JP5245893B2 - Multilayer film and method for producing the same - Google Patents

Multilayer film and method for producing the same Download PDF

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JP5245893B2
JP5245893B2 JP2009031784A JP2009031784A JP5245893B2 JP 5245893 B2 JP5245893 B2 JP 5245893B2 JP 2009031784 A JP2009031784 A JP 2009031784A JP 2009031784 A JP2009031784 A JP 2009031784A JP 5245893 B2 JP5245893 B2 JP 5245893B2
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裕 小林
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凸版印刷株式会社
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  The present invention relates to a multilayer film having a water vapor barrier function, an optical function, and a conductive function, and a method for producing the same.

Examples of multilayer films having two or three of the barrier function, the optical function, and the conductive function are known in which an optical film and a transparent conductive film are laminated as described in Patent Document 1 and Patent Document 2, respectively. Yes.
In addition, a barrier film, an optical film, and a transparent conductive film as listed in Patent Document 3 and Patent Document 4, respectively, or any of a barrier function, an optical function, and a conductive function as listed in Patent Document 5 It is known to give a plurality of functions by bonding films having the above functions by adhesion. Further, as an example of forming a thin film that simultaneously satisfies the barrier function and the antireflection function on a film, a method in which at least one layer of an optical film has a barrier function as in Patent Document 6 is known.

JP 11-286066 Patent No. 3626624 JP2005-70616 JP2006-4633 JP2006-327098 JP2004-291464

  Examples of functions required for a film used in an electronic device include an optical function and a conductive function. When these functions are separately imparted to the film, there is a problem that the number of processes increases.

Indium tin oxide (ITO), which is most commonly used as a transparent electrode, is classified as a high refractive index material with a higher refractive index than general glass and plastic substrates. When ITO is formed on the substrate, the transmittance is lowered (the reflectance is increased).
Moreover, since the transmittance in a short wavelength region is lowered, there is a problem that the transmitted color becomes yellowish. Furthermore, when the substrate is plastic, there is a problem that the properties of the ITO film deteriorate due to the influence of gas molecules represented by H2O contained in the substrate.

The present invention has been made in view of the above circumstances, and its object is to produce and supply a multilayer film excellent in optical function and conductive function.

As a means to solve the problem,
According to one aspect of the present invention, the said resin substrate to form different optical film refractive index on at least one surface of a transparent resin substrate, a multilayer film having a transparent conductive film on the outermost layer, the optical In order from the layer close to the transparent resin substrate, the film has a first thin film layer having a refractive index n1 of 1.50 to 1.70 and a film thickness d1 of 1 to 10 nm, and a refractive index n2 of 1.35 to 1. And a transparent conductive film is a third thin film having a refractive index n3 of 1.90 to 2.20 and a film thickness d3 of 10 to 30 nm. The multilayer film is characterized in that the multilayer film has a water vapor transmission rate at 40 ° C. and 90% Rh of 1.0 g / m 2 · day or less.

  By forming a thin film having an optical film and a conductive function at the same time on at least one surface of a transparent resin substrate, the number of processes is reduced compared to a multilayer film in which the optical function and the conductive function are separately formed, and an improvement in yield can be expected.

  Furthermore, by making this optical film into a laminated film using a plurality of high refractive index films and low refractive index films on a transparent substrate, it is possible to give higher optical performance than a single layer. For example, an antireflection function in the visible light region, a high transmission function, a transmission or reflection hue adjustment function, and the like are possible.

Furthermore, by forming such an optical function on both surfaces of the resin substrate, for example, the light transmittance can be further increased as compared with the case where the optical function is formed on one surface.

  By forming a metal suboxide on the thin film layer (first thin film layer) closest to the resin substrate of the thin film layer forming the optical function, the adhesion between the resin substrate and the thin film is improved, and the mechanical strength of the device Will also improve.

  Transparent conductive films typified by indium tin oxide (ITO), zinc oxide (ZnO), and tin oxide (SnO2) formed by vacuum film formation are optically classified as high refractive index materials. Therefore, by using these transparent conductive films as a part of the optical film, a multilayer film having both an optical function and a conductive function can be produced in a single step.

