WO2013141374A1 - Light-transmitting electroconductive film, method for producing same, and use therefor - Google Patents
Light-transmitting electroconductive film, method for producing same, and use therefor Download PDFInfo
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- WO2013141374A1 WO2013141374A1 PCT/JP2013/058337 JP2013058337W WO2013141374A1 WO 2013141374 A1 WO2013141374 A1 WO 2013141374A1 JP 2013058337 W JP2013058337 W JP 2013058337W WO 2013141374 A1 WO2013141374 A1 WO 2013141374A1
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- WIPO (PCT)
- Prior art keywords
- layer
- light
- light transmissive
- optical adjustment
- conductive film
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D11/00—Producing optical elements, e.g. lenses or prisms
- B29D11/0074—Production of other optical elements not provided for in B29D11/00009- B29D11/0073
- B29D11/00788—Producing optical films
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D11/00—Producing optical elements, e.g. lenses or prisms
- B29D11/0073—Optical laminates
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
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- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06F—ELECTRIC DIGITAL DATA PROCESSING
- G06F3/00—Input arrangements for transferring data to be processed into a form capable of being handled by the computer; Output arrangements for transferring data from processing unit to output unit, e.g. interface arrangements
- G06F3/01—Input arrangements or combined input and output arrangements for interaction between user and computer
- G06F3/02—Input arrangements using manually operated switches, e.g. using keyboards or dials
- G06F3/0202—Constructional details or processes of manufacture of the input device
-
- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06F—ELECTRIC DIGITAL DATA PROCESSING
- G06F3/00—Input arrangements for transferring data to be processed into a form capable of being handled by the computer; Output arrangements for transferring data from processing unit to output unit, e.g. interface arrangements
- G06F3/01—Input arrangements or combined input and output arrangements for interaction between user and computer
- G06F3/03—Arrangements for converting the position or the displacement of a member into a coded form
- G06F3/041—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means
- G06F3/044—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means by capacitive means
- G06F3/0445—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means by capacitive means using two or more layers of sensing electrodes, e.g. using two layers of electrodes separated by a dielectric layer
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/13338—Input devices, e.g. touch panels
Definitions
- the present invention relates to a light-transmitting conductive film, a manufacturing method thereof, and an application thereof.
- a light-transmitting conductive layer containing indium oxide is disposed on at least one surface of a light-transmitting support layer made of plastic or the like, directly or via another layer. Many such light-transmitting conductive films are used.
- the light-transmitting conductive layer may be arranged as a grid-like electrode, if the grid-like structure is visible from the user's viewpoint, the visibility as a touch panel is impaired, which is not preferable. Note that the fact that such a phenomenon has been eliminated is sometimes referred to as “index matching is good”.
- the light transmissive conductive film is exposed to a predetermined chemical treatment. Therefore, the light-transmitting conductive film having poor chemical resistance has a problem that it is damaged by chemical treatment in the manufacturing process.
- the electrode having the above-described lattice shape or the like when forming the electrode having the above-described lattice shape or the like, a so-called etching process is performed in which the light-transmitting conductive layer is removed only in a predetermined region by chemical treatment, and as a result Forming a shaped electrode has been performed. Accordingly, the light-transmitting conductive film that is difficult to be etched by the etching process (that is, the light-transmitting conductive layer is difficult to be removed in a desired region) has low production efficiency in the process of manufacturing the touch panel, and is easily etched excessively.
- the light-transmitting conductive layer is removed unintentionally even in a region different from the desired region.
- a light-transmitting conductive film With a light-transmitting conductive film, it is difficult to form the light-transmitting conductive layer into a desired shape. There are problems such as.
- the present invention relates to a light-transmitting conductive film comprising (A) a light-transmitting support layer, (B) an optical adjustment layer, and (C) a light-transmitting conductive layer containing indium oxide. , (2) To improve the balance between chemical resistance and (3) etching property.
- the inventors of the present invention have made extensive studies, adopting an optical adjustment layer (B) containing zirconia and having a thickness of 0.4 to 3 ⁇ m, and the entire film in the XRD measurement by the thin film method.
- the present invention has been completed by further various studies based on this new knowledge, and is as follows.
- Item 1 (A) a light transmissive support layer; (B) an optical adjustment layer; and (C) a light-transmitting conductive layer containing indium oxide,
- the optical adjustment layer (B) is disposed on at least one surface of the light transmissive support layer (A) directly or via one or more other layers, and the light transmissive conductive layer (C ) Is a light transmissive conductive film disposed on at least one surface of the light transmissive support layer (A) via at least the optical adjustment layer (B):
- a ratio of the (222) plane to the peak is 0.1 to 1.0.
- Item 2 Item 2.
- Item 3 Item 3.
- Item 4 Item 4.
- Item 5 Item 5.
- Item 6 Item 6.
- Item 7 Item 7.
- a touch panel comprising the light transmissive conductive film according to any one of Items 1 to 6.
- index matching index matching, (2) chemical resistance, and (3) an improved balance of etching properties
- A a light transmissive support layer
- B an optical adjustment layer
- C A light-transmitting conductive film containing a light-transmitting conductive layer containing indium oxide
- the first optical adjustment layer (B), the undercoat layer (D) and the light transmissive conductive layer (C) are arranged in this order on one surface of the light transmissive support layer (A), and It is sectional drawing which shows the translucent conductive film of this invention by which the 2nd optical adjustment layer (B) is directly arrange
- the light transmissive conductive film of the present invention comprises: (A) a light transmissive support layer; (B) an optical adjustment layer; and (C) a light-transmitting conductive layer containing indium oxide,
- the optical adjustment layer (B) is disposed on at least one surface of the light transmissive support layer (A) directly or via one or more other layers, and the light transmissive conductive layer (C ) Is a light transmissive conductive film disposed on at least one surface of the light transmissive support layer (A) via at least the optical adjustment layer (B):
- the light-transmitting conductive film is characterized in that the ratio of the (222) plane to the peak is 0.1 to 1.0.
- light-transmitting means having a property of transmitting light (translucent).
- Light transmissivity includes transparency.
- Light transmissivity means, for example, the property that the total light transmittance is 80% or more, preferably 85% or more, more preferably 87% or more. In the present invention, the total light transmittance is measured based on JIS-K-7105 using a haze meter (trade name: NDH-2000 manufactured by Nippon Denshoku Co., Ltd. or equivalent).
- the light transmissive support layer (A) is used as a reference.
- One layer having a large distance from the light transmissive support layer (A) is referred to as “upper layer” and the like, and the other layer having a small distance from the light transmissive support layer (A) is referred to as “lower layer”. And so on.
- each layer is determined using a commercially available reflection spectral film thickness meter (Otsuka Electronics, FE-3000, or equivalent).
- the thickness of each layer may be obtained by observation using a commercially available transmission electron microscope.
- the light-transmitting conductive film is thinly cut in a direction perpendicular to the film surface using a microtome or a focus ion beam, and the cross section is observed.
- FIG. 1 shows an embodiment of the light-transmitting conductive film of the present invention.
- the optical adjustment layer (B) and the light transmissive conductive layer (C) are arranged in this order on one surface of the light transmissive support layer (A).
- FIG. 2 shows another embodiment of the light transmissive conductive film of the present invention.
- the optical adjustment layer (B) and the light transmissive conductive layer (C) are arranged in this order on both surfaces of the light transmissive support layer (A).
- the light transmissive support layer refers to a light transmissive conductive film containing a light transmissive conductive layer, which plays a role of supporting the layer containing the light transmissive conductive layer. Although it does not specifically limit as a light transmissive support layer (A), For example, in the light transmissive conductive film for touch panels, what is normally used as a light transmissive support layer can be used.
- the material of the light transmissive support layer (A) is not particularly limited, and examples thereof include glass and various organic polymers.
- the organic polymer is not particularly limited.
