TW202129663A - Method for producing transparent conductive film - Google Patents
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- TW202129663A TW202129663A TW109134134A TW109134134A TW202129663A TW 202129663 A TW202129663 A TW 202129663A TW 109134134 A TW109134134 A TW 109134134A TW 109134134 A TW109134134 A TW 109134134A TW 202129663 A TW202129663 A TW 202129663A
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Abstract
Description
本發明係關於一種透明導電性膜之製造方法。The present invention relates to a method for manufacturing a transparent conductive film.
先前，於具有觸控感測器之圖像顯示裝置中，作為觸控感測器之電極，多使用在透明樹脂膜上形成ITO(銦錫複合氧化物)等金屬氧化物層而獲得之透明導電性膜。然而，具備該金屬氧化物層之透明導電性膜易於因屈曲而失去導電性，而存在難以使用於可撓式顯示器等之需要屈曲性之用途上之問題。Previously, in an image display device with a touch sensor, as the electrode of the touch sensor, a transparent resin film formed by forming a metal oxide layer such as ITO (Indium Tin Composite Oxide) was often used. Conductive film. However, the transparent conductive film provided with the metal oxide layer tends to lose conductivity due to bending, and there is a problem that it is difficult to use in applications requiring flexibility such as flexible displays.
另一方面，作為屈曲性高之透明導電性膜，已知包含金屬奈米線之透明導電性膜。金屬奈米線係直徑為奈米尺寸之線狀導電性物質。於包含金屬奈米線之透明導電性膜中，藉由金屬奈米線為網眼狀，而以少量之金屬奈米線形成良好之電傳導路徑，且於網眼之間隙形成開口部，而實現較高之透光率。其另一方面，由於金屬奈米線為線狀，故易於以具有配向性之狀態而配置，因此，有於包含金屬奈米線之透明導電性膜產生導電各向異性之問題。 [先行技術文獻] [專利文獻]On the other hand, as a transparent conductive film with high flexibility, a transparent conductive film containing a metal nanowire is known. Metallic nanowires are linear conductive materials with a diameter of nanometers. In a transparent conductive film containing metal nanowires, the metal nanowires are mesh-shaped, and a small amount of metal nanowires form a good electrical conduction path, and an opening is formed in the gap of the mesh, and Achieve higher light transmittance. On the other hand, since the metal nanowire is linear, it is easy to arrange it in a state of alignment. Therefore, there is a problem of conductive anisotropy in the transparent conductive film containing the metal nanowire. [Advanced Technical Literature] [Patent Literature]
[專利文獻1] 日本特表2009-505358號公報 [專利文獻2] 日本專利第6199034號[Patent Document 1] Japanese Special Publication No. 2009-505358 [Patent Document 2] Japanese Patent No. 6199034
[發明所欲解決之問題][The problem to be solved by the invention]
本發明係為了解決上述課題而完成者，其目的在於提供一種製造即便在包含金屬奈米線下導電各向異性亦為小之透明導電性膜之方法。 [解決課題之技術手段]The present invention was made in order to solve the above-mentioned problems, and its object is to provide a method for manufacturing a transparent conductive film with small conductive anisotropy even when metal nanowires are included. [Technical means to solve the problem]
本發明之透明導電性膜之製造方法包含：塗佈步驟，其一面搬送長條狀之基材，一面於該基材塗佈包含金屬奈米線之透明導電層形成用組成物而形成塗佈層；及乾燥步驟，其使該塗佈層乾燥而於該基材上形成透明導電層；且該基材之表面之平均傾斜角θa為0.5ﾟ以上。 於一個實施形態中，上述基材之表面之凹凸之平均間隔Sm為0.4 mm以下。 根據本發明之另一態樣，提供一種透明導電性膜。該透明導電性膜具備基材、及配置於該基材之一側之透明導電層，且該基材之表面之平均傾斜角θa為0.6ﾟ以上。 [發明之效果]The manufacturing method of the transparent conductive film of the present invention includes a coating step, one side of which conveys a long substrate, and one side of which is coated with a composition for forming a transparent conductive layer containing a metal nanowire to form a coating And a drying step of drying the coating layer to form a transparent conductive layer on the substrate; and the average inclination angle θa of the surface of the substrate is 0.5 ﾟ or more. In one embodiment, the average interval Sm of the unevenness on the surface of the substrate is 0.4 mm or less. According to another aspect of the present invention, a transparent conductive film is provided. The transparent conductive film includes a substrate and a transparent conductive layer arranged on one side of the substrate, and the average inclination angle θa of the surface of the substrate is 0.6ﾟ or more. [Effects of Invention]
根據本發明，可提供一種製造導電各向異性小之透明導電性膜之方法。According to the present invention, a method of manufacturing a transparent conductive film with small conductive anisotropy can be provided.
A. 透明導電性膜之製造方法
本發明之透明導電性膜之製造方法包含：塗佈步驟，其一面搬送長條狀之基材，一面於該基材塗佈包含金屬奈米線之透明導電層形成用組成物而形成塗佈層；及乾燥步驟，其使該塗佈層乾燥而於該基材上形成透明導電層。代表性而言，以一面放出輥狀態之基材並搬送該基材，一面進行上述塗佈步驟及送風步驟，形成如圖1所示般具備基材10及配置於基材10之一側之透明導電層20之長條狀之透明導電性膜100。於一個實施形態中，該透明導電性膜在乾燥步驟後被捲繞。 A. The manufacturing method of transparent conductive film The manufacturing method of the transparent conductive film of the present invention includes: a coating step, one side of which conveys a long substrate, and the other side is coated with a transparent conductive metal nanowire containing metal nanowire Layer formation composition to form a coating layer; and a drying step of drying the coating layer to form a transparent conductive layer on the substrate. Typically, the substrate in the state of a roll is fed out on one side and the substrate is conveyed, and the above-mentioned coating step and air blowing step are performed on the same side to form a
A-1. 塗佈步驟 如上述般，於塗佈步驟中，一面搬送長條狀之基材，一面於該基材塗佈包含金屬奈米線之透明導電層形成用組合物而形成塗佈層。 A-1. Coating step As described above, in the coating step, while conveying a long substrate, the substrate is coated with a transparent conductive layer forming composition containing metal nanowires to form a coating Floor.