  The film quality of a transparent conductive film tends to change depending on the atmosphere at the time of film formation. Before forming the transparent conductive film, a gas released from the plastic substrate is formed by forming a thin film having a water vapor barrier property. The influence by is suppressed. In addition, by using the thin film having the water vapor barrier property as an optical film, the number of processes is reduced as compared with a multilayer film in which the thin film having the water vapor barrier property is separately formed, and an improvement in yield can be expected.

  In addition, it is possible to prevent material deterioration by using it as a sealing electrode material for devices such as LCDs and organic ELs that need to seal materials that may be deteriorated by water vapor or oxygen, such as metal materials and organic substances. It becomes.

  By forming a hard coat, a surface smooth layer, an oligomer precipitation preventing layer, and an antifouling layer, each function can be further imparted to the multilayer film.

  Furthermore, it becomes possible to improve the handling in a process and a product specification by making this multilayer film into the laminated body which affixed on another film, a plastic substrate, and a glass substrate.

  By applying a multilayer film or a laminate to an electronic device, it is possible to manufacture an electronic device having a simpler configuration with fewer steps.

  In manufacturing the multilayer film, by using a film forming apparatus having a plurality of film forming sources and a roll-to-roll mechanism, the multilayer film can be manufactured without repeating the steps of air release and evacuation.

1 is a cross-sectional view of a multilayer film in which a hard coat is formed on one surface of a transparent resin substrate and a three-layer optical film and a transparent conductive film are formed on the opposite surface. Cross section of a multilayer film in which a hard coat, an antireflection optical film, and an antifouling layer are formed on one surface of a transparent resin substrate, and a three-layer optical film and a transparent conductive film are formed on the other surface through a smooth layer FIG. A cross-sectional view of a laminate in which a multilayer film in which an optical film and a transparent conductive film are formed on one surface of a transparent resin substrate and a film in which a hard coat is formed on another transparent resin substrate are attached using an adhesive layer is there. It is sectional drawing of the winding-type film-forming apparatus which forms a ceramic thin film on the film base material unwound from the roll, and winds around a roll, what is called roll-to-roll conveyance.

  The best mode for carrying out the present invention will be described below with reference to the drawings.

  In the schematic diagram of FIG. 1, a hard coat 12 is applied to one surface of a transparent resin substrate 11, a first thin film layer 13 having a refractive index of 1.50 to 2.20, and a second film having a refractive index of 1.35 to 1.50. A multilayer film 10 on which an optical film up to the third thin film layer 15 of a transparent conductive film having a refractive index of 1.90 to 2.20 is formed.

  The plastic film used as the transparent resin substrate 11 used in the present invention is not particularly limited as long as it has sufficient strength in the film forming step and the subsequent step and has good surface smoothness. For example, a polyethylene terephthalate film, Examples include polybutylene terephthalate film, polyethylene naphthalate film, polycarbonate film, polyethersulfone film, polysulfone film, polyarylate film, cyclic polyolefin film, and polyimide. In particular, when applied to a display device front plate, polycarbonate and polyethersulfone having excellent transparency and heat resistance are preferably used. The thickness is about 10 to 200 μm in consideration of the thinning of the member and the flexibility of the base material. Various known additives and stabilizers such as an antistatic agent, an anti-ultraviolet agent, a plasticizer, a lubricant, and an easy-adhesive agent may be used on the surface of these substrates. In order to improve the adhesion to the thin film, pretreatment may be performed by corona treatment, low temperature plasma treatment, ion bombardment treatment, chemical treatment, or the like.

  As the optical films 13 to 15, materials such as oxides, sulfides, fluorides, and nitrides can be used. The thin film made of the above inorganic compound has a different refractive index depending on the material, and the optical characteristics can be adjusted by forming a ceramic thin film having a different refractive index with a specific film thickness.

