WO2017130869A1 - Solution de noircissement pour dépôt électrolytique et procédé de fabrication d'un substrat conducteur - Google Patents

Solution de noircissement pour dépôt électrolytique et procédé de fabrication d'un substrat conducteur Download PDF

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Publication number
WO2017130869A1
WO2017130869A1 PCT/JP2017/002018 JP2017002018W WO2017130869A1 WO 2017130869 A1 WO2017130869 A1 WO 2017130869A1 JP 2017002018 W JP2017002018 W JP 2017002018W WO 2017130869 A1 WO2017130869 A1 WO 2017130869A1
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Prior art keywords
layer
copper
blackening
conductive substrate
plating solution
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PCT/JP2017/002018
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English (en)
Japanese (ja)
Inventor
下地　匠
志賀　大樹
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住友金属鉱山株式会社
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Priority to CN201780008194.1A priority Critical patent/CN108603302A/zh
Priority to JP2017564219A priority patent/JP7003665B2/ja
Priority to KR1020187020868A priority patent/KR102631091B1/ko
Publication of WO2017130869A1 publication Critical patent/WO2017130869A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/56—Electroplating: Baths therefor from solutions of alloys
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
    • C23C28/021—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material including at least one metal alloy layer
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
    • C23C28/023—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material only coatings of metal elements only
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/56—Electroplating: Baths therefor from solutions of alloys
    • C25D3/562—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/54—Electroplating of non-metallic surfaces
    • C25D5/56—Electroplating of non-metallic surfaces of plastics

Definitions

  • the present invention relates to a blackening plating solution and a method for producing a conductive substrate.
  • the capacitive touch panel converts information on the position of an adjacent object on the panel surface into an electrical signal by detecting a change in capacitance caused by the object adjacent to the panel surface. Since the conductive substrate used for the capacitive touch panel is installed on the surface of the display, the material of the conductive layer of the conductive substrate is required to have low reflectance and be difficult to be visually recognized.
  • a material for the conductive layer used for the capacitive touch panel a material having low reflectivity and not easily visible is used, and wiring is formed on a transparent substrate or a transparent film.
  • Patent Document 1 discloses a transparent conductive film including a polymer film and a transparent conductive film made of a metal oxide provided thereon by a vapor deposition method. The use of an indium oxide-tin oxide (ITO) film is disclosed.
  • ITO indium oxide-tin oxide
  • a display with a touch panel has been increased in screen size, and in response to this, a conductive substrate such as a transparent conductive film for a touch panel is required to have a large area.
  • ITO has a high electric resistance value, there is a problem that it cannot cope with an increase in the area of the conductive substrate.
  • the inventors of the present invention have studied the blackening treatment by the wet method because the vacuum environment as required by the dry method is not required, the equipment can be simplified and the productivity is excellent. It was. Specifically, it has been studied to form a blackened layer by a wet method using a plating solution containing Ni and Zn as main components.
  • the formed blackened layer is formed as a conductive layer.
  • the reactivity with the etching solution was higher than that of the copper layer.
  • the conductive substrate having a desired wiring pattern after forming a copper layer as a conductive layer and a blackened layer, it will be patterned by etching, but a copper layer for the etchant, Due to the difference in reactivity with the blackened layer, it may be difficult to pattern the blackened layer into a desired shape.
  • an object of one aspect of the present invention is to provide a blackening plating solution capable of forming a blackening layer that can be patterned into a desired shape when etched together with a copper layer.
  • a blackening plating solution having a zinc ion concentration of 0.34 g / l or more and a copper ion concentration of 0.20 g / l or more is provided.
  • a blackening plating solution capable of forming a blackening layer that can be patterned into a desired shape when etched together with a copper layer.
  • substrate which concerns on embodiment of this invention Sectional drawing of the electroconductive board
  • the blackening plating solution of this embodiment contains nickel ions, zinc ions, copper ions, amidosulfuric acid, and ammonia, and has a zinc ion concentration of 0.34 g / l or more and a copper ion concentration of 0.20 g / l. 1 or more.
  • a blackening layer formed by a wet method using a plating solution containing Ni and Zn as main components is higher in reactivity to the etching solution than the copper layer, and is etched together with the copper layer. It was difficult to form a pattern into a desired shape. Therefore, the inventors of the present invention have intensively studied a blackening plating solution capable of forming a blackening layer that can be patterned into a desired shape when etched together with a copper layer.
  • the inventors of the present invention made the blackening layer a layer containing nickel, zinc, and copper, thereby reacting the blackening layer to the etching solution. It was found that the desired shape can be obtained even when etching is performed simultaneously with the copper layer.
  • the blackening layer further containing copper suppresses the reactivity of the blackening layer to the etching solution, and even when etching is performed together with the copper layer, the copper layer and the blackening layer It was found that can be patterned into a desired shape.
