WO2003045867A1 - Substrat de verre possedant une couche transparente electroconductrice et son procede de production - Google Patents

Substrat de verre possedant une couche transparente electroconductrice et son procede de production Download PDF

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Publication number
WO2003045867A1
WO2003045867A1 PCT/JP2002/012258 JP0212258W WO03045867A1 WO 2003045867 A1 WO2003045867 A1 WO 2003045867A1 JP 0212258 W JP0212258 W JP 0212258W WO 03045867 A1 WO03045867 A1 WO 03045867A1
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WIPO (PCT)
Prior art keywords
film
glass substrate
metal
transparent conductive
metals
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Application number
PCT/JP2002/012258
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English (en)
Japanese (ja)
Inventor
Yosuke Matsukawa
Yoshihide Inako
Toshiaki Yamada
Ryoumei Omote
Original Assignee
Nissha Printing Co., Ltd.
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Filing date
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Application filed by Nissha Printing Co., Ltd. filed Critical Nissha Printing Co., Ltd.
Publication of WO2003045867A1 publication Critical patent/WO2003045867A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
    • C03C17/3417—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials all coatings being oxide coatings

Definitions

  • the present invention relates to a glass substrate with a transparent conductive film suitable for a lower electrode plate or the like constituting a touch panel device and a method for manufacturing the same.
  • touch panel devices have been widely used as input devices in portable electronic devices.
  • a transparent film having a transparent conductive film formed on the lower surface is used as the upper electrode plate, and a glass substrate with a transparent conductive film formed on the upper surface is provided with the transparent conductive film as the lower electrode plate.
  • Some are configured by being laminated so that electrodes face each other.
  • the glass substrate with a transparent conductive film, and the S i 0 2 film and the transparent conductive film formed on one surface of a glass substrate, which S i 0 2 film is formed on the other surface is generally used.
  • a coating solution for forming a SiO 2 film is coated on both surfaces of a glass substrate by an immersion pulling method to form a SiO 2 film, There is a method of forming a transparent conductive film on the surface.
  • the touch panel device In addition, as the display of portable electronic devices has become more colorized, it is necessary for the touch panel device to have high translucency and achromaticity in order to improve the visibility of displays combined with the touch panel device.
  • a glass substrate with a conductive film As a glass substrate with a conductive film, a substrate with high translucency and a hue adjustment that exhibits achromatic color when combined with a general-purpose film with a transparent conductive film used as an upper electrode plate is required. I have.
  • a method for obtaining a glass substrate with a transparent conductive film having high translucency and hue adjustment for example, as disclosed in Japanese Patent Application Laid-Open No. Hei 7-224424, There is a method in which a low refractive index film and a high refractive index film are alternately laminated by a sputtering method to form an optical multilayer film.
  • the glass substrate with the transparent conductive film in which the SiO 2 film and the transparent conductive film are formed on one surface of the glass substrate and the SiO 2 film is formed on the other surface, has a light transmitting property.
  • an object of the present invention is to provide a glass substrate with a transparent conductive film having high translucency and hue adjustability, which solves the above-mentioned problems, and a method of manufacturing the same. Disclosure of the invention
  • the present invention is configured as described below to achieve the above object.
  • a first film containing at least 90% by weight of at least one metal oxide of Zr, Ti, Al, and Si on one surface of a glass substrate; a second film containing ⁇ 2 90 wt% or more, I n, Sn, Zn, S b, Al, the least one or more metal oxides of Y and a third layer containing 90 wt% or more At least 7 layers are formed
  • a glass substrate On the other surface of the glass substrate, Z r, T i, A 1, S and a fourth layer containing at least one kind of a metallic oxide 90 wt% or more of i, S i 0 2 90 wt% or more Provided is a glass substrate provided with a transparent conductive film, which is formed by laminating at least a fifth film to be contained.
  • the first film is provided on one surface of the glass substrate
  • the fourth film contains at least 90% by weight of at least two metal oxides of Zr, Ti, A1, and Si on the other surface of the glass substrate.
  • a glass substrate provided with a transparent conductive film.
  • the first film and the fourth film have a refractive index of 1.58 to 1.73 and a thickness of 25 to 85 nm, respectively, and the second film and the fifth film
  • Each of the films has a refractive index of 1.36 to 1.48 and a thickness of 45 to: L 00 nm
  • the third film has a refractive index of 1.70 to 1.95 and a thickness of 10 to 20 nm.
  • the maximum transmittance (T max ) in the wavelength range of 380 to 780 nm is in the range of 380 to 500 nm and is 93 ° /.
  • the chroma take-up indices a * and b * of the L * a * b * color system are less than 2.0 under the measurement conditions of the C light source 2 ° field of view.
  • the transmittance (T 50 ) at a wavelength of 500 nm is 91% or more
  • the transmittance at 600 nm (T 600 ) is 89% or more
  • the transmittance at 70 OO nm is rate (T 7. 0) to provide a glass substrate with a transparent conductive film according to the fourth aspect at least 88%.
  • the glass substrate with a transparent conductive film according to the first or third aspect wherein the third film has a surface resistivity of 500 to 1200 ⁇ aperture.
  • a metal chelate compound containing at least one metal of Zr, Ti, Al, and Si on one surface of a glass substrate, at least one metal of the above metals
  • An organic acid salt containing at least one of the above metals; a hydrolyzable organic metal compound containing at least one or more of the above metals; a hydrolyzate of the above organic metal compound; After coating or printing a coating solution comprising a base material and a solvent containing at least one of the group consisting of at least one or more metal oxides, and then drying to form a first film,
  • a metal chelate compound of Si, an organic acid salt containing Si, an inorganic acid salt containing Si, a hydrolyzable organic silicon compound, a hydrolyzate of the organic silicon compound After coating or printing a main agent containing at least one member selected from the group consisting of silicon oxides, a solvent, and a strong coating solution, the coating is dried to form a second film, and on the upper surface of the second film, A metal chelate compound containing at least one or more metals of In, Sn, Zn, Sb, Al, and Y; an organic acid salt containing at least one of the above metals; and at least one or more of the above metals A group consisting of an inorganic acid salt containing a metal of the above, a hydrolyzable organometallic compound containing at least one metal of the above metals, a hydrolyzate of the above organic metal compound, and a metal oxide of at least one of the above metals And at least one of them Coating also a coating solution consisting of Is printed,
  • a method for producing a glass substrate with a transparent conductive film comprising coating or printing a coating solution capable of forming a solvent and a main agent containing at least one member selected from the group consisting of silicon oxides, followed by drying to form a fifth film.
