unit of a monomer composed of a cyclic olefin (cycloolefin). The cycloolefin-based resin used as the transparent resin film may be any of a cycloolefin polymer (COP) or a cycloolefin copolymer (COC). The cyclic olefin copolymer refers to a non-crystalline cyclic olefin-based resin which is a copolymer of a cyclic olefin and an olefin such as ethylene.
所謂上述環狀烯烴，存在有多環式之環狀烯烴與單環式之環狀烯烴。作為該多環式之環狀烯烴，可列舉：降莰烯、甲基降莰烯、二甲基降莰烯、乙基降莰烯、亞乙基降莰烯、丁基降莰烯、二環戊二烯、二氫二環戊二烯、甲基二環戊二烯、二甲基二環戊二烯、四環十二烯、甲基四環十二烯、二甲基環四-十二烯、三環戊二烯、四環戊二烯等。又，作為單環式之環狀烯烴，可列舉：環丁烯、環戊烯、環辛烯、環辛二烯、環辛三烯、環十二碳三烯等。The cyclic olefin includes a polycyclic cyclic olefin and a monocyclic cyclic olefin. Examples of the polycyclic cyclic olefin include norbornene, methyl norbornene, dimethyl norbornene, ethyl norbornene, ethylene norbornene, butyl norbornene, and Cyclopentadiene, dihydrodicyclopentadiene, methyldicyclopentadiene, dimethyldicyclopentadiene, tetracyclododecene, methyl tetracyclododecene, dimethylcyclotetra- Dodecene, tricyclopentadiene, tetracyclopentadiene, etc. Examples of the monocyclic cyclic olefin include cyclobutene, cyclopentene, cyclooctene, cyclooctadiene, cyclooctatriene, and cyclododecatriene.
環烯烴系樹脂可以市售品之形式取得，例如可列舉：日本ZEON公司製「ZEONOR」、JSR公司製「ARTON」、Polyplastics公司製「TOPAS」、三井化學公司製「APEL」等。Cycloolefin-based resins can be obtained in the form of commercially available products, and examples thereof include: "ZEONOR" manufactured by ZEON, "ARTON" manufactured by JSR, "TOPAS" manufactured by Polyplastics, and "APEL" manufactured by Mitsui Chemicals.
聚碳酸酯系樹脂並無特別限定，例如可列舉：脂肪族聚碳酸酯、芳香族聚碳酸酯、脂肪族-芳香族聚碳酸酯等。具體而言，例如可列舉：作為使用雙酚類之聚碳酸酯(PC)之雙酚A聚碳酸酯、支鏈雙酚A聚碳酸酯、發泡聚碳酸酯、共聚碳酸酯、嵌段共聚碳酸酯、聚酯碳酸酯、聚膦酸鹽碳酸酯、雙烯丙基二乙二醇碳酸酯(CR-39)等。於聚碳酸酯系樹脂中亦包含與雙酚A聚碳酸酯摻合物、聚酯摻合物、ABS摻合物、聚烯烴摻合物、苯乙烯-馬來酸酐共聚物摻合物等其他成分摻合而成者。作為聚碳酸酯樹脂之市售品，可列舉：惠和公司製「OPCON」、帝人公司製「PANLITE」、三菱氣體化學製「YUPILON(含紫外線吸收劑之聚碳酸酯)」等。The polycarbonate resin is not particularly limited, and examples thereof include aliphatic polycarbonates, aromatic polycarbonates, and aliphatic-aromatic polycarbonates. Specific examples include bisphenol A polycarbonate, branched bisphenol A polycarbonate, foamed polycarbonate, copolycarbonate, and block copolymerization as bisphenol-based polycarbonate (PC). Carbonate, polyester carbonate, polyphosphonate carbonate, diallyl diethylene glycol carbonate (CR-39), etc. Polycarbonate resins also include bisphenol A polycarbonate blends, polyester blends, ABS blends, polyolefin blends, styrene-maleic anhydride copolymer blends, and others. Ingredients blended. Examples of commercially available polycarbonate resins include "OPCON" manufactured by Huihe Company, "PANLITE" manufactured by Teijin Corporation, "YUPILON (polycarbonate containing ultraviolet absorber)" manufactured by Mitsubishi Gas Chemical, and the like.
於透明樹脂薄膜，亦可對表面預先實施濺鍍、電暈放電、噴火、紫外線照射、電子束照射、化學變化、氧化等蝕刻處理或底層塗佈處理，使與形成於透明樹脂薄膜上之硬化樹脂層或透明導電膜等之密接性提高。又，於形成硬化樹脂層或透明導電膜之前，亦可視需要藉由溶劑洗淨或超音波洗淨等將透明樹脂薄膜表面除塵、清淨化。On the transparent resin film, the surface can also be subjected to an etching treatment such as sputtering, corona discharge, flame spraying, ultraviolet irradiation, electron beam irradiation, chemical change, oxidation, or undercoating treatment in advance to harden the formed on the transparent resin film. Adhesiveness of a resin layer or a transparent conductive film is improved. In addition, before forming the hardened resin layer or the transparent conductive film, the surface of the transparent resin film may be dust-removed and cleaned by solvent cleaning or ultrasonic cleaning, if necessary.
由製造透明性較高、外觀品質優異之透明導電性薄膜等且提高於捲對捲製法中之易搬送性之觀點而言，透明樹脂薄膜之厚度宜為20~150μm之範圍內、較佳為25~100μm之範圍內、更佳為30~80μm之範圍內。若透明樹脂薄膜之厚度為未達上述範圍之下限，有機械強度不足、將薄膜基材以捲筒狀之形式連續地形成硬化樹脂層或透明導電膜之操作變得困難之情形。另一方面，若厚度超過上述範圍之上限，則有不能提升透明導電性薄膜等之耐擦傷性或作為觸控面板用之點擊特性之情形。From the viewpoint of manufacturing a transparent conductive film having high transparency and excellent appearance quality and improving ease of transportability in a roll-to-roll method, the thickness of the transparent resin film is preferably within a range of 20 to 150 μm, and more preferably The range is 25 to 100 μm, and more preferably 30 to 80 μm. If the thickness of the transparent resin film is less than the lower limit of the above range, the mechanical strength may be insufficient, and it may be difficult to continuously form the film substrate in a roll shape to form a hardened resin layer or a transparent conductive film. On the other hand, if the thickness exceeds the upper limit of the above range, the scratch resistance of a transparent conductive film or the like or the click characteristics for a touch panel may not be improved.
透明樹脂薄膜之含水量宜每10mm×10mm為5.0×10-3 g以下、較佳每10mm×10mm為3.0×10-3 g以下、更佳每10mm×10mm為1.0×10-3 g以下。藉此，由於可進一步控制透明樹脂薄膜之含水量，充分進行透明導電膜之結晶化，故可更確實地防止透明導電性薄膜之電阻值異常，且更提高透明導電膜與基材之密接性，防止膜剝離。The moisture content of the transparent resin film is preferably 5.0 × 10 -3 g per 10 mm × 10 mm, preferably 3.0 × 10 -3 g per 10 mm × 10 mm, and more preferably 1.0 × 10 -3 g per 10 mm × 10 mm. Thereby, since the moisture content of the transparent resin film can be further controlled and the transparent conductive film can be fully crystallized, abnormal resistance values of the transparent conductive film can be prevented more reliably, and the adhesion between the transparent conductive film and the substrate can be further improved. To prevent film peeling.
透明樹脂薄膜之水分率宜為0.50重量%以下、較佳為0.40重量%以下、更佳為0.30重量%以下。The moisture content of the transparent resin film is preferably 0.50% by weight or less, preferably 0.40% by weight or less, and more preferably 0.30% by weight or less.
(硬化樹脂層) 硬化樹脂層包含：第1硬化樹脂層，設置於透明樹脂薄膜之透明導電膜之面側；及第2硬化樹脂層，設置於與透明導電膜相反之面側。在透明樹脂薄膜脆弱而容易受傷時，因為在形成透明導電膜及透明導電膜之圖案化或朝電子機器之搭載等各步驟中容易受損傷，故如上所述宜於透明樹脂薄膜之兩面形成第1硬化樹脂層及第2硬化樹脂層。(Hardened resin layer) The hardened resin layer includes: a first hardened resin layer provided on the surface side of the transparent conductive film of the transparent resin film; and a second hardened resin layer provided on the surface side opposite to the transparent conductive film. When the transparent resin film is fragile and easy to be injured, it is easy to be damaged during the steps of forming the transparent conductive film and the patterning of the transparent conductive film or mounting on the electronic device, so it is appropriate to form the first and second sides of the transparent resin film as described above. 1 hardened resin layer and 2 hardened resin layer.