(基材) 上述基材之表面之平均傾斜角θa為0.5ﾟ以上。於本發明中，藉由使用表面形狀被如上述般特定之基材，而在塗佈層中金屬奈米線良好地分散，而該金屬奈米線之配向紊亂，其結果為，可製造導電各向異性小之透明導電性膜。再者，於本說明書中，所謂基材之表面係預定形成塗佈層之面。(Substrate) The average inclination angle θa of the surface of the substrate is 0.5ﾟ or more. In the present invention, by using a substrate whose surface shape is specified as described above, the metal nanowires are well dispersed in the coating layer, and the alignment of the metal nanowires is disordered. As a result, it is possible to produce conductive Transparent conductive film with small anisotropy. Furthermore, in this specification, the surface of the substrate is the surface on which the coating layer is intended to be formed.
上述基材之表面之平均傾斜角θa較佳為0.8ﾟ以上，更佳為1ﾟ以上，進一步更佳為1.2ﾟ以上，尤佳為1.4ﾟ以上。若為如此之範圍，則上述本發明之效果更顯著。平均傾斜角θa之上限，例如為3ﾟ(較佳為2.5ﾟ，更佳為2ﾟ)。於本說明書中，平均傾斜角度θa係由下述式(1)而定義。 θa=tan-1 Δa ···(1) 於上述式(1)中，Δa如下述式(2)所示般，係在規定以JIS B 0601(1994年度版)規定之粗糙度曲線之基準長度L中，將相鄰之山頂之頂點與低谷之最低點之差(高度h)之合計(h1+h2+h3···+hn)以上述基準長度L相除之值。上述粗糙度曲線係自剖面曲線中利用相位差補償形高域濾波器去除長於特定之波長之表面起伏成分之曲線。又，所謂上述剖面曲線，係指在以與對象面為直角之平面將對象面切斷時，顯現於該缺口之輪廓。 Δa=(h1+h2+h3···+hn)/L ···(2)The average inclination angle θa of the surface of the substrate is preferably 0.8ﾟ or more, more preferably 1ﾟ or more, still more preferably 1.2ﾟ or more, and particularly preferably 1.4ﾟ or more. If it is in such a range, the effect of the above-mentioned present invention will be more remarkable. The upper limit of the average inclination angle θa is, for example, 3ﾟ (preferably 2.5ﾟ, more preferably 2ﾟ). In this specification, the average inclination angle θa is defined by the following formula (1). θa=tan -1 Δa ···(1) In the above formula (1), Δa is as shown in the following formula (2), which is the basis of the roughness curve stipulated in JIS B 0601 (1994 edition) In the length L, the total (h1+h2+h3···+hn) of the difference (h1+h2+h3···+hn) between the apex of the adjacent mountain top and the lowest point of the trough is divided by the above-mentioned reference length L. The above-mentioned roughness curve is a curve obtained by using a phase difference compensation high-range filter to remove surface undulation components longer than a specific wavelength from the profile curve. In addition, the above-mentioned cross-sectional curve refers to the outline that appears in the notch when the target surface is cut by a plane at right angles to the target surface. Δa=(h1+h2+h3···+hn)/L···(2)
上述基材之表面之凹凸之平均間隔Sm較佳為0.4 mm以下，更佳為0.3 mm以下，進一步更佳為0.25 mm以下，尤佳為0.2 mm以下，最佳為0.15 mm以下。若凹凸之平均間隔Sm愈大，則愈可減小金屬奈米線之配向性，而可製造導電各向異性特別小之透明導電性膜。又，若增大凹凸之平均間隔Sm，則即便平均傾斜角θa為比較小(例如，平均傾斜角θa=0.6ﾟ～1ﾟ)，仍可獲得顯著之導電各向異性減小效果。上述凹凸之平均間隔Sm下限例如為0.03 mm(較佳為0.04 mm)。平均傾斜角θa之定義係基於JIS B 0601(1994年版)。The average interval Sm of the unevenness on the surface of the substrate is preferably 0.4 mm or less, more preferably 0.3 mm or less, still more preferably 0.25 mm or less, particularly preferably 0.2 mm or less, and most preferably 0.15 mm or less. If the average interval Sm of the unevenness is larger, the orientation of the metal nanowire can be reduced, and a transparent conductive film with particularly small conductive anisotropy can be produced. In addition, if the average interval Sm of concavities and convexities is increased, even if the average inclination angle θa is relatively small (for example, the average inclination angle θa=0.6~1ﾟ), a significant conductive anisotropy reduction effect can be obtained. The lower limit of the average interval Sm of the aforementioned concavities and convexities is, for example, 0.03 mm (preferably 0.04 mm). The definition of the average tilt angle θa is based on JIS B 0601 (1994 edition).
上述基材之表面之算術平均表面粗糙度Ra較佳為0.05 μm～3 μm，更佳為0.1 μm～1.5 μm。若為如此之範圍，則可製造導電各向異性特別小之透明導電性膜。算術平均表面粗糙度Ra之定義係基於JIS B 0601(1994年版)。The arithmetic average surface roughness Ra of the surface of the substrate is preferably 0.05 μm to 3 μm, more preferably 0.1 μm to 1.5 μm. If it is in such a range, a transparent conductive film with particularly small conductive anisotropy can be produced. The definition of arithmetic mean surface roughness Ra is based on JIS B 0601 (1994 edition).