  • the above glass substrate is provided on one surface of the glass substrate with a metal material containing at least two or more metals of Zr, Ti, A1, and Si.
  • a metal chelate compound containing at least two or more metals of Zr, Ti, A1, and Si; at least two or more of the above metals An organic acid salt containing at least two metals of the above metals; a hydrolyzable organic metal compound containing at least two or more metals of the above metals; After coating or printing a coating solution comprising a base material and a solvent containing at least one of the group consisting of decomposed products and at least two metal oxides of the above-mentioned metals, and then drying, the above-mentioned fourth film is formed.
  • a method for manufacturing a glass substrate with a transparent conductive film according to the seventh aspect is provided.
  • a metal chelate compound containing at least one metal of Zr, Ti, Al, and Si on both surfaces of a glass substrate, at least one metal of the above metals, An organic acid salt containing at least one of the above metals; an inorganic acid salt containing at least one or more of the above metals; a hydrolyzable organometallic compound containing at least one or more of the above metals; a hydrolyzate of the above organic metal compound; After coating or printing a coating liquid comprising a main agent and a solvent containing at least one of the group consisting of at least one or more metal oxides, and drying, forming a first film and a fourth film,
  • a metal chelate compound of Si, an organic acid salt containing Si, an inorganic acid salt containing Si, a hydrolyzable organic silicon compound are formed on the upper surface of the first film and the upper surface of the fourth film.
  • a coating solution comprising a base material and a solvent containing at least one of the group consisting of a hydrolyzate of an organic silicon compound and a silicon oxide
  • the coating solution is dried to form a second film and a fifth film.
  • a metal chelate compound containing at least one or more metals of In, Sn, Zn, Sb, Al, and Y, and at least one metal of the above metals
  • An organic acid salt containing at least one of the above metals; a hydrolyzable organic metal compound containing at least one or more of the above metals; a hydrolyzate of the above organic metal compound;
  • a transparent conductive film that forms a third film by coating or printing a coating liquid containing a main agent containing at least one metal oxide of at least one metal and a solvent, followed by drying and firing to form a third film
  • a method for manufacturing an attached glass substrate is a method for manufacturing an attached glass substrate. '
  • At least two or more of Zr, Ti, Al, and Si are formed on both surfaces of the glass substrate.
  • a metal chelate compound containing a metal, an organic acid salt containing at least two or more of the above metals, an inorganic acid salt containing at least two or more of the above metals, and at least two or more of the above metals A hydrolyzable organometallic compound, a hydrolyzate of the above-mentioned organometallic compound, and a coating solution comprising a main agent containing at least one of the above-mentioned metals and a solvent, and a solvent.
  • the present invention provides the method for producing a glass substrate provided with a transparent conductive film according to the ninth aspect, wherein the first film and the fourth film are formed by drying after printing.
  • the transparent conductive film according to the ninth aspect wherein the coating of the first film, the second film, the fourth film, and the fifth film is an immersion bow I method.
  • a method for manufacturing a glass substrate with a film is provided.
  • an intaglio roll that rotatably supports the third film on a support frame of a base and has on its surface a number of ink cells having a depth of 1.0 to several 1 ° / xm.
  • An ink supply device for supplying 1.0 to 10,000 mPas of ink to the surface of the intaglio roll, and an ink supply device provided at a predetermined location around the intaglio roll supported by the support frame and supplied to the intaglio roll A doctor that spreads the ink on the surface of the intaglio roll to hold a certain amount of the ink in the ink cell; and a rotatable support below the intaglio port of the support frame and the intaglio port.
  • a printing roll having a projecting portion that comes into contact with the surface of the intaglio roll and transferring the ink in the ink cell to the projecting portion; and a synchronous rotation drive of the printing roll and the intaglio roll supported by the support frame.
  • a printing medium driving device that moves between the two positions; and a control unit that controls the rotation of the printing port and the movement of the surface plate from the ⁇ position to the printing position, and the convex portion of the printing port.
  • the first layer, the second layer, the fourth layer, in the step of forming the fifth layer the maximum transmittance in the wavelength region 380 ⁇ 7 8 0 nm (T raa J is in the range of 380 to 420 nm and is 95% or more, and the chroma take-up indices a * and b * of the L * a * b * color system are 1. 5 ⁇ a * l. 5 and 1. 3.
  • the method for producing a glass substrate with a transparent conductive film according to any one of the embodiments 7 to 7 which is Ob * O: L 1 is provided.
  • the transmittance (T 5 ) at a wavelength of 500 nm is 9 PC leak 2/12258
  • the first film and the fourth film, and the second film and the fifth film each have the same composition, thickness, and refractive index as the first film.
  • the glass substrate with a transparent conductive film described in the aspect is provided.
  • the first film and the fourth film, and the second film and the fifth film each of which has the same composition, thickness, and refractive index as the seventh or the fifth film
  • a method for manufacturing a glass substrate with a transparent conductive film according to the ninth aspect is provided.
  • FIG. 1 is a cross-sectional view illustrating a glass substrate with a transparent conductive film according to one embodiment of the present invention.
  • FIG. 2 is a cross-sectional view illustrating one step of a method of manufacturing the glass substrate with a transparent conductive film according to the embodiment of the present invention.