硬化樹脂層是藉由使硬化型樹脂等硬化而獲得之層。作為所使用之樹脂並無特別限制，可使用製成硬化樹脂層形成後之皮膜具有充分之強度、具有透明性者，可列舉：熱硬化型樹脂、紫外線硬化型樹脂、電子束硬化型樹脂、二液混合型樹脂等。其等中，又以藉由紫外線照射之硬化處理，以簡單的加工操作即可有效率地形成硬化樹脂層之紫外線硬化型樹脂為佳。The cured resin layer is a layer obtained by curing a curable resin or the like. The resin to be used is not particularly limited, and a film having sufficient strength and transparency after the formation of the cured resin layer can be used, and examples thereof include thermosetting resin, ultraviolet curing resin, electron beam curing resin, Two-liquid mixed resin. Among these, a UV-curing resin that can efficiently form a hardened resin layer by a simple processing operation with a hardening treatment by ultraviolet irradiation is preferred.
作為紫外線硬化型樹脂，可列舉：聚酯系、丙烯酸系、胺甲酸乙酯系、醯胺系、聚矽氧系、環氧系等各種樹脂，包含紫外線硬化型之單體、低聚物、聚合物等。較佳使用之紫外線硬化型樹脂為丙烯酸系樹脂、環氧系樹脂或胺甲酸乙酯系樹脂，更佳為丙烯酸系樹脂或胺甲酸乙酯系樹脂。Examples of the UV-curable resin include polyester, acrylic, urethane-based, ammonium-based, silicone-based, and epoxy-based resins, and include UV-curable monomers, oligomers, Polymer, etc. The ultraviolet curing resin that is preferably used is an acrylic resin, an epoxy resin or a urethane resin, more preferably an acrylic resin or a urethane resin.
硬化樹脂層亦可包含粒子。藉由於硬化樹脂層中調配粒子，可於硬化樹脂層之表面形成***，可對透明導電性薄膜適當地賦與抗黏著性。The hardened resin layer may also contain particles. By arranging particles in the hardened resin layer, bumps can be formed on the surface of the hardened resin layer, and anti-adhesion properties can be appropriately imparted to the transparent conductive film.
作為上述粒子，可無特別限制地使用各種金屬氧化物、玻璃、塑膠等具有透明性者。例如可列舉：氧化矽、氧化鋁、氧化鈦、氧化鋯、氧化鈣等無機系粒子、由聚甲基丙烯酸甲酯、聚苯乙烯、聚胺甲酸乙酯、丙烯酸系樹脂、丙烯酸-苯乙烯共聚物等丙烯酸-苯乙烯系樹脂、苯代三聚氰胺、三聚氰胺、聚碳酸酯等各種聚合物所形成之交聯或未交聯之有機系粒子、或聚矽氧系粒子等。前述粒子可適當選擇一種或二種以上使用，但以有機系粒子為佳。由折射率之觀點，作為有機系粒子宜為丙烯酸系樹脂及丙烯酸-苯乙烯系樹脂。As the particles, those having transparency such as various metal oxides, glass, and plastics can be used without particular limitation. Examples include inorganic particles such as silica, alumina, titania, zirconia, and calcium oxide; polymethylmethacrylate, polystyrene, polyurethane, acrylic resin, and acrylic-styrene copolymerization. Crosslinked or uncrosslinked organic particles, or polysiloxane particles, which are formed from various polymers such as acrylic-styrene resin, benzene melamine, melamine, and polycarbonate. One or two or more of the particles may be appropriately selected and used, but organic particles are preferred. From the viewpoint of refractive index, the organic particles are preferably acrylic resins and acrylic-styrene resins.
粒子之直徑可考慮硬化樹脂層之***突出度或與***以外之平坦區域之厚度之關係等而適當設定，並無特別限定。再者，由對透明導電性薄膜充分地賦與抗黏著性且充分地抑制霧度之上升之觀點而言，粒子之直徑宜為0.1~5μm、較佳為0.5~4μm。再者，於本說明書中，所謂「直徑」指表示粒子分布之極大值之粒徑，藉由使用流動式粒子像分析裝置(Sysmex公司製、製品名「FPTA-3000S」)於特定條件下(Sheath液：乙酸乙酯、測定模式：HPF測定、測定方式：總計數)進行測定而求得。測定試料使用將粒子以乙酸乙酯稀釋成1.0重量%，使用超音波洗淨機均勻地分散後之試料。The diameter of the particles can be appropriately set in consideration of the protrusion degree of the hardened resin layer or the relationship with the thickness of a flat area other than the protrusion, and is not particularly limited. In addition, from the viewpoint of sufficiently imparting anti-adhesion to the transparent conductive film and sufficiently suppressing the increase in haze, the diameter of the particles is preferably 0.1 to 5 μm, and more preferably 0.5 to 4 μm. In addition, in this specification, the "diameter" means a particle diameter indicating the maximum value of particle distribution, and a flow-type particle image analyzer (manufactured by Sysmex, product name "FPTA-3000S") is used under specific conditions ( Sheath solution: ethyl acetate, measurement mode: HPF measurement, measurement method: total count). For the measurement sample, the particles were diluted to 1.0% by weight with ethyl acetate and uniformly dispersed using an ultrasonic cleaner.
粒子之含量宜相對於樹脂組成物之固體成分100重量份為0.05~1.0重量份，較佳為0.1~0.5重量份，更佳為0.1~0.2重量份。若硬化樹脂層中之粒子之含量較少，有難以形成足以對硬化樹脂層之表面賦與抗黏著性及易滑性的***之傾向。另一方面，若粒子之含量過多，則有因為粒子所致之光散射而使透明導電性薄膜之霧度變高、視認性降低之傾向。又，若粒子之含量過多，有於形成硬化樹脂層時(溶液之塗佈時)產生線條、損及視認性或透明導電膜之電性特性變得不均一之情形。The content of the particles is preferably 0.05 to 1.0 parts by weight, preferably 0.1 to 0.5 parts by weight, and more preferably 0.1 to 0.2 parts by weight with respect to 100 parts by weight of the solid content of the resin composition. If the content of the particles in the hardened resin layer is small, it is difficult to form a swell sufficient to impart anti-adhesion and slipperiness to the surface of the hardened resin layer. On the other hand, when the content of the particles is too large, the haze of the transparent conductive film tends to increase due to light scattering by the particles, and the visibility tends to decrease. In addition, if the content of the particles is too large, lines may be formed during the formation of the hardened resin layer (at the time of application of the solution), the visibility or the electrical characteristics of the transparent conductive film may become uneven.
硬化樹脂層可藉由如下方式而獲得，即：將包含各硬化型樹脂與視需要添加之粒子、交聯劑、起啟劑、增感劑等之樹脂組成物塗佈於透明樹脂薄膜上，於樹脂組成物包含溶劑時，進行溶劑之乾燥，藉由應用熱、活性能量線或該兩者中之任一者使之硬化。熱可使用空氣循環式烘箱或IR加熱器等周知機構，但並不限定於此等方法。作為活性能量線之例，有紫外線、電子束、伽瑪射線等，但並無特別限定。The hardened resin layer can be obtained by coating a transparent resin film with a resin composition containing each hardening resin and particles, a cross-linking agent, a starter, a sensitizer, and the like added as needed, When the resin composition contains a solvent, the solvent is dried, and the resin composition is hardened by applying heat, active energy rays, or both. For the heat, a well-known mechanism such as an air circulation oven or an IR heater may be used, but it is not limited to these methods. Examples of active energy rays include ultraviolet rays, electron beams, and gamma rays, but they are not particularly limited.