- examples include resins, polyamide resins, polyvinyl chloride resins, polyacetal resins, polyvinylidene chloride resins, and polyphenylene sulfide resins.
- polyester-type resin For example, a polyethylene terephthalate (PET), a polyethylene naphthalate (PEN), etc. are mentioned.
- the material of the light transmissive support layer (A) is preferably a polyester resin, and particularly preferably PET.
- the light transmissive support layer (A) may be composed of any one of these, or may be composed of a plurality of types.
- the thickness of the light transmissive support layer (A) is not particularly limited, and examples thereof include a range of 2 to 300 ⁇ m.
- the optical adjustment layer (B) is disposed directly or via one or more other layers on at least one surface of the light transmissive support layer (A).
- the optical adjustment layer (B) is preferably disposed directly on the surface of the light transmissive support layer (A).
- One layer of the optical adjustment layer (B) may be disposed.
- two or more layers may be arranged adjacent to each other or separated from each other via other layers.
- the optical adjustment layer (B) may be directly disposed on both surfaces of the light transmissive support layer (A).
- the optical adjustment layer located below has a higher refractive index than the optical adjustment layer located above. Also good.
- an optical interference action is generated between two layers having different refractive indexes, which is preferable because the transmittance of the light-transmitting conductive film is improved.
- the optical adjustment layer refers to a layer that plays a role of improving the transmittance of the light transmissive film by optical interference.
- an optical adjustment layer B
- what is normally used as an optical adjustment layer in the transparent conductive film for touchscreens can be used.
- the optical adjustment layer (B) contains zirconia.
- the zirconia contained in the optical adjustment layer (B) is preferably in the form of particles, more preferably the average particle size is 10 to 40 nm, and still more preferably the average particle size is 10 to 30 nm.
- the average particle size of zirconia is smaller than 40 nm, the etching property is further improved, and when it is larger than 10 nm, the dispersibility is further improved and the workability is further improved.
- XRD measurement by the thin film method is performed as follows.
- the X-ray diffractometer is measured by a thin film method using a Rigaku thin film evaluation sample horizontal X-ray diffractometer SmartLab or equivalent.
- a parallel beam optical arrangement is used, and CuK ⁇ rays (wavelength: 1.54186 ⁇ ) are used as a light source at a power of 40 kV and 30 mA.
- the incident side slit system uses a solar slit of 5.0 °, a height control slit of 10 mm, and an incident slit of 0.1 mm, and the light receiving side slit has a parallel slit analyzer (PSA) of 0.114 deg. Is used.
- PSA parallel slit analyzer
- the detector uses a scintillation counter.
- the sample stage uses a porous adsorption sample holder, and a sample is adsorbed and fixed by a pump.
- the incident angles are 0.40 °, 0.45 °, 0.55 °, and 0.60 °.
- the result that the peak of interest is the strongest is adopted.
- the step interval and the measurement speed are appropriately adjusted so that the X-ray diffraction pattern can be recognized.
- measurement is performed at a step interval of 0.01 ° and a measurement speed of 3.0 ° / min.
- the measurement range is 10 ° to 60 °.
- the obtained X-ray diffraction pattern does not need to be monochromatic, and each peak intensity uses a value obtained by subtracting the background.
- the average particle diameter of zirconia is determined by observation with a transmission electron microscope. Specifically, a light-transmitting conductive film is cut into thin pieces using a microtome or a focus ion beam, and the cross section is observed. Thus, the length in the long axis direction of 14 particles obtained by removing the upper 3 particles and the lower 3 particles in the long axis direction length from 20 randomly selected particles that can be visually recognized. Is the average particle diameter.
- observation is performed in different regions of the same sample.
- the zirconia particles cannot be distinguished from other particles, the particles are subjected to elemental analysis by EDX or EELS to identify the zirconia particles.
- the thickness of the optical adjustment layer (B) is 0.4 to 3 ⁇ m, preferably 0.5 to 2.5 ⁇ m, more preferably 1 to 2 ⁇ m.
- the index matching property is further improved.
- it is larger than 0.4 ⁇ m a peak derived from zirconia can be confirmed more easily, and the index matching property is further improved.
- the thickness of the optical adjustment layer (B) is measured as follows. Obtained by observation with a transmission electron microscope. Specifically, a light-transmitting conductive film is cut into thin pieces using a microtome or a focus ion beam, and the cross section is observed.
- the optical adjustment layer (B) is preferable when the average surface roughness Ra on the surface opposite to the light-transmitting support layer (A) is 0.4 to 2.0 nm in terms of etching property. It is more preferably 5 to 1.8 nm, and further preferably 0.5 to 1.5 nm.
- the average surface roughness Ra means an arithmetic average of roughness measured using a scanning probe microscope.
- the average surface roughness Ra in the present invention can be measured using a commercially available scanning probe microscope (Shimadzu Corporation, SPM-9700, or equivalent), and a 1 ⁇ m square measurement surface in a predetermined contact mode. It is a value obtained by averaging absolute deviations from an average line obtained by scanning with a probe (OMLY-TR800-PSA-1, spring constant 0.15 N / m, manufactured by OLYMPUS).
- the optical adjustment layer (B) is not particularly limited as long as the effects of the present invention are exhibited, but may further contain other components in addition to zirconia.
- the other components are not particularly limited as long as the effects of the present invention are exhibited.
- acrylic resins, silicone resins, melamine resins, and alkyd resins and colloidal particles such as silica, zirconia, titania, and alumina. Etc.
- the optical adjustment layer (B) may further contain any one of them, or may further contain a plurality of types.
- the content ratio of zirconia in the whole is not particularly limited as long as the effect of the present invention is exhibited, but is preferably 20% by weight or more. is there.
- the method of disposing the optical adjustment layer (B) is not particularly limited, and examples thereof include a method of applying to a film and curing with heat, and a method of curing with active energy rays such as ultraviolet rays and electron beams. . From the viewpoint of productivity, a method of curing with ultraviolet rays is preferable.
- the light transmissive conductive layer (C) contains indium oxide.
- the light transmissive conductive layer (C) may further contain a dopant in addition to indium oxide.
- the dopant is not particularly limited, and examples thereof include tin oxide, zinc oxide, cerium oxide, gadolinium oxide, silicon oxide, and titanium oxide. In addition to indium oxide, the light transmissive conductive layer (C) may contain these alone or as a dopant.
- a layer containing indium tin oxide (ITO) can be given as a preferred example at present, but indium oxide containing another dopant as required. A layer containing can also be used.
- Indium tin oxide is indium oxide doped with tin.
- indium tin oxide indium tin oxide obtained by using indium (III) oxide (In 2 O 3 ) and tin (IV) oxide (SnO 2 ) is preferable.
- the addition amount of SnO 2 is not particularly limited, and examples thereof include 1 to 15% by weight, preferably 2 to 10% by weight, and more preferably 3 to 8% by weight.
- the light-transmitting conductive layer (C) may contain a dopant in which another dopant is further added to indium tin oxide in a range where the total amount of dopant does not exceed the numerical range shown on the left. Although it does not specifically limit as another dopant in the left, For example, zinc, cerium, gadolinium, silicon, titanium, etc. are mentioned.
- the light transmissive conductive layer (C) may contain any one of the various indium tin oxides described above, or may contain a plurality of types.
- the light transmissive conductive layer (C) may contain particles containing indium oxide.
- the average particle diameter of the particles is not particularly limited as long as the effect of the present invention is exhibited, but is preferably 3.0 to 8.0 nm in terms of easy reduction in specific resistance, and preferably 3.5 to 6. 5 nm is more preferable, and 3.5 to 6.0 nm is more preferable.
- particles containing indium oxide indium tin oxide particles can be cited as a preferred example at present, but particles of indium oxide containing other dopants can be used as necessary.