上述基材之厚度較佳為20 μm～200 μm，更佳為30 μm～150 μm。The thickness of the aforementioned substrate is preferably 20 μm to 200 μm, more preferably 30 μm to 150 μm.
上述基材之全光線透過率較佳為30%以上，更佳為35%以上，尤佳為40%以上。The total light transmittance of the substrate is preferably 30% or more, more preferably 35% or more, and particularly preferably 40% or more.
構成上述基材之材料，可使用任意之適切之材料。具體而言，例如，可較佳地使用膜或塑膠基材等高分子基材。此係緣於在基材之平滑性及對於透明導電層形成用組合物之潤濕性上優異，且可藉由利用輥進行之連續生產而使生產性大幅度提高之故。Any suitable material can be used for the material constituting the above-mentioned base material. Specifically, for example, a polymer substrate such as a film or a plastic substrate can be preferably used. This is due to the excellent wettability of the substrate smoothness and the composition for forming a transparent conductive layer, and the productivity can be greatly improved by continuous production using rollers.
構成上述基材之材料，代表性而言是以熱固性樹脂為主成分之高分子膜。作為熱固性樹脂，例如可舉出：聚酯系樹脂、聚降冰片烯等環烯系樹脂、丙烯酸系樹脂、聚碳酸酯樹脂、纖維素系樹脂等。其中較佳為聚酯系樹脂、環烯系樹脂或丙烯酸系樹脂。該等樹脂在透明性、機械強度、熱穩定性、水分阻斷性等上優異。上述熱固性樹脂可單獨使用，或可組合兩種以上而使用。又，如使用於偏光板之光學膜，例如亦可將低相位差基材、高相位差基材、相位差板、增亮膜等用作基材。The material constituting the above-mentioned substrate is typically a polymer film with a thermosetting resin as the main component. Examples of thermosetting resins include polyester resins, cycloolefin resins such as polynorbornene, acrylic resins, polycarbonate resins, and cellulose resins. Among them, polyester-based resins, cycloolefin-based resins, or acrylic resins are preferred. These resins are excellent in transparency, mechanical strength, thermal stability, moisture barrier properties, and the like. The above-mentioned thermosetting resin may be used alone or in combination of two or more kinds. In addition, as an optical film used for a polarizing plate, for example, a low retardation substrate, a high retardation substrate, a retardation plate, a brightness enhancement film, etc. can also be used as a substrate.
作為基材之搬送方法，可採用任意之適切之方法。例如，可舉出由搬送輥進行之搬送、由搬送帶進行之搬送、該等之組合等。搬送速度例如為5 m/min～50 m/min。As the conveying method of the substrate, any suitable method can be adopted. For example, transportation by a transportation roller, transportation by a transportation belt, a combination of these, and the like can be cited. The transport speed is, for example, 5 m/min to 50 m/min.
(金屬奈米線) 所謂金屬奈米線係材質為金屬且形狀為針狀或絲狀並且直徑為奈米尺寸之導電性物質。金屬奈米線可為直線狀，亦可為曲線狀。若使用包含金屬奈米線之透明導電層，則藉由金屬奈米線為網眼狀，即便以少量之金屬奈米線仍可形成良好之電傳導路徑，而可獲得電阻小之透明導電性膜。進而，藉由金屬奈米線為網眼狀，而於網眼之間隙形成開口部，而可獲得透光率高之透明導電性膜。(Metal Nanowire) The so-called metal nanowire is a conductive material whose material is metal, is needle-like or thread-like, and has a diameter of nanometers. Metal nanowires can be straight or curved. If a transparent conductive layer containing metal nanowires is used, the mesh-shaped metal nanowires can form a good electrical conduction path even with a small amount of metal nanowires, and a transparent conductivity with low resistance can be obtained. membrane. Furthermore, since the metal nanowire has a mesh shape and an opening is formed in the gap of the mesh, a transparent conductive film with high light transmittance can be obtained.
上述金屬奈米線之粗細d與長度L與之比(縱橫比：L/d)較佳為10～100,000，更佳為50～100,000，尤佳為100～10,000。若使用如此般縱橫比大之金屬奈米線，則金屬奈米線良好地交叉，而可藉由少量之金屬奈米線表現較高之導電性。其結果為，可獲得透光率高之透明導電性膜。再者，於本說明書中，所謂「金屬奈米線之粗細」，在金屬奈米線之剖面為圓狀之情形下意指其直徑，在為橢圓狀之情形下意指其短徑，在為多角形之情形下意指最長之對角線。金屬奈米線之粗細及長度可藉由掃描型電子顯微鏡或透過型電子顯微鏡而確認。The ratio of the thickness d to the length L (aspect ratio: L/d) of the metal nanowire is preferably 10 to 100,000, more preferably 50 to 100,000, and particularly preferably 100 to 10,000. If metal nanowires with such a large aspect ratio are used, the metal nanowires cross well, and a small amount of metal nanowires can exhibit higher conductivity. As a result, a transparent conductive film with high light transmittance can be obtained. Furthermore, in this specification, the "thickness of the metal nanowire" refers to the diameter of the metal nanowire when the cross-section of the metal nanowire is round, and the short diameter when the cross section of the metal nanowire is elliptical. In the case of a polygon, it means the longest diagonal. The thickness and length of the metal nanowire can be confirmed with a scanning electron microscope or a transmission electron microscope.