硬化樹脂層可使用上述材料，藉由溼式塗佈法、凹版塗佈法或棒塗法等塗佈法、真空蒸鍍法、濺鍍法、離子鍍敷法等而形成。例如，形成含有氧化錫之氧化銦(ITO)作為透明導電膜時，若作為底層之硬化樹脂層之表面為平滑，亦可縮短透明導電膜之結晶化時間。由此觀點，硬化樹脂層宜藉由溼式塗佈法而製膜。The hardened resin layer can be formed using the above-mentioned materials by a coating method such as a wet coating method, a gravure coating method, or a bar coating method, a vacuum evaporation method, a sputtering method, an ion plating method, or the like. For example, when forming indium oxide (ITO) containing tin oxide as a transparent conductive film, if the surface of the hardened resin layer as the bottom layer is smooth, the crystallization time of the transparent conductive film can also be shortened. From this viewpoint, it is preferable that the hardened resin layer be formed into a film by a wet coating method.
硬化樹脂層之厚度宜為0.5μm~5μm、較佳為0.7μm~3μm、最佳為0.8μm~2μm。若硬化樹脂層之厚度為前述範圍，可防止受傷或防止硬化樹脂層之硬化收縮中之薄膜皺褶，可防止觸控面板等之視認性惡化。The thickness of the hardened resin layer is preferably 0.5 μm to 5 μm, preferably 0.7 μm to 3 μm, and most preferably 0.8 μm to 2 μm. If the thickness of the hardened resin layer is in the aforementioned range, it is possible to prevent injuries or to prevent film wrinkles during hardening shrinkage of the hardened resin layer, and to prevent deterioration of visibility of a touch panel or the like.
(光學調整層) 於第1硬化樹脂層與透明導電膜之間可進一步包含一層以上之光學調整層。再者，於未形成第1硬化樹脂層時，於透明樹脂薄膜與透明導電膜之間可包含一層以上之光學調整層。光學調整層是用於提升透明導電性薄膜之穿透率、或於將透明導電膜圖案化時可減低圖案殘留之圖案部與圖案不殘留之開口部之間的穿透率差及反射率差，可獲得視認性優異之透明導電性薄膜。(Optical adjustment layer) Between the first hardened resin layer and the transparent conductive film, one or more optical adjustment layers may be further included. When the first cured resin layer is not formed, one or more optical adjustment layers may be included between the transparent resin film and the transparent conductive film. The optical adjustment layer is used to improve the transmittance of a transparent conductive film or to reduce the difference in transmittance and reflectance between a pattern portion where a pattern remains and an opening portion where a pattern does not remain when the transparent conductive film is patterned. A transparent conductive film with excellent visibility can be obtained.
光學調整層宜包含黏合劑樹脂與微粒子。作為光學調整層所包含之黏合劑樹脂，可列舉：丙烯酸系樹脂、胺甲酸乙酯系樹脂、三聚氰胺系樹脂、醇酸系樹脂、矽氧烷系聚合物、有機矽烷縮合物等，以包含丙烯酸系樹脂之紫外線硬化型樹脂為佳。The optical adjustment layer should preferably contain a binder resin and fine particles. Examples of the binder resin included in the optical adjustment layer include acrylic resins, urethane resins, melamine resins, alkyd resins, siloxane polymers, and organic silane condensation products. The resin is preferably an ultraviolet curing resin.
光學調整層之折射率宜為1.6~1.8、較佳為1.61~1.78、更佳為1.62~1.75。藉此，可減低穿透率差及反射率差，可獲得視認性優異之透明導電性薄膜。The refractive index of the optical adjustment layer is preferably 1.6 to 1.8, preferably 1.61 to 1.78, and more preferably 1.62 to 1.75. Thereby, the difference in transmittance and the difference in reflectance can be reduced, and a transparent conductive film having excellent visibility can be obtained.
光學調整層亦可具有平均粒徑為1nm~500nm之微粒子。光學調整層中之微粒子之含量宜為0.1重量%~90重量%。用於光學調整層之微粒子之平均粒徑，如上所述宜為1nm~500nm之範圍、較佳為5nm~300nm。又，光學調整層中之微粒子之含量較佳為10重量%~80重量%、更佳為20重量%~70重量%。藉由於光學調整層中含有微粒子，可容易進行光學調整層本身之折射率調整。The optical adjustment layer may have fine particles having an average particle diameter of 1 to 500 nm. The content of the fine particles in the optical adjustment layer is preferably 0.1% by weight to 90% by weight. As mentioned above, the average particle diameter of the fine particles used in the optical adjustment layer is preferably in the range of 1 nm to 500 nm, and more preferably 5 nm to 300 nm. The content of the fine particles in the optical adjustment layer is preferably 10% by weight to 80% by weight, and more preferably 20% by weight to 70% by weight. Since the optical adjustment layer contains fine particles, the refractive index adjustment of the optical adjustment layer itself can be easily performed.
作為形成微粒子之無機氧化物，例如可列舉：氧化矽(二氧化矽)、中空奈米二氧化矽、氧化鈦、氧化鋁、氧化鋅、氧化錫、氧化鋯、氧化鈮等微粒子。此等中，以氧化矽(二氧化矽)、氧化鈦、氧化鋁、氧化鋅、氧化錫、氧化鋯、氧化鈮之微粒子為佳，氧化鋯為較佳。此等可單獨使用一種，亦可併用二種以上。Examples of the inorganic oxide that forms fine particles include fine particles such as silicon oxide (silicon dioxide), hollow nanometer silica, titanium oxide, aluminum oxide, zinc oxide, tin oxide, zirconia, and niobium oxide. Among these, fine particles of silicon oxide (silicon dioxide), titanium oxide, aluminum oxide, zinc oxide, tin oxide, zirconia, and niobium oxide are preferable, and zirconia is more preferable. These may be used alone or in combination of two or more.
光學調整層可含有其他無機物。作為無機物可列舉：NaF(1.3)、Na3 AlF6 (1.35)、LiF(1.36)、MgF2 (1.38)、CaF2 (1.4)、BaF2 (1.3)、BaF2 (1.3)、LaF3 (1.55)、CeF(1.63)等(括弧內之數值表示折射率)。The optical adjustment layer may contain other inorganic substances. Examples of the inorganic substance include NaF (1.3), Na 3 AlF 6 (1.35), LiF (1.36), MgF 2 (1.38), CaF 2 (1.4), BaF 2 (1.3), BaF 2 (1.3), LaF 3 ( 1.55), CeF (1.63), etc. (the values in parentheses indicate the refractive index).
光學調整層可使用上述材料，藉由溼式塗佈法、凹版塗佈法或棒塗法等塗佈法、真空蒸鍍法、濺鍍法、離子鍍敷法等而形成。例如，形成含有氧化錫之氧化銦(ITO)作為透明導電膜時，若作為底層之光學調整層之表面為平滑，亦可縮短透明導電層之結晶化時間。由此觀點，光學調整層宜藉由溼式塗佈法而製膜。The optical adjustment layer can be formed by using the above-mentioned materials by a coating method such as a wet coating method, a gravure coating method, or a bar coating method, a vacuum evaporation method, a sputtering method, an ion plating method, or the like. For example, when forming indium oxide (ITO) containing tin oxide as a transparent conductive film, if the surface of the optical adjustment layer as a bottom layer is smooth, the crystallization time of the transparent conductive layer can also be shortened. From this viewpoint, it is preferable that the optical adjustment layer is formed by a wet coating method.
光學調整層之厚度宜為40nm~150nm、較佳為50nm~130nm、更佳為70nm~120nm。若光學調整層之厚度過小，難以成為連續被膜。又，若光學調整層之厚度過大，則有透明導電性薄膜之透明性降低或容易產生裂紋之傾向。The thickness of the optical adjustment layer is preferably 40 nm to 150 nm, preferably 50 nm to 130 nm, and more preferably 70 nm to 120 nm. If the thickness of the optical adjustment layer is too small, it becomes difficult to form a continuous film. When the thickness of the optical adjustment layer is too large, the transparency of the transparent conductive film tends to decrease or cracks tend to occur.