- the average particle diameter of the particles containing indium oxide is 0.5 ⁇ m 2 in a predetermined contact mode using a commercially available scanning probe microscope (Shimadzu Corporation, SPM-9700, or equivalent). It is determined from the image obtained by scanning the measurement surface with a probe (OMLY-TR800-PSA-1, spring constant of 0.15 N / m, or equivalent) manufactured by OLYMPUS®. Specifically, particle diameters are classified by 1 nm for particles of 1 nm to 30 nm from the observed image, the number of particles integrated in each particle diameter is examined, and the particle diameter of D50 in the particle size distribution is defined as the average particle diameter. To do.
- the light transmissive conductive layer (C) is not particularly limited, but may be a crystalline or amorphous body, or a mixture thereof.
- the light-transmitting conductive film of the present invention has an improved balance of (1) index matching, (2) chemical resistance, and (3) etching property.
- the light-transmitting conductive layer (C) having the above-mentioned characteristics is obtained by heat treatment of indium oxide (or a mixture of indium oxide and dopant when a dopant is further added; hereinafter, this mixture and indium oxide are collectively referred to as “ It is sometimes referred to as “indium oxide or the like”).
- the conditions for this heat treatment can be appropriately set within the range in which the light-transmitting conductive layer (C) having the above characteristics can be obtained, and are not particularly limited. For example, heating in the atmosphere at 90 to 160 ° C. for 10 to 120 minutes Processing conditions etc. are mentioned. Specifically, heat treatment conditions in the atmosphere at 140 ° C. for 60 minutes can be given.
- the light-transmitting conductive layer (C) has a crystal body such as indium oxide or a mixture of a crystal body such as indium oxide and an amorphous body such as indium oxide.
- the light-transmitting conductive layer (C) having the above characteristics is formed by forming a layer containing indium oxide or the like on the underlying layer, and then in the atmosphere at 90 to 160 ° C., 10 to 10 ° C. It can be obtained by heat treatment for 120 minutes.
- the light transmissive conductive layer (C) is disposed on at least one surface of the light transmissive support layer (A) via at least the optical adjustment layer (B).
- the thickness of the light transmissive conductive layer (C) is 5 to 200 nm, preferably 10 to 100 nm, more preferably 15 to 50 nm. Further, as the light-transmitting conductive film for capacitive type touch panel, the thickness of the light-transmitting conductive layer (C) is 15 to 40 nm, preferably 15 to 38 nm, more preferably 17 to 35 nm.
- the method for forming the light transmissive conductive layer (C) may be either wet or dry.
- the method for forming the light-transmitting conductive layer (C) is not particularly limited, and examples thereof include an ion plating method, a sputtering method, a vacuum deposition method, a CVD method, and a pulse laser deposition method.
- a method for forming the light transmissive conductive layer (C) a sputtering method is preferable.
- the light-transmitting conductive layer (C) is formed by a sputtering method, it is not particularly limited.
- the light transmissive conductive film of the present invention has an undercoat layer directly or via one or more other layers on the surface of the light transmissive support layer (A) where the light transmissive conductive layer (C) is disposed. (D) may be arranged.
- the undercoat layer (D) is disposed, at least one of the light transmissive conductive layers (C) is supported by the light transmissive support through at least the undercoat layer (D) and the optical adjustment layer (B). It is arranged on the surface of the layer (A).
- at least one of the light transmissive conductive layers (C) may be disposed adjacent to the undercoat layer (D).
- the undercoat layer (D) is usually disposed closer to the light transmissive conductive layer (C) than the optical adjustment layer (B).
- FIG. 4 shows one embodiment of the light-transmitting conductive film of the present invention.
- the optical adjustment layer (B), the undercoat layer (D), and the light transmissive conductive layer (C) are arranged adjacent to each other in this order on one surface of the light transmissive support layer (A). ing.
- FIG. 5 shows an embodiment of the light-transmitting conductive film of the present invention.
- the optical adjustment layer (B), the undercoat layer (D), and the light transmissive conductive layer (C) are arranged adjacent to each other in this order on both surfaces of the light transmissive support layer (A). .
- FIG. 6 shows one embodiment of the light-transmitting conductive film of the present invention.
- the first optical adjustment layer (B), the undercoat layer (D), and the light transmissive conductive layer (C) are adjacent to each other in this order on one surface of the light transmissive support layer (A).
- the second optical adjustment layer (B) is directly arranged on the other surface.
- the material of the undercoat layer (D) is not particularly limited, but may be, for example, a dielectric material.
- the material for the undercoat layer (D) is not particularly limited.
- silicon oxide, silicon nitride, silicon oxynitride, silicon carbide, silicon alkoxide, alkylsiloxane and its condensate, polysiloxane, silsesquioxane, and Examples include polysilazane.
- the undercoat layer (D) may be composed of any one of them, or may be composed of a plurality of types. A light-transmitting underlayer containing silicon oxide is preferable, and a light-transmitting underlayer made of silicon oxide is more preferable.
- One layer of the undercoat layer (D) may be disposed.
- two or more layers may be arranged adjacent to each other or separated from each other via other layers.
- Examples of the thickness per layer of the undercoat layer (D) include 15 to 40 nm. When two or more layers are disposed adjacent to each other, the total thickness of all the undercoat layers (D) adjacent to each other may be within the above range. In the example list shown on the left, the following are more preferable than the above.
- the method of disposing the undercoat layer (D) may be either wet or dry, and is not particularly limited.
- the wet include a sol-gel method and a method of applying a fine particle dispersion or colloid solution. It is done.
- the method for disposing the undercoat layer (D) include a method of laminating on an adjacent layer by a sputtering method, an ion plating method, a vacuum deposition method, or a pulse laser deposition method.
- the light-transmitting conductive film of the present invention is provided with the optical adjustment layer (B) and the light-transmitting conductive layer (C) of the light-transmitting support layer (A). On the side surface, at least one layer selected from the group consisting of the undercoat layer (D) and at least one other layer (E) may be further disposed.
- Other layers (E) are not particularly limited, and examples thereof include an adhesive layer.
- the adhesive layer is a layer that is disposed adjacent to each other between the two layers and is disposed to adhere the two layers to each other. Although it does not specifically limit as a contact bonding layer, For example, what is normally used as a contact bonding layer in the transparent conductive film for touchscreens can be used.
- the light-transmitting conductive film of the present invention is preferably used for touch panels.
- the light-transmitting conductive film of the present invention is particularly preferably used for a capacitive touch panel.
- a light-transmitting conductive film used for the production of a resistive film type touch panel is required to have a surface resistivity (sheet resistance) of about 100 to 1,000 ⁇ / sq.
- a light-transmitting conductive film used for manufacturing a capacitive touch panel generally has a lower surface resistivity.
- the light-transmitting conductive film of the present invention has a reduced resistivity, and is thus preferably used for the production of a capacitive touch panel. The details of the capacitive touch panel are as described in 2.
- Capacitive touch panel of the electrostatic capacitance type touch panel ⁇ br/> invention of the present invention comprises a light transmissive, electrically-conductive film of the present invention, comprise other members according to necessity.
- the configuration of the capacitive touch panel according to the present invention include the following configurations.
- the protective layer (1) side is used so that the operation screen side faces, and the glass (5) side faces the side opposite to the operation screen.
- Protective layer (2) Light transmissive conductive film of the present invention (Y-axis direction) (3) Insulating layer (4) Light transmissive conductive film of the present invention (X-axis direction) (5) Glass
- the capacitive touch panel of the present invention is not particularly limited, for example, it can be produced by combining the above (1) to (5) and other members as required according to a usual method. it can.
- the light transmissive conductive film of the present invention can be produced by disposing each layer as described for each layer.
- the light-transmissive support layer (A) may be sequentially disposed on the surface on which the light-transmissive conductive layer (C) is disposed from the lower layer side, but the arrangement order is not particularly limited.
- another layer may be disposed on one surface of a layer that is not the light-transmissive support layer (A) (for example, the light-transmissive conductive layer (C)).