上述金屬奈米線之粗細較佳為未達500 nm，更佳為未達200 nm，尤佳為10 nm～100 nm，最佳為10 nm～50 nm。若為如此之範圍，則可形成透光率高之透明導電層。The thickness of the metal nanowire is preferably less than 500 nm, more preferably less than 200 nm, particularly preferably 10 nm to 100 nm, and most preferably 10 nm to 50 nm. If it is in such a range, a transparent conductive layer with high light transmittance can be formed.
上述金屬奈米線之長度較佳為1 μm～1000 μm，更佳為10 μm～500 μm，尤佳為10 μm～100 μm。若為如此之範圍，則可獲得導電性高之透明導電性膜。又，若金屬奈米線之長度為上述範圍，則藉由將基材之表面形狀如上述般特定而獲得之效果變大。The length of the metal nanowire is preferably 1 μm to 1000 μm, more preferably 10 μm to 500 μm, and particularly preferably 10 μm to 100 μm. If it is such a range, a transparent conductive film with high conductivity can be obtained. In addition, if the length of the metal nanowire is within the above range, the effect obtained by specifying the surface shape of the substrate as described above becomes greater.
作為構成上述金屬奈米線之金屬只要為導電性金屬，則可使用任意之適切之金屬。作為構成上述金屬奈米線之金屬，例如可舉出銀、金、銅、鎳等。又，亦可使用對該等金屬進行了鍍覆處理(例如，鍍金處理)之材料。其中較佳的是，自導電性之觀點而言為銀、銅或金，更佳的是銀。As the metal constituting the metal nanowire, any suitable metal can be used as long as it is a conductive metal. Examples of the metal constituting the metal nanowire include silver, gold, copper, nickel, and the like. In addition, materials that have been plated (for example, gold-plated) on these metals can also be used. Among them, silver, copper, or gold is preferable from the viewpoint of conductivity, and silver is more preferable.
作為上述金屬奈米線之製造方法，可採用任意之適切之方法。例如可舉出在溶液中還原硝酸銀之方法、及對前驅體表面自探針之前端部作用施加電壓或電流，而在探針前端部引出金屬奈米線，並連續性地形成該金屬奈米線之方法等。於在溶液中還原硝酸銀之方法中，可在乙二醇等聚醇、及聚乙烯吡咯烷酮之存在下，藉由液相還原硝酸銀等之銀鹽，而合成銀奈米線。均一尺寸之銀奈米線，例如可基於Xia, Y. et al., Chem. Mater. (2002)、14、4736-4745、Xia, Y. et al., Nano letters (2003) 3(7)、955-960中記載之方法而大量生產。As the manufacturing method of the above-mentioned metal nanowire, any appropriate method can be adopted. For example, a method of reducing silver nitrate in a solution, and applying a voltage or current to the surface of the precursor from the front end of the probe, and draw a metal nanowire at the front end of the probe, and continuously form the metal nanometer. Line method, etc. In the method of reducing silver nitrate in a solution, silver nanowires can be synthesized by reducing silver salts such as silver nitrate in a liquid phase in the presence of polyols such as ethylene glycol and polyvinylpyrrolidone. Uniform size silver nanowires, for example, can be based on Xia, Y. et al., Chem. Mater. (2002), 14, 4736-4745, Xia, Y. et al., Nano letters (2003) 3(7) , The method described in 955-960 and mass production.
(透明導電層形成用組合物) 透明導電層形成用組合物包含金屬奈米線。於一個實施形態中，使金屬奈米線分散於任意之適切之溶劑中而調製透明導電層形成用組合物。作為該溶劑，可舉出：水、醇系溶劑、酮系溶劑、芳醚系溶劑、烴系溶劑、芳香族系溶劑等。又，透明導電層形成用組合物亦可更包含樹脂(黏合劑樹脂)、金屬奈米線以外之導電性材料(例如，導電性粒子)、流平劑等添加劑。又 ，透明導電層形成用組合物亦可包含可塑劑、熱穩定劑、光穩定劑、滑劑、抗氧化劑、紫外線吸收劑、阻燃劑、著色劑、抗靜電劑、相溶劑、交聯劑、增稠劑、無機粒子、界面活性劑、及分散劑等添加劑。(Composition for forming transparent conductive layer) The composition for forming a transparent conductive layer contains a metal nanowire. In one embodiment, a metal nanowire is dispersed in any suitable solvent to prepare a composition for forming a transparent conductive layer. Examples of the solvent include water, alcohol-based solvents, ketone-based solvents, aromatic ether-based solvents, hydrocarbon-based solvents, and aromatic-based solvents. In addition, the composition for forming a transparent conductive layer may further contain additives such as resin (binder resin), conductive materials other than metal nanowires (for example, conductive particles), and leveling agents. In addition, the composition for forming a transparent conductive layer may also contain a plasticizer, a heat stabilizer, a light stabilizer, a slip agent, an antioxidant, an ultraviolet absorber, a flame retardant, a colorant, an antistatic agent, a phase solvent, and a crosslinking agent. , Additives such as thickeners, inorganic particles, surfactants, and dispersants.
透明導電層形成用組合物之黏度較佳為5 mP·s/25℃～300 mP·s/25℃，更佳為10 mP·s/25℃～100 mP·s/25℃。若為如此之範圍，則藉由將基材之表面形狀如上述般特定而獲得之效果變大。透明導電層形成用組合物之黏度可藉由流變儀(例如，安東帕(Anton Paar)公司之MCR302)而測定。The viscosity of the composition for forming a transparent conductive layer is preferably 5 mP·s/25°C to 300 mP·s/25°C, more preferably 10 mP·s/25°C to 100 mP·s/25°C. If it is in such a range, the effect obtained by specifying the surface shape of the substrate as described above becomes greater. The viscosity of the composition for forming a transparent conductive layer can be measured by a rheometer (for example, MCR302 from Anton Paar).