(透明導電膜) 透明導電膜亦可設置於透明樹脂薄膜上，但較佳為設置於透明樹脂薄膜之一面側所設置之第1硬化樹脂層上或光學調整層上。透明導電膜之構成材料只要包含無機物即可，並無特別限定，可適當地使用選自由銦、錫、鋅、鎵、銻、鈦、矽、鋯、鎂、鋁、金、銀、銅、鈀、鎢所組成之群中之至少一種金屬之金屬氧化物。於該金屬氧化物中，亦可視需要進一步包含上述群所示之金屬原子。例如宜使用銦錫複合氧化物(ITO)、含有銻之氧化錫(ATO)等。(Transparent conductive film) The transparent conductive film may be provided on the transparent resin film, but it is preferably provided on the first hardened resin layer or the optical adjustment layer provided on one side of the transparent resin film. The constituent material of the transparent conductive film is not particularly limited as long as it contains an inorganic substance, and may be appropriately selected from the group consisting of indium, tin, zinc, gallium, antimony, titanium, silicon, zirconium, magnesium, aluminum, gold, silver, copper, and palladium. A metal oxide of at least one metal in the group consisting of tungsten. The metal oxide may further include a metal atom represented by the above group as necessary. For example, indium tin composite oxide (ITO), antimony-containing tin oxide (ATO), and the like are preferably used.
透明導電膜之厚度並無特別限制，但為了形成其表面電阻為1×103 Ω/□以下之具有良好導電性之連續被膜，宜將厚度設為10nm以上。膜厚若過厚由於會造成透明性降低等，故宜為15~35nm、較佳為20~30nm之範圍內。若透明導電膜之厚度未達10nm，則膜表面之電阻變高且難以形成連續被膜。又，若透明導電膜之厚度超過35nm，則有造成透明性降低等情形。The thickness of the transparent conductive film is not particularly limited, but in order to form a continuous conductive film having a good surface conductivity of 1 × 10 3 Ω / □ or less, the thickness should be set to 10 nm or more. If the film thickness is too thick, it may cause a decrease in transparency, etc., so it is preferably within a range of 15 to 35 nm, and more preferably 20 to 30 nm. If the thickness of the transparent conductive film is less than 10 nm, the resistance on the surface of the film becomes high and it is difficult to form a continuous film. In addition, if the thickness of the transparent conductive film exceeds 35 nm, the transparency may be reduced.
透明導電膜之形成方法並無特別限定，可採用先前周知之方法。具體而言，例如可例示真空蒸鍍法、濺鍍法、離子鍍敷法等乾式製程。又，亦可根據需要之膜厚採用適當的方法。The method for forming the transparent conductive film is not particularly limited, and a conventionally known method can be adopted. Specifically, for example, a dry process such as a vacuum deposition method, a sputtering method, or an ion plating method can be exemplified. Further, an appropriate method may be adopted according to the required film thickness.
透明導電膜可視需要實施加熱退火處理(例如大氣環境下於80~150℃進行10~90分鐘左右)而結晶化。藉由使透明導電膜結晶化，除了將透明導電膜低電阻化外，亦提高透明性及耐久性。使非晶質之透明導電膜轉換為結晶質之方法並無特別限定，可使用空氣循環式烘箱或IR加熱器等。The transparent conductive film may be heat-annealed (for example, at a temperature of 80 to 150 ° C. for about 10 to 90 minutes) and crystallized if necessary. By crystallizing the transparent conductive film, in addition to reducing the resistance of the transparent conductive film, transparency and durability are also improved. The method for converting an amorphous transparent conductive film into a crystalline material is not particularly limited, and an air circulating oven or an IR heater can be used.
關於「結晶質」之定義，是將於透明樹脂薄膜上形成有透明導電膜之透明導電性薄膜於20℃、濃度5重量%之鹽酸中浸漬15分鐘後，水洗及乾燥，以測量儀對15mm間之端子間電阻進行測定，當端子間電阻不超過10kΩ時，表示ITO膜朝結晶質之轉換完成。再者，表面電阻值之測定可依據JIS K7194藉由四端子法而測定。The definition of "crystalline" is that a transparent conductive film formed with a transparent conductive film on a transparent resin film is immersed in hydrochloric acid at 20 ° C and a concentration of 5% by weight for 15 minutes, and then washed and dried with a measuring instrument for 15mm The resistance between the terminals is measured. When the resistance between the terminals does not exceed 10kΩ, it means that the conversion of the ITO film to the crystalline is complete. The surface resistance value can be measured by a four-terminal method in accordance with JIS K7194.
又，透明導電膜亦可藉由蝕刻等而圖案化。關於透明導電膜之圖案化，可使用先前周知之光微影法之技術進行。作為蝕刻液，宜使用酸。作為酸，例如可列舉：氯化氫、溴化氫、硫酸、硝酸、磷酸等無機酸、醋酸等有機酸及此等之混合物、以及其等之水溶液。例如於靜電容方式之觸控面板或矩陣式之電阻膜方式之觸控面板所使用之透明導電性薄膜中，宜將透明導電膜圖案化成條紋狀。再者，藉由蝕刻將透明導電膜圖案化時，若先進行透明導電膜之結晶化，則有難以藉由蝕刻進行圖案化之情形。因此，透明導電膜之退火處理宜於將透明導電膜圖案化之後進行。The transparent conductive film may be patterned by etching or the like. The patterning of the transparent conductive film can be performed by a technique known in the prior art, the photolithography method. As the etching solution, an acid is preferably used. Examples of the acid include inorganic acids such as hydrogen chloride, hydrogen bromide, sulfuric acid, nitric acid, and phosphoric acid; organic acids such as acetic acid; mixtures thereof; and aqueous solutions thereof. For example, in a transparent conductive film used in a capacitive touch panel or a matrix resistive touch panel, the transparent conductive film should be patterned into stripes. Furthermore, when the transparent conductive film is patterned by etching, if the transparent conductive film is crystallized first, it may be difficult to perform patterning by etching. Therefore, the annealing treatment of the transparent conductive film is preferably performed after patterning the transparent conductive film.
＜載體薄膜＞ 載體薄膜包含配置於透明導電性薄膜之形成有前述透明樹脂薄膜之面側之黏著劑層與保護薄膜，將透明導電性薄膜與載體薄膜貼合，形成附載體薄膜之透明導電性薄膜。將載體薄膜自附載體薄膜之透明導電性薄膜剝離時，黏著劑層可與保護薄膜一同剝離，亦可僅剝離保護薄膜。<Carrier film> The carrier film includes an adhesive layer and a protective film disposed on the transparent conductive film on which the transparent resin film is formed, and the transparent conductive film and the carrier film are laminated to form a transparent conductive film with a carrier film. film. When the carrier film is peeled from the transparent conductive film with the carrier film, the adhesive layer may be peeled together with the protective film, or only the protective film may be peeled.
(保護薄膜) 保護薄膜在與波長板或偏光板等其他薄膜積層時被剝離而廢棄，但考量利用輥進行捲取等之處理性、含水量等，作為形成保護薄膜之材料，例如可列舉與前述透明樹脂薄膜之材料相同者。由視認性變得良好之方面來看，較佳為聚酯系樹脂、環烯烴系樹脂、聚碳酸酯系樹脂，但由高透明性、低吸水性、水分阻斷性、熱穩定性、等方性等觀點來看，尤佳為非晶性樹脂之環烯烴系樹脂或聚碳酸酯系樹脂。聚酯系樹脂、環烯烴系樹脂及聚碳酸酯系樹脂之具體例，如同前述透明樹脂薄膜所記載，但考量水分率自其中進行選擇。藉此，由於可使用含水率較低之保護薄膜，可進一步控制保護薄膜之含水量，充分進行透明導電膜之結晶化，故可更確實地防止透明導電性薄膜之電阻值異常，且更提高透明導電膜與基材之密接性，防止膜剝離。(Protective film) Protective film is peeled off and discarded when laminated with other films such as wavelength plate or polarizing plate. However, considering the rationality and moisture content of the film, such as winding with a roller, examples of materials for forming protective films include The materials of the transparent resin film are the same. From the standpoint of good visibility, polyester resins, cycloolefin resins, and polycarbonate resins are preferred, but from high transparency, low water absorption, moisture blocking properties, thermal stability, etc. From the viewpoints of squareness and the like, a cycloolefin-based resin or a polycarbonate-based resin of an amorphous resin is particularly preferred. Specific examples of the polyester-based resin, the cycloolefin-based resin, and the polycarbonate-based resin are as described in the above-mentioned transparent resin film, but the moisture content is selected from them. As a result, a protective film with a lower moisture content can be used, the moisture content of the protective film can be further controlled, and the crystallization of the transparent conductive film can be fully performed, so that the abnormal resistance value of the transparent conductive film can be prevented more reliably and improved The adhesion between the transparent conductive film and the substrate prevents the film from peeling.