- one composite layer is obtained by arranging two or more layers adjacent to each other on the one hand, or at the same time, two or more layers are similarly disposed adjacent to each other on the other side.
- one type of composite layer may be obtained, and these two types of composite layers may be further arranged adjacent to each other.
- Example 1 An optical adjustment layer of an acrylate resin containing zirconia particles having an average particle diameter of 16 nm was formed on a PET resin substrate (light-transmitting support layer) having a thickness of 125 ⁇ m so as to have a thickness of 0.5 ⁇ m.
- the average particle diameter of zirconia particles was determined by observation with a transmission electron microscope as follows. Specifically, the light transmissive conductive film was covered with a resin, the light transmissive conductive film was thinly cut perpendicularly to the film using a microtome, and the cross section was observed. Thus, the length in the long axis direction of 14 particles obtained by removing the upper 3 particles and the lower 3 particles in the long axis direction length from 20 randomly selected particles that can be visually recognized. The number average value was taken as the average particle size.
- Ra of the optical adjustment layer was 0.7 nm.
- a SiO 2 layer of 20 nm was formed on this optical adjustment layer by sputtering, and indium tin oxide (ITO) was formed to a thickness of 23 nm.
- ITO indium tin oxide
- a light transmissive conductive layer is formed by a DC magnetron sputtering method using a sintered body material made of indium oxide: 95 wt% and tin oxide: 5 wt% as a target material, and heated in the atmosphere. The light-transmitting conductive film of the present invention was finally obtained.
- oxygen gas and argon gas are introduced into the chamber so that the oxygen partial pressure becomes 6.5 ⁇ 10 ⁇ 3 Pa.
- the sputtering process was performed with the chamber internal pressure set to 0.3 to 0.4 Pa. Thereafter, heat treatment was performed in the atmosphere at 140 ° C. for 60 minutes to obtain a light-transmitting conductive film of the present invention. This film was evaluated by XRD and AFM.
- XRD measurement by the thin film method was performed as follows.
- the X-ray diffractometer was measured by a thin film method using a sample horizontal X-ray diffractometer SmartLab for thin film evaluation manufactured by Rigaku.
- a parallel beam optical arrangement was used, and a CuK ⁇ ray (wavelength: 1.54186 ⁇ ) was used as a light source at a power of 40 kV and 30 mA.
- the incident side slit system uses a solar slit of 5.0 °, a height control slit of 10 mm, and an incident slit of 0.1 mm, and the light receiving side slit has a parallel slit analyzer (PSA) of 0.114 deg. Was used.
- PSA parallel slit analyzer
- the detector used was a scintillation counter.
- the sample stage used a porous adsorption sample holder, and the sample was adsorbed and fixed by a pump.
- the incident side was fixed at 0.50 °, the step interval was 0.01 °, the measurement speed was 3.0 ° / min, and the measurement range was 10 ° to 60 °.
- the average particle size of indium tin oxide was measured as follows. Using a scanning probe microscope (Shimadzu Corporation, SPM-9700), probe the 0.5 ⁇ m square measurement surface in a predetermined contact mode (OMCL-TR800-PSA-1 made by OLYMPUS Corp., spring constant 0.15 N) / M) from an image obtained by scanning. Specifically, the particle size is classified by 1 nm for indium tin oxide particles of 1 nm to 30 nm from the observed image, the number of particles integrated in each particle size is examined, and the average particle size of D50 in the particle size distribution is determined. Particle size was used.
- the average particle diameter of indium tin oxide was 6.2 nm.
- Comparative Example 1 An optical adjustment layer of an acrylate resin containing zirconia particles having an average particle diameter of 16 nm was formed to a thickness of 0.2 ⁇ m. Other than that was carried out similarly to Example 1, and obtained the transparent electroconductive film. As a result of evaluation by XRD, no peak derived from zirconia was detected. The average particle diameter of indium tin oxide was 6.8 nm.
- index matching (IM) and etching property were evaluated as follows.
- Evaluation of index matching was performed as follows. In order to form a comb pattern (2 mm width, 10 mm length) in the width direction in the vicinity of the center of the light-transmitting conductive film cut to a width of 5 cm and a length of 10 cm, the following operation was performed. One of four sides of a silicon rubber plate having a width of 5 cm and a length of 5 cm was cut into a comb pattern. The silicon rubber plate is light-transmitting conductive so that the comb-shaped pattern is placed near the center of the light-transmitting conductive film on the ITO side of the light-transmitting conductive film cut to 5 cm wide ⁇ 10 cm long Laminated to film.
- etching resist was applied to the silicon rubber side of the light-transmitting conductive film bonded with silicon rubber, dried at 80 ° C. for 30 minutes, and then the silicon rubber plate was peeled off. As a result, a light-transmitting conductive film in which the ITO surface and the etching resist surface were exposed with the comb pattern as a boundary was obtained. This was immersed in 20% hydrochloric acid for 20 minutes to dissolve ITO. Then, it was ultrasonically treated for 10 minutes while being immersed in a 0.5 M KOH solution, and washed with water to obtain a comb pattern film of ITO. A comb pattern film was placed on white paper and black paper, and the visibility at the edge of the ITO pattern was confirmed. Evaluation was performed as follows.
- the etching property was evaluated as follows.
- the light transmissive conductive film was immersed in 20% hydrochloric acid, and the time until the surface resistance could not be measured was determined.
- the immersion time was set at intervals of 10 seconds from 10 seconds to 90 seconds.
- the etching processing completion time is 40 seconds and 50 seconds, “ ⁇ ”, when 30 seconds, 60 seconds, and 70 seconds, “ ⁇ ”, when 20 seconds and 80 seconds, “ ⁇ ”, 10 seconds, 90 seconds, and More than that was evaluated as “x”. If the etching process time is too short, or conversely too long, it is difficult to control the etching process, which is not preferable.
- the chemical resistance was evaluated as follows.
- the light-transmitting conductive film was immersed in 1% hydrochloric acid for 30 minutes and washed with water.
- the ratio R / R0 of the surface resistance value R at this time and the surface resistance value R0 before being immersed in hydrochloric acid was determined.
- R / R0 is less than 1.1
- “ ⁇ ” when R / R0 is 1.1 or more and less than 1.2
- ⁇ when R / R0 is 1.2 or more and 1.3.
- it was less than “ ⁇ ” it was judged as “X” when R / R0 was 1.3 or more.
- Light-transmissive conductive film 11 Light-transmissive support layer (A) 12 Optical adjustment layer (B) 13 Light transmissive conductive layer (C) 14 Undercoat layer (D)
Abstract
Description
項1
(A)光透過性支持層;
(B)光学調整層;及び
(C)酸化インジウムを含有する光透過性導電層
を含有し、
前記光学調整層(B)が、前記光透過性支持層(A)の少なくとも一方の面に、直接又は一以上の他の層を介して配置されており、かつ
前記光透過性導電層(C)が、前記光透過性支持層(A)の少なくとも一方の面に、少なくとも光学調整層(B)を介して配置されている光透過性導電性フィルムであって:
前記光学調整層(B)が、ジルコニアを含有し、かつ厚さ0.4~3μmであり;かつ
薄膜法によるXRD測定において、ジルコニアに由来する2θ=28°付近のピークの、酸化インジウムに由来する(222)面のピークに対する比が0.1~1.0であることを特徴とする、光透過性導電性フィルム。
項2
前記光学調整層(B)の、光透過性支持層(A)とは反対側の面の平均表面粗さRaが、0.4~2.0nmである、項1に記載の光透過性導電性フィルム。
項3
前記ジルコニアの平均粒子径が、10~40nmである、項1又は2に記載の光透過性導電性フィルム。
項4
前記光透過性導電層(C)が、酸化インジウムを含有する粒子を含有し、当該粒子の平均粒子径が、3.0~8.0nmである、項1~3のいずれかに記載の光透過性導電性フィルム。
項5
前記光透過性導電層(C)が、酸化インジウムを含有する層を大気中90~160℃で10~120分間加熱することにより得られうる、項1~4のいずれかに記載の光透過性導電性フィルム。
項6
光透過性導電層(C)が、酸化インジウムスズを含有する、項1~5のいずれかに記載の光透過性導電性フィルム。
項7
項1~6のいずれかに記載の光透過性導電性フィルムを含有する、タッチパネル。 The inventors of the present invention have made extensive studies, adopting an optical adjustment layer (B) containing zirconia and having a thickness of 0.4 to 3 μm, and the entire film in the XRD measurement by the thin film method. The above problem can be solved by setting the ratio of the peak near 2θ = 28 ° derived from zirconia to the peak of the (222) plane derived from indium oxide to be 0.1 to 1.0. I found it. The present invention has been completed by further various studies based on this new knowledge, and is as follows.