  • FIG. 1 is a cross-sectional view illustrating a glass substrate with a transparent conductive film according to one embodiment of the present invention.
  • FIG. 2 is a cross-sectional view illustrating one step of a method of manufacturing the glass substrate with a transparent conductive film according to the embodiment of the present invention.
  • FIG. 3 is a cross-sectional view showing one step of the method for producing a glass substrate with a transparent conductive film of the embodiment of the present invention
  • FIG. 4 is a graph showing the spectral transmittance of the glass substrate with a transparent conductive film of the embodiment of the present invention
  • FIG. 5 is a perspective view showing a thin film forming apparatus that can be used in the method for manufacturing a glass substrate with a transparent conductive film of the embodiment of the present invention
  • FIG. 6 is a cross-sectional view showing a state in which a touch panel is formed by combining a glass substrate with a transparent conductive film and a film with a transparent conductive film according to the embodiment of the present invention.
  • FIG. 1 is a cross-sectional view showing one embodiment of a glass substrate provided with a transparent conductive film according to one embodiment of the present invention.
  • 2 and 3 are cross-sectional views illustrating one process of a method for manufacturing a glass substrate with a transparent conductive film according to the embodiment of the present invention.
  • FIG. 4 is a graph showing the spectral transmittance of the glass substrate with a transparent conductive film according to the embodiment of the present invention.
  • FIG. 5 is a perspective view showing a thin film forming apparatus that can be used in the method of manufacturing a glass substrate with a transparent conductive film according to the embodiment of the present invention.
  • 1 is a glass substrate with a transparent conductive film
  • 2 is a glass substrate
  • 3 is a first film
  • 4 is a second film
  • 5 is a third film
  • 6 is a fourth film
  • 7 is a fifth film.
  • the glass substrate 1 with a transparent conductive film comprises at least 90% by weight of at least one metal oxide of Zr, Ti, A1, Si on one surface of the glass substrate 2.
  • the first film 3 having, a second film 4 containing S I_ ⁇ 2 9 0 wt% or more, I n, S n, Z n, S b, a 1, at least one metal oxide of Y
  • a third film 5 containing at least 90% by weight of at least one metal oxide of at least one of Zr, Ti, A1, and Si on the other surface of the glass substrate 2.
  • the a fourth film 6 containing 9 0 wt% or more, in which a fifth layer 7 containing S i 0 2 9 0 wt% or more is formed by laminating at least the order 7 fire (see FIG. 1) .
  • the glass substrate 2 is not particularly limited as long as it is transparent.
  • soda lime glass, borate glass and the like can be used.
  • a glass substrate that is particularly suitable from the viewpoint of cost is soda lime glass.
  • the thickness of the glass substrate 2 is not particularly limited, but is preferably 0.15 to 1.8 mm. If the thickness is less than the above range, the strength of the touch panel device may be insufficient. If the thickness is larger than the above range, the thickness and weight of the touch panel device increase, which is not preferable, and the transmittance is lowered due to light absorption, which is not preferable.
  • a first film 3, a second film 4, and a third film 5 are sequentially formed on one surface of the glass substrate 2, and a fourth film 6 and a fifth film 7 are sequentially formed on the other surface.
  • the first film 3 is made of at least one metal oxide of Zr, Ti, A1, Si.
  • the content is 0% by weight or more. Oxides such as Al, P, Pb, B, In, Sn, and Zn may be contained as trace components. Further, the first film 3 may contain at least 90% by weight of at least two kinds of metal oxides of Zr, Ti, A1, and Si. Mixing two or more different substances in this way is
  • the immersion pull-up method is easier than the gas phase method such as the tarling method and the vapor deposition method, and the refractive index can be arbitrarily controlled by changing the mixture ratio of the substances having different refractive indexes.
  • the immersion pull-up method can reduce the cost of manufacturing equipment and materials as compared with the vapor phase method such as the sputtering method and the vapor deposition method.
  • the second layer 4 are those containing S i 0 2 9 0 wt% or more. As a trace component
  • acid scabs such as Al, P, Pb, and B.
  • the third film 5 contains at least 90% by weight of at least one metal oxide of In, Sn, Zn, Sb, Al, and Y. Oxides such as Si, A1, Ti, and Zr may be contained as trace components.
  • the third film 5 functions as a transparent conductive film in the glass substrate 1 with a transparent conductive film.
  • the surface resistivity of the third film 5 may be set to 500 to 1200 ⁇ / port (ohms per square).
  • the third film 5 can exhibit excellent physical properties as a transparent electrode of a touch panel device. If the resistance is lower than 500 ⁇ , input detection may be difficult in an analog resistive touch panel device. Further, if the resistance is higher than 1200 ⁇ / mouth, the input sensitivity may be reduced in an analog resistance film type touch panel device.
  • the surface resistivity is a term defined in Japanese Industrial Standard JISK6911, and the potential gradient in the direction parallel to the current flowing along the surface of the test piece is expressed as the current per unit width of the surface. It is the numerical value divided. The unit is marked as “ ⁇ / mouth” to distinguish it from a simple resistor.
  • the fourth film 6 are those containing Z r, T i, A l , at least one metal oxide of S i 9 0 wt 0/0 above. Oxides such as Al, P, Pb, B, In, Sn, and Zn may be contained as trace components. Further, the fourth film 6 may contain 90% by weight or more of at least two kinds of metal oxides of Zr, Ti, A1, and Si. Mixing two or more different substances in this way is easier than the immersion pull-up method compared to gas phase methods such as sputtering and evaporation, and changes the mixing ratio of substances with different refractive indices. Thus, the refractive index can be controlled at will.
  • the immersion pull-up method can reduce the cost of manufacturing equipment and materials as compared with the vapor phase method such as the sputtering method and the vapor deposition method.
  • the fifth layer 7 are those containing S i 0 2 90 wt% or more. Oxides such as Al, P, Pb and B may be contained as trace components.