保護薄膜亦可與透明樹脂薄膜相同，對表面預先實施濺鍍、電暈放電、噴火、紫外線照射、電子束照射、化學變化、氧化等蝕刻處理或底層塗佈處理，使與保護薄膜上之黏著劑層等之密接性提高。又，於形成黏著劑層之前，亦可視需要藉由溶劑洗淨或超音波洗淨等將保護薄膜表面除塵、清淨化。The protective film may be the same as the transparent resin film, and the surface is previously subjected to an etching treatment such as sputtering, corona discharge, fire spray, ultraviolet irradiation, electron beam irradiation, chemical change, oxidation, or an undercoating treatment, so as to adhere to the protective film. Adhesiveness of the agent layer is improved. In addition, before the formation of the adhesive layer, the surface of the protective film may be dust-removed and cleaned by solvent cleaning or ultrasonic cleaning, if necessary.
保護薄膜之含水量宜每10mm×10mm為1.0×10-3 g以下、較佳每10mm×10mm為0.9×10-3 g以下、更佳每10mm×10mm為0.5×10-3 g以下。再者，於此之水分量由於實測值隨著環境而變動，故宜於提供給濺鍍製膜或結晶化步驟之時點滿足前述範圍。藉此，可防止透明導電性薄膜之電阻值異常，且提高透明導電膜與基材之密接性，防止膜剝離。又，藉此由於不需要為去除水分而作為前處理之通過加熱步驟等之成膜前之除氣處理，故生產效率提高。The moisture content of the protective film should be 1.0 × 10 -3 g or less per 10mm × 10mm, preferably 0.9 × 10 -3 g or less per 10mm × 10mm, and more preferably 0.5 × 10 -3 g or less per 10mm × 10mm. Furthermore, since the amount of water measured here varies with the environment, it is suitable to satisfy the aforementioned range at the time when it is supplied to the sputtering film formation or crystallization step. Thereby, abnormal resistance value of the transparent conductive film can be prevented, the adhesion between the transparent conductive film and the substrate can be improved, and the film can be prevented from peeling off. In addition, this eliminates the need for a degassing treatment before film formation by a heating step or the like as a pretreatment to remove moisture, thereby improving production efficiency.
保護薄膜之水分率(含水率)宜為0.50重量%以下、較佳為0.40重量%以下、更佳為0.30重量%以下。藉此，由於可使用含水率較低之保護薄膜，可進一步控制保護薄膜之含水量，充分進行透明導電膜之結晶化，故可更確實地防止透明導電性薄膜之電阻值異常，且更提高透明導電膜與基材之密接性，防止膜剝離。The moisture content (water content) of the protective film is preferably 0.50% by weight or less, preferably 0.40% by weight or less, and more preferably 0.30% by weight or less. As a result, a protective film with a lower moisture content can be used, the moisture content of the protective film can be further controlled, and the crystallization of the transparent conductive film can be fully performed, so that the abnormal resistance value of the transparent conductive film can be prevented more reliably and improved The adhesion between the transparent conductive film and the substrate prevents the film from peeling.
保護薄膜之厚度宜為1~150μm、較佳為2~120μm、更佳為5~100μm。由於保護薄膜之厚度越薄，越可進而抑制保護薄膜之含水量，充分進行透明導電膜之結晶化，故可更確實地防止透明導電性薄膜之電阻值異常，且可更提高透明導電膜與基材之密接性，防止膜剝離。藉由設為前述範圍，可提高捲對捲製法之易搬送性。又，自於捲對捲製法中防止透明導電性薄膜積層體之破裂之觀點來看，保護薄膜之厚度宜為透明樹脂薄膜之厚度以上。The thickness of the protective film is preferably 1 to 150 μm, preferably 2 to 120 μm, and more preferably 5 to 100 μm. As the thickness of the protective film is thinner, the moisture content of the protective film can be further suppressed, and the transparent conductive film can be fully crystallized, so that the abnormal resistance value of the transparent conductive film can be prevented more reliably, and the transparent conductive film and the The adhesiveness of the substrate prevents the film from peeling. By setting it as the said range, the easy conveyance property of a roll-to-roll method can be improved. In addition, from the viewpoint of preventing cracking of the transparent conductive film laminate in the roll-to-roll method, the thickness of the protective film is preferably equal to or greater than the thickness of the transparent resin film.
(導電層) 由抗靜電之觀點而言，宜於前述保護薄膜之與形成有前述黏著劑層之面相反之面側進而具備導電層。導電層較佳可藉由塗佈包含導電性聚合物之導電性組成物而形成。(Conductive layer) From the viewpoint of antistatic, it is preferable to further include a conductive layer on the side of the protective film opposite to the surface on which the adhesive layer is formed. The conductive layer is preferably formed by coating a conductive composition containing a conductive polymer.
作為上述導電性組成物所包含之導電性聚合物，例如可列舉：經以聚乙炔系聚合物、聚對伸苯系聚合物、聚苯胺系聚合物、聚噻吩系聚合物、聚對伸苯伸乙烯基系聚合物、聚吡咯系聚合物、聚伸苯系聚合物、丙烯酸系聚合物改質後之聚酯系聚合物等。較佳為導電性聚合物包含選自由聚乙炔系聚合物、聚對伸苯系聚合物、聚苯胺系聚合物、聚噻吩系聚合物、聚對伸苯伸乙烯基系聚合物及聚吡咯系聚合物所組成之群中之一種以上聚合物。Examples of the conductive polymer included in the conductive composition include a polyacetylene-based polymer, a poly-p-phenylene-based polymer, a polyaniline-based polymer, a polythiophene-based polymer, and a poly-p-phenylene. Polyvinyl polymer, polypyrrole polymer, polystyrene polymer, polyester polymer modified acrylic polymer, etc. Preferably, the conductive polymer includes a polymer selected from the group consisting of a polyacetylene polymer, a polyparaphenylene polymer, a polyaniline polymer, a polythiophene polymer, a polyparaphenylene vinyl polymer, and a polypyrrole polymer. One or more polymers in a group of polymers.
更佳為使用聚噻吩系聚合物作為上述導電性聚合物。若使用聚噻吩系聚合物，可形成透明性及化學穩定性優異之導電層。作為聚噻吩系聚合物之具體例，可列舉：聚噻吩；聚(3-己基噻吩)等聚(3-C1-8 烷基-噻吩)；聚(3,4-乙二氧基噻吩)(PEDOT)、聚(3,4-丙二氧基噻吩)、聚[3,4-(1,2-環己烯)二氧基噻吩]等聚(3,4-(環)伸烷基二氧基噻吩)；聚噻吩乙烯等。More preferably, a polythiophene-based polymer is used as the conductive polymer. When a polythiophene polymer is used, a conductive layer having excellent transparency and chemical stability can be formed. Specific examples of the polythiophene-based polymer include polythiophene; poly (3-C 1-8 alkyl-thiophene) such as poly (3-hexylthiophene); and poly (3,4-ethylenedioxythiophene). (PEDOT), poly (3,4-propanedioxythiophene), poly [3,4- (1,2-cyclohexene) dioxythiophene], and other poly (3,4- (cyclo) alkylene Dioxythiophene); polythiophene ethylene and the like.
上述導電層可藉由任意之適當的方法而形成。導電性組成物例如為包含上述導電性聚合物與任意之適當的溶劑(例如水)，且於該溶劑中分散有該導電性聚合物之分散液。該分散液中之導電性聚合物之分散濃度宜為0.01重量%~50重量%、較佳為0.01重量%~30重量%。The conductive layer can be formed by any appropriate method. The conductive composition is, for example, a dispersion liquid containing the above-mentioned conductive polymer and any appropriate solvent (for example, water), and the conductive polymer is dispersed in the solvent. The dispersion concentration of the conductive polymer in the dispersion is preferably 0.01% by weight to 50% by weight, and more preferably 0.01% by weight to 30% by weight.