(A) a light transmissive support layer;
(B) an optical adjustment layer; and (C) a light-transmitting conductive layer containing indium oxide,
The optical adjustment layer (B) is disposed on at least one surface of the light transmissive support layer (A) directly or via one or more other layers, and the light transmissive conductive layer (C ) Is a light transmissive conductive film disposed on at least one surface of the light transmissive support layer (A) via at least the optical adjustment layer (B):
The optical adjustment layer (B) contains zirconia and has a thickness of 0.4 to 3 μm; and in XRD measurement by a thin film method, it has a peak around 2θ = 28 ° derived from zirconia and is derived from indium oxide. A ratio of the (222) plane to the peak is 0.1 to 1.0.
Item 2
Item 2. The light transmissive conductive material according to
Item 3
Item 3. The light transmissive conductive film according to
Item 4
Item 4. The light according to any one of
Item 5
Item 5. The light-transmitting layer according to any one of
Item 6
Item 6. The light transmissive conductive film according to any one of
Item 7
Item 7. A touch panel comprising the light transmissive conductive film according to any one of
本発明の光透過性導電性フィルムは、
(A)光透過性支持層;
(B)光学調整層;及び
(C)酸化インジウムを含有する光透過性導電層
を含有し、
前記光学調整層(B)が、前記光透過性支持層(A)の少なくとも一方の面に、直接又は一以上の他の層を介して配置されており、かつ
前記光透過性導電層(C)が、前記光透過性支持層(A)の少なくとも一方の面に、少なくとも光学調整層(B)を介して配置されている光透過性導電性フィルムであって:
前記光学調整層(B)が、ジルコニアを含有し、かつ厚さ0.4~3μmであり;かつ
薄膜法によるXRD測定において、ジルコニアに由来する2θ=28°付近のピークの、酸化インジウムに由来する(222)面のピークに対する比が0.1~1.0であることを特徴とする、光透過性導電性フィルム
である。 1. Light transmissive conductive film The light transmissive conductive film of the present invention comprises:
(A) a light transmissive support layer;
(B) an optical adjustment layer; and (C) a light-transmitting conductive layer containing indium oxide,
The optical adjustment layer (B) is disposed on at least one surface of the light transmissive support layer (A) directly or via one or more other layers, and the light transmissive conductive layer (C ) Is a light transmissive conductive film disposed on at least one surface of the light transmissive support layer (A) via at least the optical adjustment layer (B):
The optical adjustment layer (B) contains zirconia and has a thickness of 0.4 to 3 μm; and in XRD measurement by a thin film method, it has a peak around 2θ = 28 ° derived from zirconia and is derived from indium oxide. The light-transmitting conductive film is characterized in that the ratio of the (222) plane to the peak is 0.1 to 1.0.
本発明において光透過性支持層とは、光透過性導電層を含有する光透過性導電性フィルムにおいて、光透過性導電層を含有する層を支持する役割を果たすものをいう。光透過性支持層(A)としては、特に限定されないが、例えば、タッチパネル用光透過性導電性フィルムにおいて、光透過性支持層として通常用いられるものを用いることができる。 1.1 Light transmissive support layer (A)
In the present invention, the light transmissive support layer refers to a light transmissive conductive film containing a light transmissive conductive layer, which plays a role of supporting the layer containing the light transmissive conductive layer. Although it does not specifically limit as a light transmissive support layer (A), For example, in the light transmissive conductive film for touch panels, what is normally used as a light transmissive support layer can be used.
本発明の光透過性導電性フィルムは、光透過性支持層(A)の少なくとも一方の面に、直接又は一以上の他の層を介して光学調整層(B)が配置されている。光学調整層(B)は、好ましくは光透過性支持層(A)の面に、直接配置されている。 1.2 Optical adjustment layer (B)
In the light transmissive conductive film of the present invention, the optical adjustment layer (B) is disposed directly or via one or more other layers on at least one surface of the light transmissive support layer (A). The optical adjustment layer (B) is preferably disposed directly on the surface of the light transmissive support layer (A).
このような構成を採ることにより、屈折率の異なる二層間に光学干渉作用が生じ、これにより光透過性導電性フィルムの透過率が向上するので好ましい。 When two or more layers of the optical adjustment layer (B) are arranged adjacent to each other, the optical adjustment layer located below has a higher refractive index than the optical adjustment layer located above. Also good.
By adopting such a configuration, an optical interference action is generated between two layers having different refractive indexes, which is preferable because the transmittance of the light-transmitting conductive film is improved.
X線回折装置はRigaku製 薄膜評価用試料水平型X線回折装置SmartLab、又はその同等品を用いて薄膜法にて測定する。平行ビーム光学配置を用い、光源にはCuKα線(波長:1.54186Å)を40kV、30mAのパワーで用いる。入射側スリット系はソーラスリット5.0°、高さ制御スリット10mm、入射スリット0.1mmを用い、受光側スリットにはパラレルスリットアナライザー(PSA)0.114deg.を用いる。検出器はシンチレーションカウンターを用いる。試料ステージは多孔質吸着試料ホルダを用いて、ポンプにより試料を吸着固定する。X線の入射角0.50°で測定し、十分な検出感度が得られない場合には、入射角0.40°、0.45°、0.55°及び0.60°でそれぞれ測定し、目的とするピークが最も強くなる結果を採用する。ステップ間隔及び測定スピードはX線回折パターンを認識できる程度に適宜調整する。好ましくは、ステップ間隔0.01°、測定スピード3.0°/minで測定する。測定範囲を10°~60°で測定する。尚、得られたX線回折パターンについて単色化する必要はなく、各ピーク強度はバックグラウンドを差し引いた値を用いる。 In the present invention, XRD measurement by the thin film method is performed as follows.
The X-ray diffractometer is measured by a thin film method using a Rigaku thin film evaluation sample horizontal X-ray diffractometer SmartLab or equivalent. A parallel beam optical arrangement is used, and CuKα rays (wavelength: 1.54186Å) are used as a light source at a power of 40 kV and 30 mA. The incident side slit system uses a solar slit of 5.0 °, a height control slit of 10 mm, and an incident slit of 0.1 mm, and the light receiving side slit has a parallel slit analyzer (PSA) of 0.114 deg. Is used. The detector uses a scintillation counter. The sample stage uses a porous adsorption sample holder, and a sample is adsorbed and fixed by a pump. When the X-ray incident angle is 0.50 ° and sufficient detection sensitivity is not obtained, the incident angles are 0.40 °, 0.45 °, 0.55 °, and 0.60 °. The result that the peak of interest is the strongest is adopted. The step interval and the measurement speed are appropriately adjusted so that the X-ray diffraction pattern can be recognized. Preferably, measurement is performed at a step interval of 0.01 ° and a measurement speed of 3.0 ° / min. The measurement range is 10 ° to 60 °. The obtained X-ray diffraction pattern does not need to be monochromatic, and each peak intensity uses a value obtained by subtracting the background.