  • the desired shape when the copper layer and the blackened layer are etched at the same time means, for example, a shape or pattern including a wiring having a wiring width of 10 ⁇ m or less.
  • the blackening plating solution of the present embodiment is preferably a plating solution that can form a layer containing nickel, zinc, and copper as metal components, and the blackening plating solution of the present embodiment includes nickel ions, Zinc ions and copper ions can be contained.
  • the blackening plating solution of the present embodiment can contain amidosulfuric acid that functions as a complexing agent and ammonia. By containing these components, reflection of light on the surface of the copper layer is suppressed. It is possible to obtain a blackening layer having a color suitable for the above.
  • the concentration of each component in the blackening plating solution is not particularly limited, but the zinc ion concentration is preferably 0.34 g / l or more, and more preferably 0.40 g / l or more.
  • the blackening layer has a color particularly suitable for suppressing the reflection of light on the surface of the copper layer, and the reflection of the conductive substrate This is because the rate can be suppressed.
  • the upper limit of the zinc ion concentration in the blackening plating solution is not particularly limited, but is preferably 3.0 g / l or less, and more preferably 1.5 g / l or less.
  • the copper ion concentration in the blackening plating solution is preferably 0.20 g / l or more, and more preferably 0.30 g / l or more. This is because when the copper ion concentration in the blackening plating solution is 0.20 g / l or more, the reactivity of the blackening layer to the etching solution is suppressed, and even when the blackening layer is etched together with the copper layer, the desired shape is obtained. This is because it can be patterned.
  • the upper limit value of the copper ion concentration in the blackening plating solution is not particularly limited, but is preferably 2.5 g / l or less, and more preferably 1.5 g / l or less.
  • the nickel ion concentration in the blackening plating solution is not particularly limited, but is preferably 2.0 g / l or more, and more preferably 5.0 g / l or more. This is because the nickel ion concentration in the blackening plating solution is set to 2.0 g / l or more so that the blackened layer has a color particularly suitable for suppressing light reflection on the surface of the copper layer. This is because it is possible to suppress the reflectance.
  • the upper limit of the nickel ion concentration in the blackening plating solution is not particularly limited, but is preferably, for example, 30.0 g / l or less, and more preferably 20.0 g / l or less.
  • the supply method of nickel ions, zinc ions, and copper ions is not particularly limited, and can be supplied in a salt state, for example.
  • a salt state for example.
  • sulfamate and sulfate can be preferably used.
  • the same kind of salt may be used for each metal element, and different kinds of salts may be used at the same time.
  • a blackening plating solution can be prepared using the same kind of salt such as nickel sulfate, zinc sulfate, and copper sulfate.
  • a blackening plating solution can be prepared by simultaneously using different kinds of salts such as nickel sulfate, zinc sulfate, and copper sulfamate.
  • the blackening plating solution of this embodiment can contain amidosulfuric acid and ammonia in addition to nickel ions, zinc ions, and copper ions.
  • the content of amidosulfuric acid and ammonia in the blackening plating solution of the present embodiment is not particularly limited, and can be arbitrarily selected according to the degree of suppression of reflectance required for the blackening layer to be formed. can do.
  • the concentration of amidosulfuric acid in the blackening plating solution is not particularly limited.
  • it is preferably 1 g / l or more and 50 g / l or less, and preferably 5 g / l or more and 20 g / l or less.
  • ammonia also has a function of adjusting the pH of the blackening plating solution of the present embodiment. That is, the pH of the blackening plating solution of this embodiment can be adjusted with ammonia.
  • the pH range of the blackening plating solution of the present embodiment is not particularly limited, but is preferably 4.0 or more and 6.5 or less, for example.
  • a blackening layer having a color capable of particularly suppressing light reflection can be formed by setting the pH of the blackening plating solution to 4.0 or more.
  • a part of the components of the blackening plating solution is deposited, or when the blackening layer is formed using the blackening plating solution, It is because it can suppress more reliably that a color nonuniformity arises in a formation layer, and is preferable.
  • a blackened layer that can be patterned into a desired shape when etched together with the copper layer can be formed.
  • the blackening plating solution of this embodiment can be used suitably when forming the blackening layer which can fully suppress the reflection of the light in the copper layer surface of an electroconductive board
  • the conductive substrate of the present embodiment includes a transparent substrate, a copper layer disposed on at least one surface of the transparent substrate, a blackened layer formed on the copper layer using a blackened plating solution, Can have.
  • the conductive substrate in the present embodiment is a substrate having a copper layer and a blackened layer on the surface of the transparent base before patterning the copper layer and the like, and a substrate obtained by patterning the copper layer and the like, that is, And a wiring board.
  • the transparent substrate is not particularly limited, and a transparent substrate such as a resin substrate (resin film) that transmits visible light or a glass substrate can be preferably used.