  • the glass substrate 1 with a transparent conductive film having the above-described configuration has high translucency and hue adjustability.
  • the first film 3 and the fourth film 6 have a refractive index of 1.58 to 1.73 and a film thickness of 25 to 85 nm
  • the second film 4 and the fifth film 7 have a refractive index of 1.36 to L.
  • the film thickness be 45 to 100 nm
  • the refractive index of the third film 5 be 1.70 to 1.95
  • the film thickness be 10 to 2 Onm.
  • the touch panel device When combined with a general-purpose film with a transparent conductive film used as an upper electrode plate, the touch panel device as a whole eliminates the phenomenon of absorption of a specific wavelength range of light and coloring such as yellowing, and achromaticity. Can be easily achieved.
  • 101 is a transparent resin film
  • 102 is an upper transparent conductive film disposed on the glass substrate side of the transparent resin film 101
  • 103 is disposed on the lower transparent conductive film 5, which is a third film.
  • the large number of transparent dot spacers 104 are spacers for forming a predetermined gap between the upper transparent conductive film 102 and the lower transparent conductive film 5.
  • the transparent resin film 101 When the transparent resin film 101 is pressed by a pen or the like, the upper transparent conductive film 102 on the inner surface of the transparent resin finolem 101 comes into contact with the lower transparent conductive film 5 in the gap between the dot spacers 103, so that the input is performed. As a result, a touch panel is constructed.
  • the film thickness of the first film 3 and the fourth film 6 is set to X (nm), the second film 4 and the fifth film
  • the film thickness of 7 is y (nm)
  • the film satisfies the relationship of 80-0.4x ⁇ y ⁇ 100-0.5x.
  • the glass substrate 1 with a transparent conductive film of the above embodiment of the present invention has a wavelength region of 380
  • the maximum transmittance (T max ) at 780 nm to 780 nm is 93% or more in the range of 380 to 500 nm, and the chromatic take index a * and b * of the L * a * b * color system But C light source2.
  • T max the maximum transmittance
  • a * and b * are the International Commissioner for Lighting PC leak 2/12258
  • X, ⁇ , and ⁇ are the three characteristics of visual perception when the human eye sees the color of the object.
  • X, ⁇ , and ⁇ are the three characteristics of visual perception when the human eye sees the color of the object.
  • ⁇ 116 (Y / Y.) 1/3 —16
  • X, ⁇ , and ⁇ are the three characteristics of visual perception when the human eye sees the color of the object.
  • X, ⁇ , and ⁇ are the three characteristics of visual perception when the human eye sees the color of the object.
  • ⁇ Represents each stimulus value felt by ⁇ . , ⁇ . , ⁇ .
  • ⁇ for C standard light. 98.072
  • the maximum transmittance (T max ) in the wavelength range of 380 to 780 nm is in the range of 380 to 500 nm and is 93% or more.
  • the glass substrate 1 with a transparent conductive film has excellent hue adjustability.
  • the glass substrate with a transparent conductive film 1 that satisfies these requirements is combined with a general-purpose film with a transparent conductive film used as an upper electrode plate (see FIG. 6), a specific wavelength of light as a whole touch panel device is obtained. This eliminates the phenomenon of coloring, such as absorption of the region and yellowing, making it possible to easily exhibit achromaticity.
  • the transmittance at 500 nm (T 500 ) is 91% or more, the transmittance at 600 nm (T 600 ) is 89% or more, and the transmittance at 700 nm (T 7) is 88% or more. More preferably, there is.
  • the glass substrate 1 with a transparent conductive film having higher translucency and hue adjustability can be obtained.
  • the following method may be used.
  • One surface of the glass substrate 2 includes a metal chelate compound containing at least one or more metals of Zr, Ti, Al, and Si, and at least one or two or more metals of the above metals Organic acid salts, inorganic acid salts containing at least one or more metals of the above metals, calo containing at least one or more metals of the above metals
  • the coating liquid is coated or printed, and then dried to form the first film 3 (see FIG. 2). After drying, bake if necessary.
  • the baking of the first film 3 can be performed, for example, by heating using a hot air circulation electric furnace, an infrared heater, or the like.
  • a second solution 4 is formed by coating or printing a coating solution comprising a main agent containing at least one of the group consisting of silicon oxides and a solvent, and then drying it (see FIG. 3). After drying, bake if necessary.
  • the firing of the second film 4 can be performed in the same manner as the firing of the first film 3.
  • the third film 5 is fired after drying.
  • the baking of the third film 5 can be performed, for example, by heating while controlling the atmosphere using a vacuum gas replacement furnace or the like.
  • a metal chelate compound containing at least one or more of Zr, Ti, Al, and Si, or at least one or more of the above metals an organic acid salt containing a metal, an inorganic acid salt containing at least one or more of the above metals, a hydrolyzable organic metal compound containing at least one or more of the above metals, Coating or printing a coating liquid comprising a solvent and a main agent containing at least one selected from the group consisting of at least one or two or more metal oxides of the above metals; Thereafter, it is dried to form the fourth film 6 (see FIG. 2). After drying, bake if necessary T JP02 / 12258
  • the sintering of the fourth film 6 can be performed in the same manner as the first film 3.
  • a metal chelate compound of Si, an organic acid salt containing Si, an inorganic acid salt containing Si, a hydrolyzable organic silicon compound, a hydrolyzate of the above organic silicon compound A coating solution consisting of a base material containing at least one elemental oxide from the group consisting of oxides, a solvent and a solvent is coated or printed, and then dried to form a fifth film 7 (see FIG. 3). After drying, bake if necessary. The sintering of the fifth film 7 can be performed in the same manner as the second film 5.
  • the fourth film 6 and the fifth film 7 can be formed at any time before and after the formation of the first to third films. In particular, if the fourth film 6 is formed at the same time as the formation of the first film 3 and the fifth film 7 is performed at the same time as the formation of the second film 4, it is reasonable to increase the number of operations that can be performed repeatedly.