Multilayer films can increase or decrease the transmittance or reflectance of specific wavelength regions by causing interference between layers. For this purpose, the refractive index and film thickness of these layers must be reduced. Must be within a certain range.
For example, when a material having a refractive index of more than 1.50 of the second thin film layer is used or when a film thickness exceeding 40 nm is deposited, the transmitted light increases and a yellowish film is obtained. Conversely, if a refractive index material lower than 1.35 is used, or if the film thickness is less than 10 nm, the total light transmittance is reduced, and the effect of the second thin film layer cannot be obtained. It is unsuitable to make it thick.
For the first thin film layer, a material less than the chemical theory is often used from the viewpoint of improving the adhesion between the resin substrate and the thin film layer. In this case, if the film thickness exceeds 10 nm, the transmittance decreases and the film thickness is less than 1 nm. In this case, the area deposited on the surface of the resin substrate is insufficient, and the adhesiveness is lowered.

  Materials having a low refractive index include magnesium oxide (1.6), silicon dioxide (1.5), magnesium fluoride (1.4), calcium fluoride (1.3 to 1.4), cerium fluoride ( 1.6), aluminum fluoride (1.3), and the like. Moreover, as a material with a high refractive index, titanium oxide (2.4), zirconium oxide (2.4), zinc sulfide (2.3), tantalum oxide (2.1), zinc oxide (2.1), Examples include indium oxide (2.0), niobium oxide (2.3), and tantalum oxide (2.2). However, the numerical value in the parenthesis represents the refractive index.

  Examples of the material having the barrier performance among the materials of the thin film layer include silicon, aluminum oxide, nitride, and oxynitride, but are not particularly limited. On the other hand, barrier performance can also be improved by a method of forming a dense thin film by treating the thin film with heat or plasma during or after the formation of the thin film layer. The effect can be enhanced by applying a bias to the resin substrate during the plasma treatment.

  As a manufacturing method of the optical film and the transparent conductive film in the present invention, any film forming method may be used as long as the film thickness can be controlled, and the dry method is excellent for producing a thin film. For this, a vacuum vapor deposition method, a physical vapor deposition method such as sputtering, or a chemical vapor deposition method such as a CVD method can be used. In particular, in order to form a thin film having a uniform film quality over a large area, a sputtering method in which the process is stable and the thin film becomes dense is desirable.

Examples of the transparent conductive film 15 include indium oxide, zinc oxide, and tin oxide, or two or three kinds of mixed oxides thereof, and those to which other additives are added. -Various materials can be used depending on the application, and are not particularly limited. At present, the most reliable and proven material is indium tin oxide (ITO).
Further, the surface resistance value of the transparent conductive film 15 is preferably 150 Ω / □ or more from the viewpoint of light transmittance with respect to the surface resistance value of the transparent conductive film, and is 800 Ω / □ or less from the viewpoint of film durability. It is desirable to be.

  When using indium tin oxide (ITO), which is the most common transparent conductive film, the content ratio of tin oxide doped in indium oxide is selected at an arbitrary ratio according to the specifications required for the device. For example, a sputtering target material used to crystallize a thin film for the purpose of increasing mechanical strength desirably has a tin oxide content of less than 10% by weight. In order to make the thin film amorphous and flexible, it is necessary to use tin oxide. The content ratio is desirably 10% by weight or more. Further, when low resistance is required for the thin film, the content ratio of tin oxide is desirably in the range of 3 wt% to 20 wt%.

The film quality of a transparent conductive film tends to change depending on the atmosphere at the time of film formation. Before forming the transparent conductive film, a gas released from the plastic substrate is formed by forming a thin film having a water vapor barrier property. The influence by is suppressed. In addition, by using the thin film having the water vapor barrier property as an optical film, the number of processes is reduced as compared with a multilayer film in which the thin film having the water vapor barrier property is separately formed, and an improvement in yield can be expected.
The water vapor transmission rate can be measured by a method represented by JIS-Z0208 or JIS-Z7129. As for the water vapor transmission rate, under an environment of 40 ° C and 90% Rh, before forming the outermost transparent conductive film, about 1.5 g / m2 ・ day or less, with the transparent conductive film formed, 1.0 g / m2 ・ day The following is desirable.
When the water vapor transmission rate exceeds 1.0 g / m2 · day, when the device is used in a poor environment of high temperature and humidity, water vapor passes through the laminated film into the device, causing malfunction due to short circuit in the device due to condensation. If it has a serious impact that leads to the destruction of the device.
Further, when used as an electrode of an organic device such as an organic EL, it is easily corroded by water molecules, and the device does not function early.
Therefore, considering the effect on the device, the lower the water vapor transmission rate, the better. However, when the transparent conductive film is formed, if it is 1.0 g / m2 · day or less, there is little performance variation. A transparent conductive film with good properties can be formed.