  • a transparent substrate such as a resin substrate (resin film) that transmits visible light or a glass substrate can be preferably used.
  • a resin such as a polyamide resin, a polyethylene terephthalate resin, a polyethylene naphthalate resin, a cycloolefin resin, a polyimide resin, or a polycarbonate resin can be preferably used.
  • PET polyethylene terephthalate
  • COP cycloolefin polymer
  • PEN polyethylene naphthalate
  • polyamide, polyimide, polycarbonate, and the like can be more preferably used as the material for the resin substrate that transmits visible light.
  • the thickness of the transparent base material is not particularly limited, and can be arbitrarily selected according to the strength, capacitance, light transmittance, and the like required for a conductive substrate.
  • the thickness of the transparent substrate can be, for example, 10 ⁇ m or more and 200 ⁇ m or less.
  • the thickness of the transparent substrate is preferably 20 ⁇ m or more and 120 ⁇ m or less, and more preferably 20 ⁇ m or more and 100 ⁇ m or less.
  • the thickness of the transparent substrate is preferably 20 ⁇ m or more and 50 ⁇ m or less.
  • the total light transmittance of the transparent substrate is preferably higher.
  • the total light transmittance is preferably 30% or more, and more preferably 60% or more.
  • the visibility of the display can be sufficiently secured.
  • the total light transmittance of the transparent substrate can be evaluated by the method defined in JIS K 7361-1.
  • the method for forming the copper layer on the transparent substrate is not particularly limited, it is preferable not to dispose an adhesive between the transparent substrate and the copper layer in order not to reduce the light transmittance. That is, the copper layer is preferably formed directly on at least one surface of the transparent substrate. In addition, when arrange
  • the copper layer preferably has a copper thin film layer.
  • the copper layer may have a copper thin film layer and a copper plating layer.
  • a copper thin film layer can be formed on a transparent substrate by a dry plating method, and the copper thin film layer can be used as a copper layer. Thereby, a copper layer can be directly formed on the transparent substrate without using an adhesive.
  • a dry plating method for example, a sputtering method, a vapor deposition method, an ion plating method, or the like can be preferably used.
  • the copper thin film layer and the copper plating layer are formed by forming a copper plating layer by an electroplating method which is a kind of wet plating method using the copper thin film layer as a power feeding layer. It can also be set as the copper layer which has. Since the copper layer has the copper thin film layer and the copper plating layer, the copper layer can be directly formed on the transparent substrate without using an adhesive.
  • the thickness of the copper layer is not particularly limited, and when the copper layer is used as a wiring, it can be arbitrarily selected according to the magnitude of the current supplied to the wiring, the wiring width, and the like.
  • the thickness of a copper layer is 5 micrometers or less, and it is more preferable that it is 3 micrometers or less.
  • the copper layer preferably has a thickness of 50 nm or more, more preferably 60 nm or more, and 150 nm. More preferably, it is the above.
  • a copper layer has a copper thin film layer and a copper plating layer as mentioned above, it is preferable that the sum total of the thickness of a copper thin film layer and the thickness of a copper plating layer is the said range.
  • the thickness of the copper thin film layer is not particularly limited. The following is preferable.
  • the copper layer can be used as wiring by patterning it into a desired wiring pattern, for example. And since a copper layer can make an electrical resistance value lower than ITO conventionally used as a transparent conductive film, the electrical resistance value of an electroconductive board
  • substrate can be made small by providing a copper layer.
  • the blackening layer can be formed using the blackening plating solution described above. For this reason, for example, after forming the copper layer, it can be formed on the upper surface of the copper layer by a wet method such as an electrolytic plating method.
  • the thickness of the blackening layer is not particularly limited, but is preferably 30 nm or more, for example, and more preferably 50 nm or more. This is because light reflection on the surface of the copper layer can be particularly suppressed by setting the thickness of the blackened layer to 30 nm or more.
  • the upper limit of the thickness of the blackening layer is not particularly limited, but even if it is thicker than necessary, the time required for film formation and the time required for etching when forming the wiring are increased, resulting in an increase in cost. Will be invited.
  • the thickness of the blackened layer is preferably 120 nm or less, and more preferably 90 nm or less.
  • the blackening layer when the blackening layer is formed by the blackening plating solution described above, the blackening layer can be a layer containing nickel, zinc, and copper. Moreover, the component derived from the various additional components contained in the blackening plating solution as described above can also be contained.
  • the conductive substrate can be provided with any layer other than the above-mentioned transparent base material, copper layer, and blackening layer.
  • an adhesion layer can be provided.
  • the copper layer can be formed on the transparent substrate, but when the copper layer is directly formed on the transparent substrate, the adhesion between the transparent substrate and the copper layer may not be sufficient. . For this reason, when forming a copper layer directly on the upper surface of a transparent base material, a copper layer may peel from a transparent base material at the time of a manufacture process or use.