また、ジルコニア粒子と他の粒子との区別がつかない場合は、EDXやEELSにより、粒子の元素分析を行い、ジルコニア粒子を特定する。 In the present invention, the average particle diameter of zirconia is determined by observation with a transmission electron microscope. Specifically, a light-transmitting conductive film is cut into thin pieces using a microtome or a focus ion beam, and the cross section is observed. Thus, the length in the long axis direction of 14 particles obtained by removing the upper 3 particles and the lower 3 particles in the long axis direction length from 20 randomly selected particles that can be visually recognized. Is the average particle diameter. As a result of observation with a transmission electron microscope, when a predetermined amount of particles cannot be visually recognized, observation is performed in different regions of the same sample.
When the zirconia particles cannot be distinguished from other particles, the particles are subjected to elemental analysis by EDX or EELS to identify the zirconia particles.
光透過性導電層(C)は、酸化インジウムを含有する。光透過性導電層(C)は、酸化インジウムに加えてドーパントをさらに含有していてもよい。ドーパントとしては特に限定されないが、例えば、スズ酸化物、亜鉛酸化物、セリウム酸化物、ガドリニウム酸化物、シリコン酸化物及びチタン酸化物等が挙げられる。光透過性導電層(C)は酸化インジウムに加えて、ドーパントとしてこれらを単独で含有していてもよいし、複数種を含有していてもよい。光透過性導電層(C)としては、現状では酸化インジウムスズ(tin-dopedindiumoxide(ITO))を含有する層を好ましい一例として挙げることができるが、必要に応じて他のドーパントを含有する酸化インジウムを含有する層を用いることもできる。 1.3 Light transmissive conductive layer (C)
The light transmissive conductive layer (C) contains indium oxide. The light transmissive conductive layer (C) may further contain a dopant in addition to indium oxide. The dopant is not particularly limited, and examples thereof include tin oxide, zinc oxide, cerium oxide, gadolinium oxide, silicon oxide, and titanium oxide. In addition to indium oxide, the light transmissive conductive layer (C) may contain these alone or as a dopant. As the light-transmitting conductive layer (C), a layer containing indium tin oxide (ITO) can be given as a preferred example at present, but indium oxide containing another dopant as required. A layer containing can also be used.
本発明の光透過性導電性フィルムは、光透過性支持層(A)の光透過性導電層(C)が配置されている面に、直接又は一以上の他の層を介してアンダーコート層(D)が配置されていてもよい。アンダーコート層(D)が配置されている場合、少なくとも一方の前記光透過性導電層(C)が、少なくとも前記アンダーコート層(D)及び光学調整層(B)を介して前記光透過性支持層(A)の前記面に配置されている。この場合、少なくとも一方の前記光透過性導電層(C)が、前記アンダーコート層(D)に隣接して配置されていてもよい。また、この場合、アンダーコート層(D)は通常、光学調整層(B)よりも光透過性導電層(C)に近い側に配置されている。 1.4 Undercoat layer (D)
The light transmissive conductive film of the present invention has an undercoat layer directly or via one or more other layers on the surface of the light transmissive support layer (A) where the light transmissive conductive layer (C) is disposed. (D) may be arranged. When the undercoat layer (D) is disposed, at least one of the light transmissive conductive layers (C) is supported by the light transmissive support through at least the undercoat layer (D) and the optical adjustment layer (B). It is arranged on the surface of the layer (A). In this case, at least one of the light transmissive conductive layers (C) may be disposed adjacent to the undercoat layer (D). In this case, the undercoat layer (D) is usually disposed closer to the light transmissive conductive layer (C) than the optical adjustment layer (B).
本発明の光透過性導電性フィルムは、光透過性支持層(A)の光学調整層(B)及び光透過性導電層(C)が配置されている側の面に、アンダーコート層(D)及び少なくとも1種のその他の層(E)からなる群より選択される少なくとも1種の層がさらに配置されていてもよい。 1.5 Other layers The light-transmitting conductive film of the present invention is provided with the optical adjustment layer (B) and the light-transmitting conductive layer (C) of the light-transmitting support layer (A). On the side surface, at least one layer selected from the group consisting of the undercoat layer (D) and at least one other layer (E) may be further disposed.
本発明の光透過性導電性フィルムは、タッチパネルのために好ましく用いられる。本発明の光透過性導電性フィルムは、特に、静電容量型タッチパネルのためにより好ましく用いられる。抵抗膜方式タッチパネルの製造のために用いられる光透過性導電性フィルムは一般に表面抵抗率(シート抵抗)が100~1,000Ω/sq程度は必要であるとされる。これに対して静電容量型タッチパネルの製造のために用いられる光透過性導電性フィルムは一般に表面抵抗率が低いほうが有利である。本発明の光透過性導電性フィルムは、抵抗率が低減されており、これにより、静電容量型タッチパネルの製造のために好ましく用いられる。静電容量型タッチパネルについて詳細は、2で説明する通りである。 1.6 Use of light-transmitting conductive film of the present invention The light-transmitting conductive film of the present invention is preferably used for touch panels. The light-transmitting conductive film of the present invention is particularly preferably used for a capacitive touch panel. In general, a light-transmitting conductive film used for the production of a resistive film type touch panel is required to have a surface resistivity (sheet resistance) of about 100 to 1,000 Ω / sq. On the other hand, a light-transmitting conductive film used for manufacturing a capacitive touch panel generally has a lower surface resistivity. The light-transmitting conductive film of the present invention has a reduced resistivity, and is thus preferably used for the production of a capacitive touch panel. The details of the capacitive touch panel are as described in 2.
本発明の静電容量型タッチパネルは、本発明の光透過性導電性フィルムを含み、さらに必要に応じてその他の部材を含んでなる。 2. Capacitive touch panel of the electrostatic capacitance type touch panel <br/> invention of the present invention comprises a light transmissive, electrically-conductive film of the present invention, comprise other members according to necessity.
(1)保護層
(2)本発明の光透過性導電性フィルム(Y軸方向)
(3)絶縁層
(4)本発明の光透過性導電性フィルム(X軸方向)
(5)ガラス
本発明の静電容量型タッチパネルは、特に限定されないが、例えば、上記(1)~(5)、並びに必要に応じてその他の部材を通常の方法に従って組み合わせることにより製造することができる。 Specific examples of the configuration of the capacitive touch panel according to the present invention include the following configurations. The protective layer (1) side is used so that the operation screen side faces, and the glass (5) side faces the side opposite to the operation screen.
(1) Protective layer (2) Light transmissive conductive film of the present invention (Y-axis direction)
(3) Insulating layer (4) Light transmissive conductive film of the present invention (X-axis direction)
(5) Glass Although the capacitive touch panel of the present invention is not particularly limited, for example, it can be produced by combining the above (1) to (5) and other members as required according to a usual method. it can.
本発明の光透過性導電性フィルムは、それぞれの層について説明した通りそれぞれの層を配置することにより製造することができる。例えば、光透過性支持層(A)の光透過性導電層(C)が配置されている側の面に、下層側から順次配置させてもよいが、配置の順番は特に限定されない。例えば、最初に光透過性支持層(A)ではない層(例えば、光透過性導電層(C))の一方の面に他の層を配置させてもよい。あるいは、一方で2種以上の層を互いに隣接するように配置させることにより1種の複合層を得てから、又はそれと同時に、他方で同様に2種以上の層を互いに隣接するように配置させることにより1種の複合層を得て、これらの2種の複合層をさらに互いに隣接するように配置させてもよい。 3. Production method of light transmissive conductive film of the present invention The light transmissive conductive film of the present invention can be produced by disposing each layer as described for each layer. For example, the light-transmissive support layer (A) may be sequentially disposed on the surface on which the light-transmissive conductive layer (C) is disposed from the lower layer side, but the arrangement order is not particularly limited. For example, first, another layer may be disposed on one surface of a layer that is not the light-transmissive support layer (A) (for example, the light-transmissive conductive layer (C)). Alternatively, one composite layer is obtained by arranging two or more layers adjacent to each other on the one hand, or at the same time, two or more layers are similarly disposed adjacent to each other on the other side. Thus, one type of composite layer may be obtained, and these two types of composite layers may be further arranged adjacent to each other.