  • the baking step is always required for the third film 5, but is optional for the first film 3, the second film 4, the fourth film 6, and the fifth film 7. Also, the first film 3, the second film 4, the fourth film 6, and the fifth film 7 should not be fired each time each film is formed, but should be fired after forming a plurality of films. It may be.
  • an organic metal material, an inorganic metal material, a composite material thereof and a solvent can be appropriately selected and used.
  • a commercially available product prepared by using a metal compound or the like as a coating liquid, or a sol formed by hydrolyzing a metal compound or the like by a general sol-gel method can be used.
  • the coating liquid referred to in the above embodiment of the present invention means a liquid yarn composition that can be used in various film forming methods such as a coating method and a printing method, and is used in the coating method. It is not limited to those.
  • tetrabutoxyzirconium zirconium tributoxy Xia cetyl ⁇ Seto ne over preparative, zirconium tetrachloride, Z r OH (OC 4 H 9) 2 C 5 H 7 ⁇ 2, Z r 0 2, Te Toraiso propoxytitanium, titanium ⁇ cetyl ⁇ Seto titanate, titanium tetrachloride, T i OH ( ⁇ _C 3 H 7) 3, T I_ ⁇ 2, i Seo propoxide, aluminum ⁇ cetyl ⁇ Seto sulfonates, Anoreminiumu chloride, A l (OH) 3, A 1 2 0 3, Tetorae Tokishishiran, tetra isopropoxide volume silane, four Kei containing chloride, Kei-containing soda, S i OH (OC 2 H 5) 3, and the like S i 0 2.
  • coating liquids include Atron NZr manufactured by Nippon Soda Co., Ltd., Ethylsilicate 28 manufactured by Konorecoat Co., Ltd., Opto Lake 1120 Z manufactured by Catalyst Chemicals Co., Ltd., and MK C-silicate MS51 manufactured by Mitsubishi Chemical Corporation.
  • Examples of the material that can be used for each of the second film 4 and the fifth film 7 include methyl silicate, ethyl silicate, and methyltrimethoxysilane.
  • Examples of commercially available coating liquid Tokyo Ohka Kogyo S i 0 2 dip solution Co., Ltd. (M OF- P- S i 80315, MO FPS i 90315), Nissan Chemical Industries, Ltd. made the low-refractive-S i O 2 dip solution (LR501 ) and so on.
  • Materials that can be used for the third film 5 include triisopropoxy indium, tetraisopropoxy tin, tin 2-ethylhexanoate, tetrabutoxy tin, dibutyl tin bis (acetyl acetate), indium nitrate, In n (OH) (CH3COCHOCH3) 2, I n 2 0 3, acetate Zn, Zn Asechirua Seteto, tri isobutoxy antimony, antimony trichloride, Isopuropokishia Rumyeumu, aluminum ⁇ cetyl ⁇ Seto sulphonate, aluminum chloride, A 1 (O
  • an intaglio roll 13 rotatably supported by a support frame 12 of a base 11 and having a large number of ink cells having a depth of 1.0 to several tens on its surface, an intaglio roll
  • An ink supply device 15 for supplying 1.0 to 10,000 mPa ⁇ s of ink to the surface of the ink jet printer 13, and an ink supplied to the intaglio roll 13 at a predetermined position around the intaglio roll 13 supported by the support frame 12.
  • a printing roll 14 that transfers the ink in the ink cells on the surface to the projections 17; a driving device 18 that is supported by the support frame 12 and drives the printing roll 14 and the intaglio roll 13 to rotate synchronously;
  • the print medium A is placed on the base 11 and is movable between the retracted positions B and C away from the print roll 14 and the print position A where the print medium 14 contacts the print roll 14.
  • the platen 21 and the platen 21 are moved between the retracted positions B and C, and the printing medium drive unit 20 is rotated.
  • the print rolls 14 are rotated and the platen 19 is printed at the position B.
  • solvents used in the printing method for the method of forming the third film 5 include solvents such as ethyl ethyl solvent, dipropylene glycol monomethyl ether, etc., solvents, solvents, canolebitone-based solvents such as phthalene carbitol, and ethylene glycol. Glycol solvents such as glue and hexylene glycol are preferred from the viewpoint of film forming properties and life of the coating solution.
  • the immersion pulling method By immersing the glass substrate 2 in a coating liquid used for forming the first film 3 and the fourth film 6 and pulling it up, the first film 3 and the fourth film 6 can be simultaneously coated. Further, the glass substrate 2 on which the first film 3 and the fourth film 6 are formed is immersed in a coating liquid used for forming the second film 4 and the fifth film 7, and the glass substrate 2 is pulled up. The second film 4 and the fifth film 7 can be formed simultaneously.
  • the immersion pull-up method can reduce costs in terms of manufacturing equipment and materials, as compared with gas-phase methods such as sputtering and vapor deposition.
  • Solvents used for the immersion pull-up method for forming the first film 3, the second film 4, the fourth film 6, and the fifth film 7 include alcohol solvents such as methanol and ethanol, methyl acetate, ethyl acetate, and the like. Preferred are ester solvents, ketone solvents such as acetone and methyl ethyl ketone. Further, the solvent may be composed of these single materials, or may be composed of two or more materials.
  • the first film 3 and the fourth film 6 and the second film 4 and the fifth film 7 may have the same composition, thickness, and refractive index, respectively.
  • two films can be simultaneously formed by the immersion pull-up method, so that the cost can be reduced.
  • the optical characteristics due to the accumulation of process variations are reduced. The effect on sex can be reduced.
  • a first film 3, a second film 4, a fourth film 6, and a fifth film 7 are formed on the glass substrate 2, and the first film 3, the second film 4, the fourth film 6, and the fifth film 7 are formed.