作為上述導電性組成物之塗佈方法，可採用任意之適當的方法。例如可列舉：棒塗法、輥塗法、凹版塗佈法、桿塗法、狹縫噴嘴式塗佈法、簾塗法、噴注式刮刀塗佈法、逗點式塗佈法。作為乾燥溫度，代表性為50℃以上、較佳為90℃以上、更佳為110℃以上。乾燥溫度較佳為200℃以下、更佳為180℃以下。乾燥時間較佳為1分鐘~1小時、更佳為1分鐘~30分鐘、最佳為1分鐘~10分鐘。As a method for applying the conductive composition, any appropriate method can be adopted. Examples thereof include a bar coating method, a roll coating method, a gravure coating method, a rod coating method, a slit nozzle coating method, a curtain coating method, a spray blade coating method, and a comma coating method. The drying temperature is typically 50 ° C or higher, preferably 90 ° C or higher, and more preferably 110 ° C or higher. The drying temperature is preferably 200 ° C or lower, and more preferably 180 ° C or lower. The drying time is preferably 1 minute to 1 hour, more preferably 1 minute to 30 minutes, and most preferably 1 minute to 10 minutes.
上述導電層之厚度較佳為1nm~500nm、更佳為1nm~400nm、最佳為1nm~300nm。若為此種範圍，可良好地形成能控制電性特性之導電層。The thickness of the conductive layer is preferably 1 nm to 500 nm, more preferably 1 nm to 400 nm, and most preferably 1 nm to 300 nm. Within this range, a conductive layer capable of controlling electrical characteristics can be formed satisfactorily.
上述導電性組成物可視需要進一步包含任意之適當的添加劑。作為添加劑之具體例，可列舉：分散穩定劑、界面活性劑、消泡劑等。所使用之添加劑之種類及量可視目的而適當設定。The above-mentioned conductive composition may further contain any appropriate additive, if necessary. Specific examples of the additives include a dispersion stabilizer, a surfactant, and an antifoaming agent. The type and amount of the additives used can be appropriately set depending on the purpose.
(黏著劑層) 作為黏著劑層，只要具有透明性者即可，可無特別限制地使用。具體而言，例如可適當地選擇使用以丙烯酸系聚合物、聚矽氧系聚合物、聚酯、聚胺甲酸乙酯、聚醯胺、聚乙烯醚、乙酸乙烯酯/氯乙烯共聚物、改質聚烯烴、環氧系、氟系、天然橡膠、合成橡膠等橡膠系等之聚合物作為基礎聚合物者。特別是由光學透明性優異、表現適度的潤溼性、凝集性及接著性等黏著特性，耐候性及耐熱性等亦優異之方面而言，宜使用丙烯酸系黏著劑。(Adhesive layer) As the adhesive layer, any material having transparency is used, and it can be used without particular limitation. Specifically, for example, acrylic polymers, silicone polymers, polyesters, polyurethanes, polyamides, polyvinyl ethers, vinyl acetate / vinyl chloride copolymers, modified polymers Polyolefin, epoxy-based, fluorine-based, natural rubber, synthetic rubber and other rubber-based polymers are used as the base polymer. In particular, acrylic adhesives are suitable in terms of excellent optical transparency, moderate adhesion properties such as wettability, cohesiveness, and adhesiveness, as well as excellent weather resistance and heat resistance.
黏著劑層之形成方法並無特別限制，可列舉於剝離片塗佈黏著劑組成物，使之乾燥後，轉印於基材薄膜之方法(轉印法)、於保護薄膜直接塗佈、乾燥黏著劑組成物之方法(直接印刷法)或藉由共擠出之方法等。再者，於黏著劑中亦可視需要適當地使用黏著賦與劑、塑化劑、填充劑、抗氧化劑、紫外線吸收劑、矽烷偶合劑等。The method for forming the adhesive layer is not particularly limited, and examples thereof include a method of applying an adhesive composition to a release sheet, drying it, and then transferring it to a substrate film (transfer method), directly coating and drying the protective film. A method of the adhesive composition (direct printing method) or a method of coextrusion. In addition, an adhesive agent, a plasticizer, a filler, an antioxidant, an ultraviolet absorber, a silane coupling agent, and the like may be appropriately used in the adhesive as needed.
黏著劑層之較佳厚度為5μm~100μm、更佳為10μm~50μm、最佳為15μm~35μm。The thickness of the adhesive layer is preferably 5 μm to 100 μm, more preferably 10 μm to 50 μm, and most preferably 15 μm to 35 μm.
＜觸控面板＞ 自附載體薄膜之透明導電性薄膜剝離載體薄膜或保護薄膜後之透明導電性薄膜，例如可適合應用作為靜電容方式、電阻膜方式等之觸控面板等電子機器之透明電極。<Touch panel> 透明 Transparent conductive film with a carrier film. The transparent conductive film after peeling off the carrier film or protective film. For example, it can be used as a transparent electrode for electronic devices such as touch panels such as electrostatic capacitance method and resistive film method. .
於形成觸控面板時，可於前述透明導電性薄膜之一個或二個主面經由透明之黏著劑層貼合玻璃或高分子薄膜等其他基材等。例如，亦可形成如下積層體，即於透明導電性薄膜之未形成有透明導電膜之側之面經由透明的黏著劑層貼合透明基體而成者。透明基體可由一片基體薄膜構成，亦可為二片以上基體薄膜之積層體(例如經由透明的黏著劑層而積層者)。又，亦可於貼合在透明導電性薄膜之透明基體之外表面設置硬塗層。作為用於貼合透明導電性薄膜與基材之黏著劑層，如前所述，只要為具有透明性者，即可無特別限制地使用。When forming a touch panel, one or two main surfaces of the transparent conductive film may be bonded with other substrates such as glass or polymer film through a transparent adhesive layer. For example, a laminated body may be formed in which a transparent substrate is bonded to a surface of a transparent conductive film on which a transparent conductive film is not formed through a transparent adhesive layer. The transparent substrate may be composed of one substrate film, or may be a laminated body of two or more substrate films (for example, those laminated through a transparent adhesive layer). In addition, a hard coat layer may be provided on the outer surface of the transparent substrate bonded to the transparent conductive film. As the adhesive layer for bonding a transparent conductive film and a substrate, as described above, as long as it has transparency, it can be used without particular limitation.
[實施例] 以下使用實施例詳細地說明本發明，但本發明在不超過其要旨之範圍內，並不限定於以下實施例。[Examples] The following describes the present invention in detail using examples, but the present invention is not limited to the following examples within a range not exceeding the gist thereof.
＜評價＞ (1)厚度之測定 厚度，關於具有1μm以上之厚度者使用測微式厚度計(Mitutoyo公司製)進行測定。又，未達1μm之厚度以瞬間多重測光系統(大塚電子公司製 MCPD2000)進行測定。如ITO膜等厚度般之奈米尺寸之厚度以FB-2000A(日立高科技股份有限公司製)製作剖面觀察用樣品，剖面TEM觀察使用HF-2000(日立高科技股份有限公司製)測定膜厚。將評價結果顯示於表1。<Evaluation> (1) Measurement of thickness Thickness is measured using a micrometer type thickness meter (manufactured by Mitutoyo) for those having a thickness of 1 μm or more. The thickness of less than 1 m was measured with an instantaneous multiple photometry system (MCPD2000 manufactured by Otsuka Electronics Co., Ltd.). Nanometer-sized thicknesses such as the thickness of ITO films are made using FB-2000A (manufactured by Hitachi High-tech Co., Ltd.) for section observation samples, and section TEM observation is performed using HF-2000 (manufactured by Hitachi High-Tech Co., Ltd.) . The evaluation results are shown in Table 1.
(2)含水量及水分率(含水率)之測定 將保護薄膜切成10mm×10mm□之樣品，放入加熱氣化裝置(三菱化學Analytech，VA-200型)，將經以150℃加熱之載體氣體導入至滴定單元內(三菱化學Analytech，CA-200型)，藉由卡耳-費雪法(氣化法)測定加熱中之水分釋放量，測定含水量及水分率。再者，所謂水分率為每1g之水分量，可與含水量同樣地算出。關於透明樹脂薄膜亦以與前述同樣方法測定含水量及水分率。將評價結果顯示於表1。(2) Measurement of water content and moisture content (water content) The protective film is cut into a sample of 10mm × 10mm □, and placed in a heating and gasification device (Mitsubishi Chemical Analytech, VA-200 model). The carrier gas was introduced into a titration unit (Analytech, CA-200), and the amount of water released during heating was measured by the Carr-Fisher method (gasification method), and the water content and water content were measured. The water content per 1 g can be calculated in the same manner as the water content. Regarding the transparent resin film, the water content and the water content were also measured in the same manner as described above. The evaluation results are shown in Table 1.