透明導電層形成用組合物中之金屬奈米線之分散濃度較佳為0.01重量%～5重量%。若為如此之範圍，則本發明之效果顯著。The dispersion concentration of the metal nanowires in the composition for forming a transparent conductive layer is preferably 0.01% by weight to 5% by weight. If it is in such a range, the effect of the present invention is remarkable.
作為上述透明導電層形成用組合物之塗佈方法，可採用任意之適切之方法。作為塗佈方法，例如可舉出：噴塗、棒塗、輥塗、模塗、噴墨塗、絲網塗、浸塗、凸版印刷法、凹版印刷法、照相凹版印刷法等。As the coating method of the composition for forming the transparent conductive layer, any appropriate method can be adopted. Examples of coating methods include spray coating, bar coating, roll coating, die coating, inkjet coating, screen coating, dip coating, relief printing, gravure printing, gravure printing, and the like.
上述塗佈層之單位面積之重量，較佳為0.3 g/m2 ～30 g/m2 ，更佳為1.6 g/m2 ～16 g/m2 。若為如此之範圍，則藉由將基材之表面形狀如上述般特定而獲得之效果變大。The weight per unit area of the coating layer is preferably 0.3 g/m 2 to 30 g/m 2 , more preferably 1.6 g/m 2 to 16 g/m 2 . If it is in such a range, the effect obtained by specifying the surface shape of the substrate as described above becomes greater.
上述塗佈層之膜厚較佳為1 μm～50 μm，更佳為2 μm～40 μm。The film thickness of the coating layer is preferably 1 μm-50 μm, more preferably 2 μm-40 μm.
A-2. 乾燥步驟 如上述般，於乾燥步驟中，使上述塗佈層乾燥而於該基材上形成透明導電層。 A-2. Drying step As described above, in the drying step, the coating layer is dried to form a transparent conductive layer on the substrate.
作為塗佈層之乾燥方法，可採用任意之適切之乾燥方法(例如自然乾燥、送風乾燥、加熱乾燥)。例如，於加熱乾燥之情形下，乾燥溫度代表性而言為80℃～150℃，乾燥時間代表性而言為1～20分鐘。As the drying method of the coating layer, any suitable drying method (for example, natural drying, air blowing drying, heat drying) can be adopted. For example, in the case of heating and drying, the drying temperature is typically 80°C to 150°C, and the drying time is typically 1 to 20 minutes.
可在乾燥步驟之後進行任意之適切之處理。例如，在使用包含黏合劑樹脂之透明導電層形成用組合物之情形下，可進行藉由紫外線照射等而實施之固化處理。Any appropriate treatment can be performed after the drying step. For example, in the case of using a composition for forming a transparent conductive layer containing a binder resin, curing treatment by ultraviolet irradiation or the like can be performed.
B. 透明導電性膜
藉由上述之製造方法而形成透明導電性膜。圖1係本發明之一個實施形態之透明導電性膜之概略剖視圖。透明導電性膜100包含：基材10；及透明導電層20，其配置於該基材10之一側。 B. Transparent conductive film A transparent conductive film is formed by the above-mentioned manufacturing method. Fig. 1 is a schematic cross-sectional view of a transparent conductive film according to an embodiment of the present invention. The transparent
透明導電性膜之表面電阻值較佳為0.1 Ω/□～1000 Ω/□，更佳為0.5 Ω/□～300 Ω/□，尤佳為1 Ω/□～200 Ω/□。透明導電性膜之TD(與MD正交之方向)上之表面電阻值相對於MD(搬送方向)上之表面電阻值之比(TD/MD)，較佳為0.7～1.5，更佳為0.8～1.2，尤佳為0.9～1.1。表面電阻值可藉由三菱化學分析科技(MITSUBISHI CHEMICAL ANALYTECH)公司之「阻抗率自動測定系統 MCP-S620型·MCP-S521型」而測定。The surface resistance of the transparent conductive film is preferably 0.1 Ω/□～1000 Ω/□, more preferably 0.5 Ω/□～300 Ω/□, especially preferably 1 Ω/□～200 Ω/□. The ratio (TD/MD) of the surface resistance value of the transparent conductive film in TD (direction orthogonal to MD) to the surface resistance value in MD (transport direction), preferably 0.7 to 1.5, more preferably 0.8 ～1.2, particularly preferably 0.9～1.1. The surface resistance value can be measured by the "Automatic resistivity measurement system MCP-S620 type·MCP-S521 type" of MITSUBISHI CHEMICAL ANALYTECH.
上述透明導電性膜之霧度值較佳為20%以下，更佳為10%以下，尤佳為0.1%～5%。The haze value of the transparent conductive film is preferably 20% or less, more preferably 10% or less, and particularly preferably 0.1% to 5%.
上述透明導電性膜之全光線透過率較佳為30%以上，更佳為35%，尤佳為40%以上。The total light transmittance of the transparent conductive film is preferably 30% or more, more preferably 35%, and particularly preferably 40% or more.
上述基材之表面之平均傾斜角θa為0.6ﾟ以上，較佳為0.8ﾟ以上，更佳為1ﾟ以上，進一步更佳為1.2ﾟ以上，尤佳為1.4ﾟ以上。若為如此之範圍，則上述本發明之效果更顯著。平均傾斜角θa之上限例如為3ﾟ(較佳為2.5ﾟ，更佳為2ﾟ)。再者，基材之表面之上述平均傾斜角θa係在透明導電層形成前測定者。The average inclination angle θa of the surface of the substrate is 0.6ﾟ or more, preferably 0.8ﾟ or more, more preferably 1ﾟ or more, still more preferably 1.2ﾟ or more, and particularly preferably 1.4ﾟ or more. If it is in such a range, the effect of the above-mentioned present invention will be more remarkable. The upper limit of the average inclination angle θa is, for example, 3ﾟ (preferably 2.5ﾟ, more preferably 2ﾟ). Furthermore, the above-mentioned average inclination angle θa of the surface of the substrate is measured before the formation of the transparent conductive layer.