  • the maximum transmittance (T max ) in the wavelength range of 380 to 780 nm is in the range of 380 to 42011111 and is 95% or more, and the power of the L * a * b * color system
  • the chroma takeness indices a * and b * may be configured such that 11.5 ⁇ a * ⁇ l.5 and 13.0 ⁇ b * ⁇ 0.
  • the maximum transmittance ( Tmax ) in the wavelength region of 380 to 780 nm is in the range of 380 to 42 Onm and is 95% or more.
  • the glass substrate 1 with the transparent conductive film has excellent hue adjustability.
  • a third film 6 serving as a transparent conductive film is provided on the second film 4, and when combined with a general-purpose film with a transparent conductive film used as an upper electrode plate, the touch panel device as a whole is required.
  • a general-purpose film with a transparent conductive film used as an upper electrode plate the touch panel device as a whole is required.
  • the transmittance at wavelength 500 nm (T 500 ) is 91% or more, the transmittance at 600 nm (T 600 ) is 89% or more, and the transmittance at 700 nm (T 700 ) is 88% or more Is more preferred.
  • T 500 The transmittance at wavelength 500 nm
  • T 600 the transmittance at 600 nm
  • T 700 the transmittance at 700 nm
  • the coating liquid used to form the first to third films 3 to 5 includes, for example, stabilization of the coating liquid, viscosity adjustment, smoothness and drying property of the first to third films 7 and visualization, etc.
  • Various additives and the like can be mixed according to the purpose.
  • the type of the additive is not particularly limited as long as it can obtain desired properties with respect to coating properties of the coating liquid and a film made of a metal oxide.
  • additives For example, stabilizers such as ammonia and acetic acid, fillers such as Zr, Ti, Si, Pb, A1, In, Sn, Zn, etc.
  • surfactants such as polyethylene oxide and dyes such as oil color.
  • the amount of additive used is less than 10% by weight, based on the total weight of the coating solution. If the amount of the additive is 10% by weight or more, the performance of the first to third films 3 to 6 is impaired, and for example, the refractive index after film formation may not fall within a predetermined range. is there.
  • the glass substrate 1 with a transparent conductive film obtained by the above-described manufacturing method has high translucency and hue adjustability as described above.
  • FIG. 4 is a graph showing the transmittance of the glass substrate 1 with a transparent conductive film having various configurations.
  • a indicates the spectral transmittance of the glass substrate 1 with a transparent conductive film, the hue of which is adjusted according to the above embodiment of the present invention.
  • b indicates the spectral transmittance of the glass substrate 2 on which the first film 3, the second film 4, the fourth film 6, and the fifth film 7 are formed and the third film 5 is not formed.
  • c indicates the spectral transmittance of the glass substrate on which the optical multilayer film is formed (see Japanese Patent Application Laid-Open No. 7-242442).
  • the glass substrate 1 with a transparent conductive film of the above embodiment of the present invention has a high light transmittance in a wavelength region of 380 to 500 nm and a light transmittance in other wavelength regions. It can be confirmed that the film has a well-balanced light-transmitting property without a large decrease in the efficiency. In addition, since the transmittance in a long wavelength portion is slightly lower, it can be confirmed that the hue is adjusted to have a bluish color.
  • Z r O 2 phase Nippon Soda Co., Ltd. is a hydrolyzate of a hydrolyzable organometallic compound Atoron NZ r (5 wt 0/0 question, zirconium alkoxide a precursor-containing) 4 5 parts by weight prepared from co Rukoto S i O 2 equivalent of the precursor-containing steel E chill silicate 2 8 (2 8 wt%, Ltd.) 5 parts by weight of methyl alcohol 2 5 wt was diluted with parts and mixed solvent acetone 2 5 parts by weight, Z r 0 2 and S i 0 2 3. was 6 5% by weight equivalent of the precursor mixture coating solution 1 0 0 parts by weight was prepared.
  • the above-mentioned coating solution is filled in a dipping pulling tank, and the washing is performed as a glass substrate.
  • a purified 30 OmmX 35 Omm 1.1 mm soda-lime glass plate was placed in a dipping and pulling tank, and then pulled up at a speed of 10 cmZ to coat both surfaces of the glass substrate with the above coating liquid. Then, at 150 ° C hot air circulation type open
  • a SiO 2 dip solution (MO FPS 1 80315, manufactured by Tokyo Ohka Kogyo Co., Ltd., a precursor-containing coating equivalent to 8% by weight of SiO 2 phase) was used.
  • Liquid) 50 parts by weight were diluted with a mixed solvent of 25 parts by weight of ethyl acetate and 25 parts by weight of methanol to prepare 100 parts by weight of a coating liquid corresponding to 4% by weight of SiO 2 .
  • Fill the immersion lifting tank with the above coating liquid immerse the glass substrate on which the first and fourth films are formed in the above coating liquid, and pull up at a speed of 20 cmZ to coat the coating liquid on both sides. did.
  • the second film having a Si 2 content of 90% by weight or more, a refractive index of 1.46, a film thickness of 75 nm and a Films were formed on the first and fourth films, respectively.
  • the glass substrate on which the first film, the second film, the fourth film, and the fifth film are formed as described above has a maximum transmittance (T max ) in the wavelength range of 380 to 780 nm of 390 nm, which is 96 nm. . 2%, transmittance at 500 nm (T 5 ..) is 93.3%,
  • Transmittance at 600 nm (T 6 ..) is 91.2%
  • This glass substrate was placed in a hot air circulating open at 85 ° C for 20 minutes to perform pre-drying, and then in a vacuum purged box furnace at an oxygen flow rate of 2 liters / minute and a heating rate of 15 ° C / minute for 500 minutes. The temperature was raised to ° C. After keeping the film for 30 minutes to completely oxidize the film, the inside of the furnace was once depressurized by a vacuum pump.
  • the glass substrate with a transparent conductive film obtained in this way has a surface resistance of 650 ⁇ square and a maximum transmittance (T max ) of 440 nm in the wavelength range of 380 to 780 nm.