  The hard coat layer 12 is not particularly limited as long as it has transparency, appropriate hardness, and mechanical strength. A curable resin or a thermosetting resin by irradiation with ionizing radiation or ultraviolet rays can be used, and an ultraviolet irradiation curable acrylic or organosilicon resin or a thermosetting polysiloxane resin is particularly preferable. Since the second thin film layer is a low refractive index material, it is more preferable that these resins have the same or slightly higher refractive index than the transparent resin substrate 21. If the film thickness is 3 μm or more, the strength is sufficient, but the range of 3 to 7 μm is preferable from the viewpoint of transparency, coating accuracy, and handling.

  In the schematic diagram of FIG. 2, a hard coat 22, an antireflection optical film (thin film layers 23 to 26), and an antifouling layer 27 are formed on one surface of a transparent resin substrate 21, and a smooth layer 28 is formed on the other surface. The multilayer film 20 is formed by sequentially forming optical films (thin film layers 29 to 31 and the thin film layer 31 is a transparent conductive film).

The antireflection optical film is usually provided with an antireflection function by forming thin films having different refractive indexes. A high refractive index thin film having a refractive index of 1.90 to 2.50 is formed from a single layer formed by forming an inorganic thin film having a refractive index lower than that of the substrate by vacuum film formation or by applying an ultraviolet irradiation curable resin. There are various types including low-refractive-index thin films having a refractive index of 1.30 to 1.50, which are formed by forming a plurality of layers on a transparent resin substrate. A low reflection characteristic can be realized.
The average reflectance at a wavelength of 380 to 780 nm when measured by excluding the reflection of the surface on which the transparent conductive film is formed of the formed antireflection optical film is preferably 2% or less in order to ensure visibility. . The reason is,

  The smooth layer 28 is applied for the purpose of improving the smoothness of the surface of the transparent conductive film 32 by forming an optical film before film formation. The antifouling layer 27 is formed for the purpose of making the surface difficult to get dirty.

  The material for forming the smooth layer 28 may be any material having transparency, appropriate hardness, and mechanical strength, and examples thereof include resin materials such as acrylic resins, organic silicone resins, and polysiloxanes. In the wet process, coating can be performed using various coating methods such as microgravure and screen. Further, when coating the organic layer, it is possible to increase the hardness and make it easy to lubricate by mixing a resin filler or an inorganic filler in the coating solution. On the other hand, the method for forming the protective layer by the organic vapor deposition method is not particularly limited. For example, acrylate or methacrylate or a mixed resin solution thereof is evaporated by an organic vapor deposition apparatus and condensed on a film on a coating drum. Then, a protective layer can be formed by performing a hardening process with an electron beam irradiation apparatus. Further, ultraviolet curing may be used instead of electron beam curing.

  The antifouling layer 27 is water-repellent and / or oil-repellent, thereby protecting the surface and further improving the antifouling property. Any material can be used as long as it satisfies the required performance. It is not something. As a typical example, an organic compound, preferably a fluorine-containing organic compound is suitable. For example, a compound having a hydrophobic group is preferable as a material exhibiting water repellency, and fluorocarbon, perfluorosilane, and the like, and these polymer compounds are suitable.

  These materials can be formed using various coating methods such as a vacuum film forming process such as a vacuum vapor deposition method and a plasma CVD method, and a wet process such as microgravure and screen printing depending on the material. When used in an optical device, the film thickness must be set so as not to impair the optical function, and is preferably 50 nm or less, more preferably 10 nm or less.

  3 schematically shows a multilayer film 40 in which an optical film (thin film layers 42 to 44, and the thin film layer 44 is a transparent conductive film) is formed on one surface of a transparent resin substrate 41, and another transparent substrate 46 is hard. A laminated body 48 in which a film on which a coat 47 is formed is attached using an adhesive layer 45.