上述基材之表面之凹凸之平均間隔Sm較佳為0.4 mm以下，更佳為0.3 mm以下，進一步更佳為0.25 mm以下，尤佳為0.2 mm以下，最佳為0.15 mm以下。再者，基材之表面之上述凹凸之平均間隔Sm係在透明導電層形成前被測定者。The average interval Sm of the unevenness on the surface of the substrate is preferably 0.4 mm or less, more preferably 0.3 mm or less, still more preferably 0.25 mm or less, particularly preferably 0.2 mm or less, and most preferably 0.15 mm or less. Furthermore, the average interval Sm of the above-mentioned concavities and convexities on the surface of the substrate is measured before the formation of the transparent conductive layer.
上述基材之表面之算術平均表面粗糙度Ra較佳為0.05 μm～3 μm，更佳為0.1 μm～1.5 μm。再者，基材之表面之上述算術平均表面粗糙度Ra係在透明導電層形成前測定者。The arithmetic average surface roughness Ra of the surface of the substrate is preferably 0.05 μm to 3 μm, more preferably 0.1 μm to 1.5 μm. Furthermore, the arithmetic average surface roughness Ra of the surface of the substrate is measured before the transparent conductive layer is formed.
透明導電層之單位面積之重量較佳為0.001 g/m2 ～0.09 g/m2 ，更佳為0.005 g/m2 ～0.05 g/m2 。The weight per unit area of the transparent conductive layer is preferably 0.001 g/m 2 to 0.09 g/m 2 , more preferably 0.005 g/m 2 to 0.05 g/m 2 .
上述透明導電層之金屬奈米線之含有比例，相對於構成透明導電層之黏合劑樹脂100重量份，較佳為0.1重量份～50重量份，更佳為0.1重量份～30重量份。若為如此之範圍，則可獲得在導電性及光透過性上優異之透明導電性膜。 [實施例]The content ratio of the metal nanowire in the transparent conductive layer is preferably 0.1 to 50 parts by weight, and more preferably 0.1 to 30 parts by weight relative to 100 parts by weight of the binder resin constituting the transparent conductive layer. If it is in such a range, a transparent conductive film excellent in conductivity and light transmittance can be obtained. [Example]
以下，藉由實施例對於本發明具體性地進行説明，但本發明並不受該等實施例任何限定。實施例之評估方法如以下所述般。再者，關於厚度，在利用環氧樹脂進行包埋處理後藉由利用超薄切片機切削而形成剖面，並使用日立高新技術(High-Technologies)公司製之掃描型電子顯微鏡「S-4800」而測定。Hereinafter, the present invention will be specifically described with examples, but the present invention is not limited in any way by these examples. The evaluation methods of the examples are as follows. Regarding the thickness, the cross section was formed by cutting with an ultra-thin microtome after embedding with epoxy resin, and using a scanning electron microscope "S-4800" manufactured by Hitachi High-Technologies. And determined.
(1)基材表面之形狀 依照JIS B0601(1994年度版)，測定平均凹凸間距離Sm(mm)及算術平均表面粗糙度Ra(μm)。具體而言，於與測定面為相反側之面，利用黏著劑貼合玻璃板(松浪(MATSUNAMI)公司製、MICRO SLIDE GLASS、品號S、厚度1.3 mm、45×50 mm)，而製作試料。使用具有前端部(金剛石)之曲率半徑R=2 μm之測定針之觸針式表面粗糙度測定器((股)小阪研究所製、高精度細微形狀測定器、商品名「SURFCODER ET4000」)，在掃描速度0.1 mm/秒、截止值0.8 mm、測定長4 mm之條件下，於一定方向上測定前述試料之防眩層之表面形狀，而求得凹凸之平均間隔Sm，且，自所獲得之表面粗糙度曲線求得平均傾斜角度θa(ﾟ)。(1) The shape of the substrate surface According to JIS B0601 (1994 edition), the average distance between unevenness Sm (mm) and the arithmetic average surface roughness Ra (μm) are measured. Specifically, a glass plate (manufactured by MATSUNAMI, MICRO SLIDE GLASS, article number S, thickness 1.3 mm, 45×50 mm) was bonded to the surface opposite to the measurement surface with an adhesive to prepare a sample . Use a stylus-type surface roughness tester (made by Kosaka Laboratories, a high-precision fine shape tester, trade name "SURFCODER ET4000") with a measuring needle with a tip (diamond) curvature radius R=2 μm, Under the conditions of scanning speed of 0.1 mm/sec, cutoff value of 0.8 mm, and measuring length of 4 mm, the surface shape of the anti-glare layer of the aforementioned sample was measured in a certain direction, and the average interval between concavities and convexities Sm was obtained, and obtained from Calculate the average inclination angle θa(ﾟ) from the surface roughness curve.
(2) 表面電阻值 對於透明導電性膜之表面電阻值(MD及TD之表面電阻值)，使用NAPSON股份有限公司製之非接觸表面電阻測試儀、商品名「EC-80」，藉由渦電流法進行了測定。測定溫度設為23℃。(2) Surface resistance value The surface resistance value of the transparent conductive film (surface resistance value of MD and TD) was measured by the eddy current method using a non-contact surface resistance tester manufactured by NAPSON Co., Ltd., trade name "EC-80". The measurement temperature was 23°C.