  • An ellipsometer (DH A-XAVW / S 6 manufactured by Mizojiri Optical Industrial Co., Ltd.) was used for the measurement of the refractive index.
  • a step gauge (ET10, manufactured by Kosaka Laboratory Co., Ltd.) was used to measure the film thickness.
  • a spectrophotometer (UV3100, manufactured by Shimadzu Corporation) was used to measure light transmittance and hue.
  • hue the chroma takeness indices (a *, b *) indicating hue and saturation in the L * a * b * color system in a wavelength range of 380 to 780 nm, a C light source, and a 2 ° visual field were evaluated.
  • the measurement of the surface resistance Koijika, resistivity meter (Mitsubishi Petrochemical Co., Ltd. (currently, Ltd. die ⁇ Instruments menu N') made Lo resta MCP- T 5 ..) was used.
  • T i O 2 is 71 wt%, S I_ ⁇ 2 29 wt. / 0, a refractive index of 1.6 9, the film thickness to obtain a first film Contact Yopi fourth film of 36 nm. Subsequently, a second film and a fifth film were formed in the same manner as in Example 1.
  • Example 2 Next, a third film was formed on the second film of the highly translucent glass in the same manner as in Example 1 to obtain a glass substrate with a transparent conductive film.
  • the glass substrate with a transparent conductive film obtained in this manner has a surface transmittance of 700 ⁇ , a maximum transmittance (T max ) in a wavelength region of 380 to 780 nm of 46 Onm of 95.8%, and a wavelength of 500 nm. Is 95.6 %, the transmittance at 600 nm (T 600 ) is 93.8%, and the transmittance at 700 nm (T 70 ) is 92.0%.
  • a transparent touch panel device was obtained in the same manner as in Example 1, which was almost colorless and transparent, and had excellent visibility even when installed on a color liquid crystal. The image quality was clearly felt.
  • tetraisopropoxy emissions Nacalai tester Ltd., 28 weight 0/0 T i 0 2 equivalent
  • Mitsubishi Was mixed with (S i O 2 equivalent of 52 weight 0/0) 5 parts by weight Asechiruaseton 10 parts by weight Chemical Co., Ltd.
  • MK C Silicate MS 5 1 was added and stirred for one hour and distilled water 1 part by weight solution, acetone 82 parts by weight ⁇ tl, 5 wt 0/0 equivalent T i O 2 and S i mixed coating solution 108 parts by weight of O 2 was prepared.
  • the first film and the fourth film were coated on a glass substrate in the same manner as in Example 1 using the above-mentioned coating solution, and then dried in a hot air circulation open at 150 ° C. for 20 minutes.
  • the second film and the fifth film were coated in the same manner as in Example 1, followed by drying and firing.
  • the first film and the fourth film thus obtained have a Ti 0 2 of 35% by weight S i 0 2
  • the weight was 65% by weight, the refractive index was 1.60, and the film thickness was 55 nm.
  • the second film and the fifth film had 90% by weight or more of SiO 2 , a refractive index of 1.46, and a thickness of 75 nm.
  • the glass substrate on which the first, second, fourth, and fifth films were formed had a maximum transmittance (T max ) of 96.6% in the wavelength region of 380 to 780 nm at 420 nm. , Transmission at 500 nm (T 5. ) 95.2%, 60
  • the transmittance at Onm (T 600 ) is 92.8%, and the transmittance at 700 nm (T 600 )
  • Example 2 Next, a third film was formed on the second film in the same manner as in Example 1 to obtain a glass substrate with a transparent conductive film.
  • the glass substrate with a transparent conductive film obtained in this way has a surface resistance of 700 ⁇ , a maximum transmittance (T max ) in the wavelength region of 380 to 780 nm of 460 nm, 94.8%, and a transmission of 500 nm.
  • the transmittance (T 500 ) is 94.4%
  • the transmittance at 600 nm (T 600 ) is 92.8%
  • the transmittance at 700 nm (T 700 ) is 91.7%
  • Example 4 Using this glass substrate with a transparent conductive film, a transparent touch panel device was obtained in the same manner as in Example 1. The device was almost colorless and transparent, and had excellent visibility and visibility even when installed on a color liquid crystal. The image quality was clearly improved. (Example 4)
  • a first film and a fourth film were formed in the same manner as in Example 1 except that the coating liquid for forming the second film and the fifth film was used, and then a second film and a fifth film were formed.
  • the second film and the fifth film, S i 0 2 is about 95 wt. /.
  • the refractive index was 1.38 and the film thickness was about 65 nm.
  • the thus obtained glass substrate on which the first, second, fourth and fifth films are formed has a maximum transmittance (T max ) in the wavelength region of 380 to 780 nm of 420 nm.
  • T max maximum transmittance
  • the transmittance at 500 nm (T 500 ) is 93.5%
  • the transmittance at 600 nm (T 600 ) is 90.6%
  • the transmittance at 700 nm (T 70 ) is 89.
  • Example 2 Next, a third film was formed on the second film in the same manner as in Example 1 to obtain a glass substrate with a transparent conductive film.
  • the glass substrate with a transparent conductive film thus obtained had a surface resistance of 700 ⁇ / port, a maximum transmittance (T max ) in the wavelength range of 380 to 780 nm of 480 nm of 96.0%, transmittance at 500 nm (T 500) is transmittance at 95. 2% 600 nm (T 6 ..) is 93.8%, the transmittance at 700 nm (T 70 0) is 91.4%, chroma
  • a transparent touch panel device was obtained in the same manner as in Example 1. The device was almost colorless and transparent, and had excellent visibility even when installed on a color liquid crystal display. The image quality was clearly felt.
  • a glass substrate with a transparent conductive film was obtained in the same manner as in Example 1 except that the coating liquid for forming the third film was used.
  • the glass substrate with a transparent conductive film obtained in this manner has a surface resistance of 600 ⁇ / port and a maximum transmittance (T max ) in the wavelength range of 380 to 780 nm of 9440% at 440 nm.