  Another transparent substrate 46 can be appropriately selected from the same resin film, plastic substrate, and glass substrate as the transparent resin substrate 41. By using a flexible resin film, the multilayer film 40 wound in a roll shape and the adhesive 45 can be laminated and wound on a roll.

  The schematic diagram of FIG. 4 shows a winding-type vacuum film forming apparatus 50 that forms a ceramic thin film on a film base material unwound from a roll and winds the film on a roll, so-called roll-to-roll conveyance.

  It has a film forming unit (55a to 55e) and a film forming chamber (56a to 56e) capable of forming a thin film in a vacuum chamber. Laminate. For the film formation process of materials with slow film formation speed, two or more film formation units are provided, and by matching with the other film formation speed process, multiple ceramic thin film layers are formed inline at once. It is also possible to do. When depositing multiple thin films at once, conductance between deposition chambers should be as small as possible so that impurities and deposition gas are not mixed with each other in each thin film layer. It is preferable that a differential pressure between the film forming chambers can be 1: 100 or more by providing an intermediate chamber with a pump attached between the chambers.

  Next, the present invention will be described in detail with specific examples.

  As shown in FIG. 1, a dual magnetron sputtering (DMS) method is used on a surface opposite to the hard coat forming surface of a polyethylene terephthalate (188 μm, 1000 mm width) substrate having a hard coat having a thickness of 3 μm formed on one side. A multilayer film was prepared in which a SiOx (1 <x <2) thin film having a refractive index of 1.70 was formed to 3 nm, a SiO2 thin film having a refractive index of 1.45 was formed to 18 nm, and an ITO thin film having a refractive index of 1.98 was formed to 20 nm. Since high energy ions were incident on the thin film during the film formation, a dense film was formed.

  The water vapor transmission rate of the produced multilayer film was measured and found to be 0.5 g / m 2 · day. A multilayer film having a surface resistance of 310Ω / □ and a total light transmittance of 89.1% was obtained. When the variation in the surface resistance value was confirmed, a good film with a standard deviation of 7.5 was obtained.

SiOx (1 <x <2) with a refractive index of 1.70 by vacuum deposition on the opposite side of the hard coat formation surface of a resin substrate with a 3μm thick hard coat on one side of 188μm polyethylene terephthalate A multilayer film was produced in which a thin film of 3 nm, a refractive index of 1.45 SiO2 thin film of 30 nm, and a refractive index of 1.98 ITO thin film of 20 nm were formed. At this time, using a device in which the magnetic field balance of the cathode was adjusted, high energy ions were incident on the thin film to form a dense film.
Then, a touch panel was formed by placing the multilayer film as an upper electrode and a transparent conductive film facing the glass substrate through a spacer on a lower electrode in which ITO was formed on the glass substrate.

The water vapor transmission rate of the produced multilayer film was measured and found to be 0.3 g / m 2 · day. A multilayer film having a surface resistance of 250Ω / □ and a total light transmittance of 88.5% was obtained. When the linearity of the manufactured touch panel was measured, it showed a good characteristic of 0.8%.
In addition, even after leaving the touch panel in an environment of 60 ° C and 90% RH for 1000 hours, there was no problem with the operation of the touch panel.

Comparative Example 1

  A polyethylene terephthalate (188μm, 1000mm width) substrate with a 3μm thick hard coat formed on one side has a refractive index of 1.45 nm with a refractive index of 1.45 on a surface opposite to the hard coat forming surface by vacuum deposition. A multilayer film with a 1.98 ITO thin film formed to 20 nm was prepared.

The water vapor transmission rate of the produced multilayer film was measured and found to be 3.0 g / m 2 · day. A multilayer film having a surface resistance value of 430Ω / □ and a total light transmittance of 88.7% was obtained. However, when the variation in the surface resistance value was confirmed, it was a film having a large surface resistance distribution with a standard deviation of 29.3.
Furthermore, a touch panel was produced using the produced multilayer film, left in an environment of 60 ° C. and 90% RH for 1000 hours, and then taken out to room temperature. As a result, dew condensation was observed inside the touch panel. When the operation of the touch panel was confirmed with normal keystroke weight (250gf), it was confirmed that the ON / OFF switching time was longer than usual and the OFF signal could not be obtained (short).