厚さ125μmのPET樹脂基材(光透過性支持層)上に平均粒子径が16nmのジルコニア粒子を含むアクリレート系樹脂の光学調整層を厚さ0.5μmとなるように形成した。 Example 1
An optical adjustment layer of an acrylate resin containing zirconia particles having an average particle diameter of 16 nm was formed on a PET resin substrate (light-transmitting support layer) having a thickness of 125 μm so as to have a thickness of 0.5 μm.
その後、大気中、140℃で60分加熱処理して、本発明の光透過性導電性フィルムを得た。このフィルムをXRDおよびAFMにて評価した。 At this time, Ra of the optical adjustment layer was 0.7 nm. A SiO 2 layer of 20 nm was formed on this optical adjustment layer by sputtering, and indium tin oxide (ITO) was formed to a thickness of 23 nm. Specifically, a light transmissive conductive layer is formed by a DC magnetron sputtering method using a sintered body material made of indium oxide: 95 wt% and tin oxide: 5 wt% as a target material, and heated in the atmosphere. The light-transmitting conductive film of the present invention was finally obtained. At this time, after evacuating the chamber to 5.0 × 10 −4 Pa or less, oxygen gas and argon gas are introduced into the chamber so that the oxygen partial pressure becomes 6.5 × 10 −3 Pa. The sputtering process was performed with the chamber internal pressure set to 0.3 to 0.4 Pa.
Thereafter, heat treatment was performed in the atmosphere at 140 ° C. for 60 minutes to obtain a light-transmitting conductive film of the present invention. This film was evaluated by XRD and AFM.
平均粒子径が25nmのジルコニア粒子を含むアクリレート系樹脂の光学調整層を厚さ1.0μmとなるように形成した。それ以外は、実施例1と同様とし、本発明の光透過性導電性フィルムを得た。XRDによる評価の結果、ジルコニアに由来する2θ=28°付近のピークの、酸化インジウムに由来する(222)面のピークに対する比は0.30であった。また、酸化インジウムスズの平均粒子経は5.7nmであった。 Example 2
An optical adjustment layer of an acrylate resin containing zirconia particles having an average particle diameter of 25 nm was formed to a thickness of 1.0 μm. Other than that was carried out similarly to Example 1, and obtained the transparent electroconductive film of this invention. As a result of evaluation by XRD, the ratio of the peak around 2θ = 28 ° derived from zirconia to the peak of (222) plane derived from indium oxide was 0.30. The average particle diameter of indium tin oxide was 5.7 nm.
平均粒子径が25nmのジルコニア粒子を含むアクリレート系樹脂の光学調整層を厚さ2.0μmとなるように形成した。それ以外は、実施例1と同様とし、本発明の光透過性導電性フィルムを得た。XRDによる評価の結果、ジルコニアに由来する2θ=28°付近のピークの、酸化インジウムに由来する(222)面のピークに対する比は0.65であった。また、酸化インジウムスズの平均粒子経は3.6nmであった。 Example 3
An optical adjustment layer of an acrylate resin containing zirconia particles having an average particle diameter of 25 nm was formed to a thickness of 2.0 μm. Other than that was carried out similarly to Example 1, and obtained the transparent electroconductive film of this invention. As a result of evaluation by XRD, the ratio of the peak near 2θ = 28 ° derived from zirconia to the peak of the (222) plane derived from indium oxide was 0.65. The average particle diameter of indium tin oxide was 3.6 nm.
平均粒子径が25nmのジルコニア粒子を含むアクリレート系樹脂の光学調整層を厚さ2.9μmとなるように形成した。それ以外は、実施例1と同様とし、本発明の光透過性導電性フィルムを得た。XRDによる評価の結果、ジルコニアに由来する2θ=28°付近のピークの、酸化インジウムに由来する(222)面のピークに対する比は0.94であった。また、酸化インジウムスズの平均粒子経は4.2nmであった。 Example 4
An optical adjustment layer of an acrylate resin containing zirconia particles having an average particle diameter of 25 nm was formed to a thickness of 2.9 μm. Other than that was carried out similarly to Example 1, and obtained the transparent electroconductive film of this invention. As a result of evaluation by XRD, the ratio of the peak near 2θ = 28 ° derived from zirconia to the peak of the (222) plane derived from indium oxide was 0.94. The average particle diameter of indium tin oxide was 4.2 nm.
平均粒子径が34nmのジルコニア粒子を含むアクリレート系樹脂の光学調整層を厚さ1.0μmとなるように形成した。このとき、光学調整層のRaは1.8nmであった。それ以外は、実施例1と同様とし、本発明の光透過性導電性フィルムを得た。XRDによる評価の結果、ジルコニアに由来する2θ=28°付近のピークの、酸化インジウムに由来する(222)面のピークに対する比は0.32であった。また、酸化インジウムスズの平均粒子経は7.7nmであった。 Example 5
An optical adjustment layer of acrylate resin containing zirconia particles having an average particle diameter of 34 nm was formed to a thickness of 1.0 μm. At this time, Ra of the optical adjustment layer was 1.8 nm. Other than that was carried out similarly to Example 1, and obtained the transparent electroconductive film of this invention. As a result of evaluation by XRD, the ratio of the peak near 2θ = 28 ° derived from zirconia to the peak of the (222) plane derived from indium oxide was 0.32. The average particle diameter of indium tin oxide was 7.7 nm.
平均粒子径が16nmのジルコニア粒子を含むアクリレート系樹脂の光学調整層を厚さ0.2μmとなるように形成した。それ以外は、実施例1と同様とし、光透過性導電性フィルムを得た。XRDによる評価の結果、ジルコニアに由来するピークは検出されなかった。また、酸化インジウムスズの平均粒子経は6.8nmであった。 Comparative Example 1
An optical adjustment layer of an acrylate resin containing zirconia particles having an average particle diameter of 16 nm was formed to a thickness of 0.2 μm. Other than that was carried out similarly to Example 1, and obtained the transparent electroconductive film. As a result of evaluation by XRD, no peak derived from zirconia was detected. The average particle diameter of indium tin oxide was 6.8 nm.
平均粒子径が16nmのジルコニア粒子を含むアクリレート系樹脂の光学調整層を厚さ5.0μmとなるように形成した。それ以外は、実施例1と同様とし、光透過性導電性フィルムを得た。XRDによる評価の結果、ジルコニアに由来する2θ=28°付近のピークの、酸化インジウムに由来する(222)面のピークに対する比は1.5であった。また、酸化インジウムスズの平均粒子経は4.9nmであった。 Comparative Example 2
An optical adjustment layer of an acrylate resin containing zirconia particles having an average particle diameter of 16 nm was formed to a thickness of 5.0 μm. Other than that was carried out similarly to Example 1, and obtained the transparent electroconductive film. As a result of evaluation by XRD, the ratio of the peak around 2θ = 28 ° derived from zirconia to the peak of (222) plane derived from indium oxide was 1.5. The average particle diameter of indium tin oxide was 4.9 nm.
平均粒子径が45nmのジルコニア粒子を含むアクリレート系樹脂の光学調整層を厚さ2.8μmとなるように形成した。このとき、光学調整層のRaは2.5nmであった。それ以外は、実施例1と同様とし、光透過性導電性フィルムを得た。XRDによる評価の結果、ジルコニアに由来する2θ=28°付近のピークの、酸化インジウムに由来する(222)面のピークに対する比は1.5であった。また、酸化インジウムスズの平均粒子経は8.4nmであった。 Comparative Example 3
An optical adjustment layer of acrylate resin containing zirconia particles having an average particle diameter of 45 nm was formed to a thickness of 2.8 μm. At this time, Ra of the optical adjustment layer was 2.5 nm. Other than that was carried out similarly to Example 1, and obtained the transparent electroconductive film. As a result of evaluation by XRD, the ratio of the peak around 2θ = 28 ° derived from zirconia to the peak of (222) plane derived from indium oxide was 1.5. The average particle diameter of indium tin oxide was 8.4 nm.