[製造例1]透明導電層形成用組合物之調製 基於Chem. Mater. 2002，14，4736-4745中記載之方法，合成銀奈米線。 以使上文中獲得之銀奈米線成為0.2重量%、及使十二烷基五乙二醇成為0.1重量%之濃度之方式分散於純水中，而獲得透明導電層形成用組合物。[Manufacturing Example 1] Preparation of a composition for forming a transparent conductive layer Based on the method described in Chem. Mater. 2002, 14, 4736-4745, silver nanowires were synthesized. The silver nanowire obtained above was dispersed in pure water so that the concentration of the silver nanowire was 0.2% by weight and the concentration of dodecylpentaethylene glycol was 0.1% by weight, to obtain a composition for forming a transparent conductive layer.
[實施例1] 於PET膜(東麗(TORAY)公司製、商品名「U40」、厚度：23 μm)，塗佈包含：丙烯酸單體(大阪有機化學工業公司製、商品名「Viscoat#300」、固形分56重量%)100重量份、粒子(積水化成公司製、商品名「TECHPOLYMER SSX-105」)30重量份、引發劑(BASF公司製、商品名「Irgacure 127」)0.5重量份、及乙酸丁酯35重量份之塗佈液，在100℃下乾燥2分鐘，其後照射300 mJ之紫外線，而於PET膜上形成基材A(厚度：20 μm)。 於自PET膜剝離之上述基材A上，使用棒式塗佈機(第一理科股份有限公司製、產品名「棒式塗佈機 No.16」)塗佈製造例1中所調製之透明導電層形成用組成物，在120℃之送風乾燥機內乾燥2分鐘，而形成透明導電層，而獲得具備基材及透明導電層之透明導電性膜。再者，基材A之形成有透明導電層之面之平均傾斜角θa為1.5ﾟ，凹凸之平均間隔Sm為0.05 mm。 將所獲得之透明導電性膜提供給上述評估(2)。將結果示於表1。[Example 1] On PET film (manufactured by Toray, brand name "U40", thickness: 23 μm), the coating contains: acrylic monomer (manufactured by Osaka Organic Chemical Industry Co., Ltd., brand name "Viscoat #300", solid content 56 % By weight) 100 parts by weight, 30 parts by weight of particles (manufactured by Sekisui Kasei, trade name "TECHPOLYMER SSX-105"), 0.5 parts by weight of initiator (manufactured by BASF, trade name "Irgacure 127"), and 35 parts by weight of butyl acetate Parts by weight of the coating solution were dried at 100°C for 2 minutes, and then irradiated with 300 mJ of ultraviolet rays to form a substrate A (thickness: 20 μm) on the PET film. On the above-mentioned substrate A peeled from the PET film, a bar coater (manufactured by Daiichi Science Co., Ltd., product name "bar coater No. 16") was used to coat the transparent prepared in Manufacturing Example 1 The composition for forming a conductive layer was dried in an air dryer at 120°C for 2 minutes to form a transparent conductive layer, and a transparent conductive film provided with a substrate and a transparent conductive layer was obtained. Furthermore, the average inclination angle θa of the surface of the substrate A on which the transparent conductive layer is formed is 1.5ﾟ, and the average interval Sm of the unevenness is 0.05 mm. The obtained transparent conductive film was provided to the above-mentioned evaluation (2). The results are shown in Table 1.
[實施例2] 使用粒子(總研化學公司製、商品名「SX-350H」)5重量份來取代粒子(積水化成公司製、商品名「TECHPOLYMER SSX-105」)30重量份，且於塗佈液中添加了觸變劑(國峰(KUNIMINE)工業公司製、商品名「SAN)0.2重量份，除此以外，與實施例1同樣地，形成基材B(厚度：20 μm)。其後，藉由與實施例1同樣之方法，形成透明導電層，而獲得具備基材及透明導電層之透明導電性膜。再者，基材D之形成有透明導電層之面之平均傾斜角θa為0.9ﾟ，凹凸之平均間隔Sm為0.15 mm。 將所獲得之透明導電性膜提供給上述評估(2)。將結果於表1中顯示。[Example 2] Use 5 parts by weight of particles (manufactured by Soken Chemical Co., Ltd., brand name "SX-350H") instead of 30 parts by weight of particles (manufactured by Sekisui Chemical Co., Ltd., brand name "TECHPOLYMER SSX-105"), and added to the coating liquid Except for 0.2 parts by weight of a thixotropic agent (manufactured by Kunimine Industrial Co., Ltd., trade name "SAN), the base material B (thickness: 20 μm) was formed in the same manner as in Example 1. Then, it was combined with In the same manner as in Example 1, a transparent conductive layer was formed to obtain a transparent conductive film with a substrate and a transparent conductive layer. Furthermore, the average inclination angle θa of the surface of the substrate D on which the transparent conductive layer was formed was 0.9ﾟ, The average interval Sm of bumps is 0.15 mm. The obtained transparent conductive film was provided to the above-mentioned evaluation (2). The results are shown in Table 1.
[實施例3] 除了將粒子(總研化學公司製、商品名「SX-350H」)之添加量設為10重量份以外，與實施例2同樣地，形成基材C(厚度：20 μm)。其後，藉由與實施例1同樣之方法，形成透明導電層，而獲得具備基材及透明導電層之透明導電性膜。再者，基材C之形成有透明導電層之面之平均傾斜角θa為1.5ﾟ，凹凸之平均間隔Sm為0.12 mm。 將所獲得之透明導電性膜提供給上述評估(2)。將結果於表1中顯示。[Example 3] The base material C (thickness: 20 μm) was formed in the same manner as in Example 2 except that the addition amount of the particles (manufactured by Soken Chemical Co., Ltd., brand name "SX-350H") was 10 parts by weight. Then, by the same method as Example 1, a transparent conductive layer was formed, and a transparent conductive film provided with a base material and a transparent conductive layer was obtained. Furthermore, the average inclination angle θa of the surface of the substrate C on which the transparent conductive layer is formed is 1.5ﾟ, and the average interval Sm of the unevenness is 0.12 mm. The obtained transparent conductive film was provided to the above-mentioned evaluation (2). The results are shown in Table 1.