DESCRIPTION OF SYMBOLS 10 ... Multilayer film 11 ... Transparent resin substrate 12 ... Hard coat 13 ... 1st thin film layer 14 ... 2nd thin film layer 15 ... 3rd thin film layer, transparent conductive film 20 ... Multilayer film 21 ... Transparent resin substrate 22 ... hard coat 23 ... optical thin film 24 ... optical thin film 25 ... optical thin film 26 ... optical thin film 27 ... antifouling layer 28 ... smooth layer 29 ... first thin film layer 30 ... second thin film layer 31 ... third thin film layer, Transparent conductive film 40 ... multilayer film 41 ... transparent resin substrate 42 ... first thin film layer 43 ... second thin film layer 44 ... third thin film layer, transparent conductive film 45 ... adhesive layer 46 ... other transparent substrate 47 ... Hard coat 48 ... Laminate 50 ... Winding type vacuum film forming apparatus 51 ... Unwinding roll 52 ... Winding roll 53 ... Free roll 54 ... Transparent resin substrates 55a to e ... Film forming units 56a to e ... Film forming chamber 57 ... Cooling drum

Claims (9)

  1. A multilayer film having an optical film having a refractive index different from that of the resin substrate on at least one surface of a transparent resin substrate, and having a transparent conductive film as an outermost layer,
    The optical film includes, in order from a layer close to a transparent resin substrate, a first thin film layer having a refractive index n1 of 1.50 to 1.70 and a film thickness d1 of 1 to 10 nm, and a refractive index n2 of 1.35. A second thin film layer having a thickness d2 of 10 to 40 nm at ˜1.50,
    The transparent conductive film is composed of a third thin film layer having a refractive index n3 of 1.90 to 2.20 and a film thickness d3 of 10 to 30 nm.
    The multilayer film, wherein the multilayer film has a water vapor transmission rate at 40 ° C. and 90% Rh of 1.0 g / m 2 · day or less.
  2. The multilayer film according to claim 1 , wherein a metal suboxide layer is formed on the resin substrate side of the first thin film layer.
  3. The said transparent conductive film consists of an oxide which uses at least one of In, Zn, and Sn as a main raw material, and the surface resistance value is the range of 150-800 ohms / square, The Claim 1 or 2 characterized by the above-mentioned. Multilayer film.
  4. One side or the hard coat on both surfaces of the transparent resin substrate, the surface smooth layer, of the oligomer precipitation-preventing layer, the multilayer film according to any one of claims 1 to 3, wherein at least one layer is formed .
  5. A thin film is laminated on the surface of the transparent resin substrate opposite to the side on which the transparent conductive film is formed so as to reduce reflection in the visible light region, and reflection on the surface on which the transparent conductive film is formed is excluded. The multilayer film according to any one of claims 1 to 4 , wherein an average reflectance at a wavelength of 380 to 780 nm when measured is 2% or less.
  6. The multilayer film according to any one of claims 1 to 5, wherein an antifouling layer is formed on the outermost surface of the surface opposite to the surface on which the transparent conductive film of the transparent resin substrate is formed. .
  7.   A laminate comprising the multilayer film according to any one of claims 1 to 6 and another film, a plastic substrate, and a glass substrate bonded together using means such as an adhesive and an adhesive.
  8. An electronic device using the multilayer film or laminate according to any one of claims 1 to 7 .
  9. The method for producing a multilayer film according to any one of claims 1 to 6 , wherein a plurality of targets are arranged in a vacuum device, a transparent resin substrate is continuously unwound from a roll, and the atmosphere in the device is air. A method for producing a multilayer film, comprising forming an optical film and a transparent conductive film without releasing the film, and finally winding the film on a roll.
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US10183466B2 (en) 2014-11-20 2019-01-22 Nitto Denko Corporation Transparent electroconductive film with protective film

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