幅5cm×長さ5cmのシリコンゴム板の4辺の一つをくし型パターン状に切断した。幅5cm×長さ10cmにカットした光透過性導電性フィルムのITO側、かつ、くし型パターンが光透過性導電性フィルムの中央部付近に配置されるようにシリコンゴム板を光透過性導電性フィルムに貼り合わせた。シリコンゴムを貼り合わせた光透過性導電性フィルムのシリコンゴム側にエッチングレジストを塗布し、80℃で30分乾燥後、シリコンゴム板を剥がした。これにより、くし型パターンを境界としてITO表面とエッチングレジスト表面が露出する光透過性導電性フィルムを得た。これを、20%塩酸に20分浸漬し、ITOを溶かした。その後、0.5MのKOH溶液に浸漬しながら10分間超音波処理し、水洗することによりITOのくし型パターンフィルムを得た。
白色の紙および黒色の紙の上にくし型パターンフィルムを置き、それぞれITOパターンのエッジにおける視認性を確認した。
評価は次のようにして行った。白色紙上および黒色紙上でITOのパターンがほとんど確認できないときを「◎」、白色紙上および黒色紙上でITOのパターンがほとんど確認できないが、何れかの試料において観察角度を変えることによりパターンを確認できることがあるときを「○」、観察角度を変えることにより何れかの試料においてパターンを必ず確認できるときを「△」、両方の試料においてパターンを確認できるときを「×」とした。 Evaluation of index matching was performed as follows. In order to form a comb pattern (2 mm width, 10 mm length) in the width direction in the vicinity of the center of the light-transmitting conductive film cut to a width of 5 cm and a length of 10 cm, the following operation was performed.
One of four sides of a silicon rubber plate having a width of 5 cm and a length of 5 cm was cut into a comb pattern. The silicon rubber plate is light-transmitting conductive so that the comb-shaped pattern is placed near the center of the light-transmitting conductive film on the ITO side of the light-transmitting conductive film cut to 5 cm wide × 10 cm long Laminated to film. An etching resist was applied to the silicon rubber side of the light-transmitting conductive film bonded with silicon rubber, dried at 80 ° C. for 30 minutes, and then the silicon rubber plate was peeled off. As a result, a light-transmitting conductive film in which the ITO surface and the etching resist surface were exposed with the comb pattern as a boundary was obtained. This was immersed in 20% hydrochloric acid for 20 minutes to dissolve ITO. Then, it was ultrasonically treated for 10 minutes while being immersed in a 0.5 M KOH solution, and washed with water to obtain a comb pattern film of ITO.
A comb pattern film was placed on white paper and black paper, and the visibility at the edge of the ITO pattern was confirmed.
Evaluation was performed as follows. When the ITO pattern on the white paper and the black paper can hardly be confirmed, “◎”, the ITO pattern on the white paper and the black paper can hardly be confirmed, but the pattern can be confirmed by changing the observation angle in any sample. “◯” indicates a certain case, “Δ” indicates that the pattern can be confirmed in any sample by changing the observation angle, and “X” indicates that the pattern can be confirmed in both samples.
光透過性導電性フィルムを20%塩酸に浸漬し、表面抵抗が計測不能になるまでの時間を求めた。光透過性導電性フィルムは10秒~90秒までの10秒間隔で浸漬時間を設定し、表面抵抗が計測不能になった時間をエッチング処理完了時間とした。
エッチング処理完了時間が40秒、50秒のときを「◎」、30秒、60秒、70秒のときを「○」、20秒、80秒のときを「△」、10秒、90秒およびそれ以上を「×」として評価した。エッチング処理時間が短すぎても、また反対に長すぎてもエッチング処理を制御することが困難となり、好ましくない。 The etching property was evaluated as follows.
The light transmissive conductive film was immersed in 20% hydrochloric acid, and the time until the surface resistance could not be measured was determined. For the light-transmitting conductive film, the immersion time was set at intervals of 10 seconds from 10 seconds to 90 seconds.
When the etching processing completion time is 40 seconds and 50 seconds, “◎”, when 30 seconds, 60 seconds, and 70 seconds, “◯”, when 20 seconds and 80 seconds, “△”, 10 seconds, 90 seconds, and More than that was evaluated as “x”. If the etching process time is too short, or conversely too long, it is difficult to control the etching process, which is not preferable.
11 光透過性支持層(A)
12 光学調整層(B)
13 光透過性導電層(C)
14 アンダーコート層(D) 1 Light-transmissive
12 Optical adjustment layer (B)
13 Light transmissive conductive layer (C)
14 Undercoat layer (D)
Claims (6)
- (A)光透過性支持層;
(B)光学調整層;及び
(C)酸化インジウムスズを含有する光透過性導電層
を含有し、
前記光学調整層(B)が、前記光透過性支持層(A)の少なくとも一方の面に、直接又は一以上の他の層を介して配置されており、かつ
前記光透過性導電層(C)が、前記光透過性支持層(A)の少なくとも一方の面に、少なくとも光学調整層(B)を介して配置されている光透過性導電性フィルムであって:
前記光学調整層(B)が、ジルコニアを含有し、かつ厚さ0.4~3μmであり;かつ
薄膜法によるXRD測定において、ジルコニアに由来する2θ=28°付近のピークの、酸化インジウムスズに由来する(222)面のピークに対する比が0.1~1.0であること
を特徴とする、光透過性導電性フィルム。 (A) a light transmissive support layer;
(B) an optical adjustment layer; and (C) a light-transmitting conductive layer containing indium tin oxide,
The optical adjustment layer (B) is disposed on at least one surface of the light transmissive support layer (A) directly or via one or more other layers, and the light transmissive conductive layer (C ) Is a light transmissive conductive film disposed on at least one surface of the light transmissive support layer (A) via at least the optical adjustment layer (B):
The optical adjustment layer (B) contains zirconia and has a thickness of 0.4 to 3 μm; and in the XRD measurement by a thin film method, the peak in the vicinity of 2θ = 28 ° derived from zirconia is indium tin oxide. A light transmissive conductive film, characterized in that the ratio of the derived (222) plane to the peak is 0.1 to 1.0. - 前記光学調整層(B)の、光透過性支持層(A)とは反対側の面の平均表面粗さRaが、0.4~2.0nmである、請求項1に記載の光透過性導電性フィルム。 The light transmissive property according to claim 1, wherein an average surface roughness Ra of the surface of the optical adjustment layer (B) opposite to the light transmissive support layer (A) is 0.4 to 2.0 nm. Conductive film.
- 前記ジルコニアの平均粒子径が、10~40nmである、請求項1又は2に記載の光透過性導電性フィルム。 The light transmissive conductive film according to claim 1 or 2, wherein the zirconia has an average particle diameter of 10 to 40 nm.
- 前記酸化インジウムスズの平均粒子径が、3.0~8.0nmである、請求項1~3のいずれかに記載の光透過性導電性フィルム。 The light-transmitting conductive film according to any one of claims 1 to 3, wherein the indium tin oxide has an average particle diameter of 3.0 to 8.0 nm.
- 前記光透過性導電層(C)が、酸化インジウムスズを含有する層を大気中90~160℃で10~120分間加熱することにより得られうる、請求項1~4のいずれかに記載の光透過性導電性フィルム。 The light according to any one of claims 1 to 4, wherein the light transmissive conductive layer (C) can be obtained by heating a layer containing indium tin oxide at 90 to 160 ° C for 10 to 120 minutes in the atmosphere. Transparent conductive film.
- 請求項1~5のいずれかに記載の光透過性導電性フィルムを含有する、タッチパネル。 A touch panel comprising the light transmissive conductive film according to any one of claims 1 to 5.
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