[比較例1] 除了使用PET膜(東麗(TORAY)公司製、商品名「U40」、厚度：23 μm、平均傾斜角：0.1ﾟ、凹凸之平均間隔Sm：0.04 mm)作為基材B而取代基材A以外，與實施例1同樣地，獲得透明導電性膜。將所獲得之透明導電性膜提供給上述評估(2)。將結果於表1中顯示。[Comparative Example 1] Except for using PET film (manufactured by Toray Co., Ltd., trade name "U40", thickness: 23 μm, average tilt angle: 0.1ﾟ, average interval between unevenness Sm: 0.04 mm) as substrate B instead of substrate A In the same manner as in Example 1, a transparent conductive film was obtained. The obtained transparent conductive film was provided to the above-mentioned evaluation (2). The results are shown in Table 1.
[比較例2] 除了使用粒子(積水化成公司製、商品名「TECHNOPOLYMER SSX-101」)15重量份取代粒子(積水化成公司製、商品名「TECHPOLYMER SSX-105」)30重量份以外，與實施例1同樣地形成基材D(厚度：20 μm)。其後，藉由與實施例1同樣之方法，形成透明導電層，而獲得具備基材及透明導電層之透明導電性膜。再者，基材D之形成有透明導電層之面之平均傾斜角θa為0.3ﾟ，凹凸之平均間隔Sm為0.19 mm。 將所獲得之透明導電性膜提供給上述評估(2)。將結果於表1中顯示。[Comparative Example 2] Formed in the same manner as in Example 1, except that 15 parts by weight of particles (manufactured by Sekisui Chemical Co., Ltd., brand name "TECHNOPOLYMER SSX-101") were used instead of 30 parts by weight of particles (manufactured by Sekisui Chemical Co., Ltd., brand name "TECHNOPOLYMER SSX-105") Substrate D (thickness: 20 μm). Then, by the same method as Example 1, a transparent conductive layer was formed, and a transparent conductive film provided with a base material and a transparent conductive layer was obtained. Furthermore, the average inclination angle θa of the surface of the substrate D on which the transparent conductive layer is formed is 0.3ﾟ, and the average interval Sm of the unevenness is 0.19 mm. The obtained transparent conductive film was provided to the above-mentioned evaluation (2). The results are shown in Table 1.
【表1】
[參考例1] 於PET膜塗佈包含：丙烯酸單體(大阪有機化學工業公司製、商品名「Viscoat#300」、固形分56重量%)100重量份、粒子(積水化成公司製、商品名「TECHPOLYMER SSX-101」)10重量份、引發劑(BASF公司製、商品名「Irgacure 127」)0.5重量份、及乙酸丁酯35重量份之塗佈液，在100℃下乾燥2分鐘，其後照射300 mJ之紫外線，而於PET膜上形成基材C(厚度：20 μm)。 於自PET膜剝離之上述基材C上，使用棒式塗佈機(第一理科股份有限公司製、產品名「棒式塗佈機 No.16」)塗佈製造例1中所調製之透明導電層形成用組成物，在120℃之送風乾燥機內乾燥2分鐘，而形成透明導電層，而獲得具備基材及透明導電層之透明導電性膜。再者，基材C之形成有透明導電層之面之平均傾斜角θa為0.1ﾟ，凹凸之平均間隔Sm為0.27 mm。 將所獲得之透明導電性膜提供給上述評估(2)，結果為：MD之表面電阻值為41 Ω，TD之表面電阻值為62 Ω。[Reference example 1] The coating on the PET film contains: 100 parts by weight of acrylic monomer (manufactured by Osaka Organic Chemical Industry Co., Ltd., brand name "Viscoat #300", solid content 56% by weight), particles (manufactured by Sekisui Chemical Co., Ltd., brand name "TECHPOLYMER SSX-101" ") 10 parts by weight, 0.5 parts by weight of initiator (manufactured by BASF, trade name "Irgacure 127"), and 35 parts by weight of butyl acetate, dried at 100°C for 2 minutes, and then irradiated with 300 mJ Ultraviolet rays, and the substrate C (thickness: 20 μm) was formed on the PET film. On the above-mentioned substrate C peeled from the PET film, a bar coater (manufactured by Daiichi Science Co., Ltd., product name "bar coater No. 16") was used to coat the transparent prepared in Manufacturing Example 1 The composition for forming a conductive layer was dried in an air dryer at 120°C for 2 minutes to form a transparent conductive layer, and a transparent conductive film provided with a substrate and a transparent conductive layer was obtained. Furthermore, the average inclination angle θa of the surface of the substrate C on which the transparent conductive layer is formed is 0.1 ﾟ, and the average interval Sm of the unevenness is 0.27 mm. The obtained transparent conductive film was provided to the above evaluation (2), and the result was that the surface resistance value of MD was 41 Ω, and the surface resistance value of TD was 62 Ω.
10:基材 20:透明導電層 100:透明導電性膜10: Substrate 20: Transparent conductive layer 100: Transparent conductive film
圖1係本發明之一個實施形態之透明導電性膜之概略剖視圖。Fig. 1 is a schematic cross-sectional view of a transparent conductive film according to an embodiment of the present invention.
10:基材 10: Substrate
20:透明導電層 20: Transparent conductive layer
100:透明導電性膜 100: Transparent conductive film
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