  • the transmittance at 500 nm (T 50o ) is 94.0 %
  • the transmittance at 600 nm (T 600 ) is 92.4%
  • the transmittance at 700 nm (T 70 ) is 91.2%.
  • both surfaces of the glass substrate 2 contained 90% by weight or more of SiO 2 , a refractive index of 1.46, and a film thickness of 75 nm.
  • the second and fifth films were formed.
  • the glass substrate on which the second film and the fifth film thus obtained are formed has a maximum transmittance (T max ) in the wavelength region of 380 to 780 nm at 520 nm of 93.1%, and at 500 nm.
  • Transmittance (T 500 ) is 93.0%
  • Transmittance at 600 nm (T 600 ) is 92.
  • Transmittance at 700 nm (T 700 ) Power 91.4%
  • a transparent touch panel device was obtained in the same manner as in Example 1. The device was slightly yellowish, and when installed on a liquid crystal display, there was a clear lack of vividness. It was something you could feel.
  • Example 2 The same procedure as in Example 1 was carried out except that the surface of the glass substrate on which the third film was not formed was masked, and only one surface was formed.
  • the transparent conductive film was composed of the first, second, and third films. A glass substrate with a film was obtained. That is, this glass substrate with a transparent conductive film has no film on the back surface and has three layers formed only on the front side.
  • the present invention has the following configuration, and thus has the following effects.
  • the glass substrate with a transparent conductive film according to the present invention includes a first film containing at least 90% by weight of at least one or more metal oxides of Zr, Ti, Al, and Si on one surface of the glass substrate. , S a second film containing i O 2 of 90% by weight or more, I n, Sn, Zn, S b, a l, third film containing at least one kind of metal oxide 90 wt% or more of Y When And at least 90% by weight of at least one metal oxide of Zr, Ti, Al, Si on the other surface of the glass substrate. and the membrane, since the fifth layer containing S i 0 2 9 0 wt% or more is configured as made shape with at least sequentially laminated, and excellent high light-hue adjustability It is provided.
  • the method for producing a glass substrate with a transparent conductive film of the present invention includes: a metal chelate compound containing at least one metal of Zr, Ti, A1, Si on one surface of a glass substrate; An organic acid salt containing at least one metal, an inorganic acid salt containing at least one metal of the above metals, a hydrolyzable organometallic compound containing at least one metal of the above metals, and a hydrolyzate of the above organic metal compound After coating or printing a coating liquid comprising a base material and a solvent containing at least one or two of at least one or more metal oxides of the above-mentioned metals, and then drying and drying the first film Forming a metal chelate compound of Si, an organic acid salt containing Si, an inorganic acid salt containing Si, a hydrolyzable organic silicon compound, and a water solution of the above organic silicon compound on the upper surface of the first film.
  • Decomposed product, silicate After coating or printing a coating solution consisting of a main agent containing at least one member from the group consisting of a solvent and a solvent, it is dried to form a second film, and on the upper surface of the second film, In, Sn, Z a metal chelate compound containing at least one metal of n, Sb, Al, and Y; an organic acid salt containing at least one metal of the above metals; and an inorganic acid containing at least one metal of the above metals At least one of the group consisting of a salt, a hydrolyzable organometallic compound containing at least one metal of the above metals, a hydrolyzate of the above organometallic compound, and a metal oxide of at least one metal of the above metals After coating or printing a coating liquid comprising a main agent containing one kind and a solvent, drying and firing are performed to form a third film, and on the other surface of the glass substrate, Zr, Ti, A1, Si At least one metal A metal chel
  • the fourth layer and the fifth layer are formed on the back surface of the glass substrate with a transparent conductive film, reflection on the back surface in a specific wavelength range is reduced, and high translucency as an excellent touch panel device is obtained. It is possible to have hue adjustability.

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Abstract

Substrat de verre comportant des couches transparentes conductrices d'électricité et composées du substrat de verre (2) lui-même, d'une première couche (3) laminée sur une surface du substrat et contenant au moins un oxyde de métal tel que Zr, Ti, Al et Si selon une quantité égale ou supérieure à 90 % en poids, d'une deuxième couche (4) contenant SoO2 en quantité égale ou supérieure à 90 % en poids et d'une troisième couche (5) contenant au moins un oxyde de métal tel que In, Sn, Zn, Sb, Al et Y en quantité égale ou supérieure à 90 % en poids. L'autre surface de ce substrat (2) comporte dans l'ordre suivant, une quatrième couche (6) contenant au moins un oxyde de métal tel que Zr, Ti, Al et Si en quantité égale ou supérieure à 90 % en poids et une cinquième couche (7) contenant SiO2 en quantité égale ou supérieure à 90 % en poids.
PCT/JP2002/012258 2001-11-26 2002-11-25 Substrat de verre possedant une couche transparente electroconductrice et son procede de production WO2003045867A1 (fr)

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JP2001-358896 2001-11-26

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06293957A (ja) * 1993-02-10 1994-10-21 Nippon Soda Co Ltd 高抵抗化酸化インジウム膜
JPH07242442A (ja) * 1994-03-01 1995-09-19 Nippon Soda Co Ltd 透明導電膜付ガラスおよび透明導電膜の成膜方法
JPH1153114A (ja) * 1997-07-31 1999-02-26 Central Glass Co Ltd タッチパネルの基板用低反射ガラス

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06293957A (ja) * 1993-02-10 1994-10-21 Nippon Soda Co Ltd 高抵抗化酸化インジウム膜
JPH07242442A (ja) * 1994-03-01 1995-09-19 Nippon Soda Co Ltd 透明導電膜付ガラスおよび透明導電膜の成膜方法
JPH1153114A (ja) * 1997-07-31 1999-02-26 Central Glass Co Ltd タッチパネルの基板用低反射ガラス

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