(3)到達電阻值之測定 將附載體薄膜之透明導電性薄膜藉由熱風循環式烘箱以120℃實施20、30、40分鐘加熱處理，測定其到達電阻值。表面電阻依據JIS K7194藉由四端子法進行測定。將評價結果顯示於表1。(3) Measurement of arrival resistance value The transparent conductive film with a carrier film was subjected to heat treatment at 120 ° C for 20, 30, and 40 minutes in a hot air circulation oven to measure the arrival resistance value. The surface resistance was measured by the four-terminal method in accordance with JIS K7194. The evaluation results are shown in Table 1.
(4)表面電阻值之標準偏差 將於前述到達電阻值之測定中以120℃實施30分鐘加熱處理時之附載體薄膜之透明導電性薄膜，於寬度方向以間隔15cm測定五處之表面電阻值，求得其標準偏差。將評價結果顯示於表1。(4) The standard deviation of the surface resistance value will be the transparent conductive film with a carrier film when it is subjected to heat treatment at 120 ° C for 30 minutes in the aforementioned measurement of the reached resistance value, and the surface resistance value is measured at a distance of 15 cm in the width direction. And find its standard deviation. The evaluation results are shown in Table 1.
(5)結晶化速度 非晶質之透明導電膜結晶化之結晶化速度，藉由前述到達電阻值之變化而進行評價。又，此處將無保護薄膜之透明導電性薄膜(參考例1)設為結晶化速度之基準值。將評價結果顯示於表1。(5) Crystallization rate: The crystallization rate of the amorphous transparent conductive film is evaluated based on the aforementioned change in the resistance value. Here, a transparent conductive film (Reference Example 1) without a protective film is used as a reference value for the crystallization rate. The evaluation results are shown in Table 1.
○：結晶化速度與基準值相同程度 ×：結晶化速度比基準值慢○: The crystallization rate is about the same as the reference value ×: The crystallization rate is slower than the reference value
(6)密接性 依據JIS K-5600進行測定。將附載體薄膜之透明導電性薄膜藉由熱風循環式烘箱以130℃實施90分鐘加熱處理後，將樣品切成5cm見方，將透明導電膜(ITO)面藉由切割器以間隔約1mm劃出縱橫各11條傷痕，製作100格。於其上黏貼透明膠帶(積水公司製、#252)，以刮勺反覆加壓10次後，附加扣環急速地剝離膠帶，計算1格之1/4以上之面積被剝離之情形，確認透明導電膜有無剝離。再者，改變刮勺加壓及剝離方向，反覆進行二次，第二次的加壓將透明膠帶旋轉90°進行。將評價結果顯示於表1。(6) Adhesiveness Measured in accordance with JIS K-5600. The transparent conductive film with a carrier film was heat-treated in a hot air circulation oven at 130 ° C for 90 minutes, and then the sample was cut into 5 cm squares, and the transparent conductive film (ITO) surface was cut by a cutter at an interval of about 1 mm. There are 11 scars on the vertical and horizontal sides, making 100 grids. Scotch tape (# 252, manufactured by Sekisui Co., Ltd.) was affixed thereon, and after repeatedly pressing with a spatula for 10 times, the buckle was quickly peeled off with an additional buckle, and a quarter or more of one square was peeled off to confirm transparency. Whether the conductive film is peeled off. Furthermore, the direction of pressure and peeling of the spatula was changed, and it was repeated twice, and the second pressure was performed by rotating the transparent tape by 90 °. The evaluation results are shown in Table 1.
○：無剝離(5/100以下)、密接性良好 ×：有剝離(比5/100大)、密接性差○: No peeling (less than 5/100), good adhesion ×: With peeling (larger than 5/100), poor adhesion
[實施例1] (硬化樹脂層之形成) 將包含100重量份之紫外線硬化性樹脂組成物(DIC公司製 商品名「UNIDIC(註冊商標)RS29-120」、胺甲酸乙酯系多官能聚丙烯酸酯)及0.2重量份之直徑為3μm之交聯丙烯酸-苯乙烯系球狀粒子(積水樹脂公司製「SSX105」)的放入球狀粒子之硬化性樹脂組成物塗佈於厚度50μm之聚環烯烴薄膜(日本ZEON製 商品名「ZEONOR(註冊商標)、面內雙折射率0.0001」)之一面，自其表面照射紫外線，形成厚度1μm之第2硬化樹脂層。除了不包含球狀粒子外，於聚環烯烴薄膜之另一面藉由與上述相同方法，以厚度成為1μm之方式形成第1硬化樹脂層。[Example 1] (Formation of hardened resin layer) 100 parts by weight of an ultraviolet curable resin composition (trade name "UNIDIC (registered trademark) RS29-120" manufactured by DIC Corporation), a urethane-based polyfunctional polyacrylic acid Ester) and 0.2 parts by weight of crosslinked acrylic-styrene spherical particles ("SSX105" manufactured by Sekisui Resin Co., Ltd.) having a diameter of 3 μm, and a spherical resin-containing curable resin composition was applied to a 50 μm thick polycyclic ring One side of an olefin film (trade name "ZEONOR (registered trademark) manufactured by ZEON Japan, in-plane birefringence 0.0001") was irradiated with ultraviolet rays from its surface to form a second hardened resin layer having a thickness of 1 μm. The first hardened resin layer was formed on the other side of the polycycloolefin film so as to have a thickness of 1 μm by the same method except that spherical particles were not included.
(光學調整層之形成) 於兩面形成有硬化樹脂層之聚環烯烴薄膜之第1硬化樹脂層面側塗佈作為光學調整層之折射率1.62之含有氧化鋯粒子之紫外線硬化型組成物(JSR公司製、商品名「OPSTAR-Z7412」)，形成塗佈層。接著，以80℃乾燥3分鐘後，立即自形成有塗佈層之側以臭氧形式高壓水銀燈(80W/cm、15cm聚光型：累積光量300mj)對塗佈層照射紫外線，以厚度成為0.1μm之方式形成光學調整層。(Formation of optical adjustment layer) A UV-curable composition containing zirconia particles having a refractive index of 1.62 as an optical adjustment layer was applied to the first cured resin layer side of a polycycloolefin film having cured resin layers formed on both sides (JSR Corporation) (Product name, "OPSTAR-Z7412") to form a coating layer. Next, after drying at 80 ° C for 3 minutes, immediately from the side where the coating layer was formed, a high-pressure mercury lamp (80W / cm, 15cm light-condensing type: cumulative light amount 300mj) was irradiated with ultraviolet rays to the coating layer to a thickness of 0.1 μm. In this way, an optical adjustment layer is formed.
(透明導電膜之形成) 於平行平板型之捲取式磁控濺鍍裝置安裝以90：10之重量比含有氧化銦與氧化錫之燒結體靶材，一面搬送基材，一面藉由真空排氣，以水之分壓成為5×10-4 Pa為止進行真空排氣。之後，調整氬氣及氧氣之導入量，一面以搬送速度7.7m/分鐘、搬送張力40~120N搬送基材，一面以輸出12.5kW藉由DC濺鍍對光學調整層面(第1硬化樹脂層)進行成膜，形成厚度22nm之ITO膜。藉由四端子法測定所獲得之ITO之表面電阻，結果為300Ω/□。(Formation of transparent conductive film) Installed in a parallel flat-type reel-type magnetron sputtering device containing a sintered body target containing indium oxide and tin oxide in a weight ratio of 90:10, while the substrate is being transported and vacuum exhausted The gas is evacuated until the partial pressure of water becomes 5 × 10 -4 Pa. After that, the introduction amount of argon and oxygen was adjusted, while the substrate was transported at a transport speed of 7.7 m / min and a transport tension of 40 to 120 N, while the optical adjustment level (the first hardened resin layer) was DC sputtered while outputting 12.5 kW. Film formation was performed to form an ITO film with a thickness of 22 nm. The surface resistance of the obtained ITO was measured by a four-terminal method, and the result was 300 Ω / □.
(載體薄膜之形成) 藉由一般之溶液聚合，以丙烯酸丁酯/丙烯酸=100/6(重量比)獲得重量平均分子量60萬之丙烯酸系聚合物。相對於此丙烯酸系聚合物100重量份，添加6重量份之環氧系交聯劑(三菱瓦斯化學製 商品名「TETRAD-C(註冊商標)」)，準備丙烯酸系黏著劑。於作為保護薄膜之厚度50μm之聚環烯烴薄膜(日本ZEON製 商品名「ZEONOR(註冊商標)」)的單面塗佈前述丙烯酸系黏著劑，於150℃加熱90秒，形成厚度10μm之黏著劑層。接著，於前述黏著劑層之表面貼合於單面經實施聚矽氧處理之PET剝離片(厚度25μm)之聚矽氧處理面，於50℃保存二天，製作附有剝離片之載體薄膜。又，於使用時去除前述剝離片，使用載體薄膜。(Formation of a carrier film) An acrylic polymer having a weight average molecular weight of 600,000 was obtained by general solution polymerization with butyl acrylate / acrylic acid = 100/6 (weight ratio). With respect to 100 parts by weight of the acrylic polymer, 6 parts by weight of an epoxy-based crosslinking agent (trade name "TETRAD-C (registered trademark) manufactured by Mitsubishi Gas Chemical Co., Ltd.") was added to prepare an acrylic adhesive. The acrylic adhesive was coated on one side of a 50 μm thick polycycloolefin film (trade name “ZEONOR (registered trademark)” manufactured by ZEON, Japan) as a protective film, and heated at 150 ° C. for 90 seconds to form a 10 μm thick adhesive. Floor. Next, the surface of the aforementioned adhesive layer was bonded to the silicone-treated surface of a silicone release-treated PET release sheet (thickness: 25 μm) on one side, and stored at 50 ° C. for two days to prepare a carrier film with a release sheet. The release sheet was removed during use, and a carrier film was used.
(附載體薄膜之透明導電性薄膜之形成) 於透明導電性薄膜之未形成透明導電膜之面側積層載體薄膜之附黏著劑層之保護薄膜，製作附載體薄膜之透明導電性薄膜。(Formation of a transparent conductive film with a carrier film) A protective film with an adhesive layer is laminated on the carrier film of the transparent conductive film on the side where the transparent conductive film is not formed to produce a transparent conductive film with a carrier film.
[實施例2~6] 除了於實施例1中如表1所示般變更透明樹脂薄膜及保護薄膜之基材及厚度外，以與實施例1相同方法製作附載體薄膜之透明導電性薄膜。再者，關於表1所記載之基材，PET使用聚對苯二甲酸乙二酯薄膜(三菱樹脂股份有限公司製、T612E25)，PC使用聚碳酸酯樹脂(帝人製 商品名「PANLITE」)。[Examples 2 to 6] A transparent conductive film with a carrier film was prepared in the same manner as in Example 1 except that the substrate and thickness of the transparent resin film and the protective film were changed as shown in Table 1 in Example 1. Regarding the substrates described in Table 1, polyethylene terephthalate film (manufactured by Mitsubishi Resin Co., Ltd., T612E25) was used for PET, and polycarbonate resin (trade name "PANLITE" manufactured by Teijin) was used for PC.
[比較例1] 除了於實施例1中取代聚環烯烴薄膜而使用聚對苯二甲酸乙二酯薄膜(三菱樹脂股份有限公司製、T612E25)作為保護薄膜外，以與實施例1相同方法製作附載體薄膜之透明導電性薄膜。[Comparative Example 1] 制作 It was produced in the same manner as in Example 1, except that a polyethylene terephthalate film (manufactured by Mitsubishi Resin Co., Ltd., T612E25) was used instead of the polycycloolefin film in Example 1. Transparent conductive film with carrier film.
[比較例2~3] 除了於實施例1中如表1所示般變更保護薄膜之基材及厚度外，以與實施例1相同方法製作附載體薄膜之透明導電性薄膜。再者，關於表1所記載之基材，PET使用聚對苯二甲酸乙二酯薄膜(三菱樹脂股份有限公司製、T612E25)，PC使用聚碳酸酯樹脂(帝人製 商品名「PUREACE」)。[Comparative Examples 2 to 3] A transparent conductive film with a carrier film was produced in the same manner as in Example 1 except that the base material and thickness of the protective film were changed as shown in Table 1 in Example 1. Regarding the substrates described in Table 1, polyethylene terephthalate film (manufactured by Mitsubishi Resin Co., Ltd., T612E25) was used for PET, and polycarbonate resin (trade name "PUREACE" manufactured by Teijin) was used for PC.
[參考例1] 於實施例1中不形成載體薄膜，而僅製作透明導電性薄膜。[Reference Example 1] In Example 1, a carrier film was not formed, and only a transparent conductive film was produced.
(結果及考察) 實施例1~6之附載體薄膜之透明導電性薄膜，於120℃加熱約20分鐘後完成從非晶質朝結晶質之結晶化，到達電阻值(表面電阻值)之變動亦小，到達電阻值較低。相對於基準(參考例1)之結晶化速度亦獲得良好之結果。又，與透明導電膜之密接性亦高，不發生膜剝離。另一方面，比較例1~3之附載體薄膜之透明導電性薄膜，即使於120℃加熱約40分鐘後亦有沒完成從非晶質朝結晶質之結晶化之情形，到達電阻值(表面電阻值)之變動亦大，到達電阻值較高。相對於基準(參考例1)之結晶化速度亦慢。又，與透明導電膜之密接性亦低，發生膜剝離。(Results and investigations) The transparent conductive film with a carrier film of Examples 1 to 6, after heating at 120 ° C for about 20 minutes, the crystallization from amorphous to crystalline was completed, and the resistance value (surface resistance value) changed. It is also small, and the arrival resistance value is low. Good results were also obtained with respect to the crystallization rate with respect to the reference (Reference Example 1). Moreover, the adhesiveness with a transparent conductive film is also high, and film peeling does not occur. On the other hand, the transparent conductive film with a carrier film of Comparative Examples 1 to 3 did not finish crystallization from amorphous to crystalline even after heating at 120 ° C for about 40 minutes, reaching the resistance value (surface The variation in resistance value is also large, and the reaching resistance value is high. The crystallization rate was also slow compared to the reference (Reference Example 1). Moreover, the adhesiveness with a transparent conductive film was also low, and film peeling occurred.
1‧‧‧保護薄膜1‧‧‧ protective film
2‧‧‧黏著劑層2‧‧‧ Adhesive layer
3‧‧‧透明樹脂薄膜3‧‧‧ transparent resin film
4‧‧‧透明導電膜4‧‧‧ transparent conductive film
5‧‧‧第2硬化樹脂層5‧‧‧ 2nd hardened resin layer
6‧‧‧第1硬化樹脂層6‧‧‧ 1st hardened resin layer
7‧‧‧光學調整層7‧‧‧Optical adjustment layer
10‧‧‧載體薄膜10‧‧‧ carrier film
20‧‧‧透明導電性薄膜20‧‧‧ transparent conductive film
圖1是本發明之一實施形態之附載體薄膜之透明導電性薄膜之模式性剖面圖。 圖2是本發明之另一實施形態之附載體薄膜之透明導電性薄膜之模式性剖面圖。FIG. 1 is a schematic cross-sectional view of a transparent conductive film with a carrier film according to an embodiment of the present invention. Fig. 2 is a schematic cross-sectional view of a transparent conductive film with a carrier film according to another embodiment of the present invention.
Claims (8)
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| CN111326291A (en) * | 2018-12-17 | 2020-06-23 | 日东电工株式会社 | Method for producing conductive thin film |
| CN113954479A (en) * | 2019-06-20 | 2022-01-21 | 昭和电工株式会社 | Transparent conductive film laminate and method for processing same |
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| JP5430722B2 (en) * | 2012-07-31 | 2014-03-05 | 日東電工株式会社 | Adhesive composition, adhesive layer, adhesive sheet, surface protective sheet, optical surface protective sheet, and optical film with surface protective sheet |
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| CN111210944B (en) * | 2018-11-22 | 2023-07-25 | 日东电工株式会社 | Method for producing conductive film |
| CN111326291A (en) * | 2018-12-17 | 2020-06-23 | 日东电工株式会社 | Method for producing conductive thin film |
| CN113954479A (en) * | 2019-06-20 | 2022-01-21 | 昭和电工株式会社 | Transparent conductive film laminate and method for processing same |
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