  • an adhesion layer can be disposed on the transparent substrate in order to improve the adhesion between the transparent substrate and the copper layer. That is, it can also be set as the electroconductive board
  • the adhesion layer between the transparent substrate and the copper layer By disposing the adhesion layer between the transparent substrate and the copper layer, the adhesion between the transparent substrate and the copper layer can be improved, and the copper layer can be prevented from peeling from the transparent substrate.
  • the adhesion layer can function as a blackening layer. For this reason, it becomes possible to also suppress reflection of the light of a copper layer by the light from the lower surface side of a copper layer, ie, the transparent base material side.
  • the material constituting the adhesion layer is not particularly limited.
  • the adhesion between the transparent substrate and the copper layer, the degree of suppression of light reflection on the required copper layer surface, and a conductive substrate are used. It can be arbitrarily selected according to the degree of stability to the environment (for example, humidity and temperature).
  • the adhesion layer preferably contains at least one metal selected from, for example, Ni, Zn, Mo, Ta, Ti, V, Cr, Fe, Co, W, Cu, Sn, and Mn.
  • the adhesion layer may further contain one or more elements selected from carbon, oxygen, hydrogen, and nitrogen.
  • the adhesion layer can also include a metal alloy containing at least two kinds of metals selected from Ni, Zn, Mo, Ta, Ti, V, Cr, Fe, Co, W, Cu, Sn, and Mn. Also in this case, the adhesion layer can further include one or more elements selected from carbon, oxygen, hydrogen, and nitrogen.
  • a metal alloy containing at least two kinds of metals selected from Ni, Zn, Mo, Ta, Ti, V, Cr, Fe, Co, W, Cu, Sn, and Mn a Cu—Ti—Fe alloy is used as a metal alloy containing at least two kinds of metals selected from Ni, Zn, Mo, Ta, Ti, V, Cr, Fe, Co, W, Cu, Sn, and Mn.
  • a Cu—Ti—Fe alloy is used as a metal alloy containing at least two kinds of metals selected from Ni, Zn, Mo, Ta, Ti, V, Cr, Fe, Co, W, Cu, Sn, and Mn.
  • the method for forming the adhesion layer is not particularly limited, but it is preferable to form the film by a dry plating method.
  • a dry plating method for example, a sputtering method, an ion plating method, a vapor deposition method, or the like can be preferably used.
  • the adhesion layer is formed by a dry method, it is more preferable to use a sputtering method because the film thickness can be easily controlled.
  • one or more elements selected from carbon, oxygen, hydrogen, and nitrogen can be added to the adhesion layer, and in this case, the reactive sputtering method can be more preferably used.
  • the adhesion layer includes one or more elements selected from carbon, oxygen, hydrogen, and nitrogen
  • one or more elements selected from carbon, oxygen, hydrogen, and nitrogen in the atmosphere when forming the adhesion layer Can be added to the adhesion layer.
  • carbon monoxide gas and / or carbon dioxide gas when adding oxygen, oxygen gas, when adding hydrogen, hydrogen gas and / or water
  • nitrogen gas can be added to the atmosphere when dry plating is performed.
  • a gas containing one or more elements selected from carbon, oxygen, hydrogen, and nitrogen is preferably added to an inert gas and used as an atmosphere gas during dry plating.
  • an inert gas For example, argon can be used preferably.
  • the adhesion layer By forming the adhesion layer by the dry plating method as described above, the adhesion between the transparent substrate and the adhesion layer can be enhanced. And since an adhesion layer can contain a metal as a main component, for example, its adhesiveness with a copper layer is also high. For this reason, peeling of a copper layer can be suppressed by arrange
  • the thickness of the adhesion layer is not particularly limited, but is preferably 3 nm to 50 nm, for example, more preferably 3 nm to 35 nm, and still more preferably 3 nm to 33 nm.
  • the thickness of the adhesion layer is preferably 3 nm or more as described above.
  • the upper limit value of the thickness of the adhesion layer is not particularly limited, but even if it is thicker than necessary, the time required for film formation and the time required for etching when forming the wiring are increased, resulting in an increase in cost. Will be invited.
  • the thickness of the adhesion layer is preferably 50 nm or less as described above, more preferably 35 nm or less, and further preferably 33 nm or less.
  • the conductive substrate of the present embodiment can have a transparent base material, a copper layer, and a blackening layer. Moreover, it can also have layers, such as a contact
  • FIG. 1A, FIG. 1B, FIG. 2A, and FIG. 2B show examples of cross-sectional views of the conductive substrate of this embodiment on a plane parallel to the lamination direction of the transparent base material, the copper layer, and the blackening layer.
  • the conductive substrate of the present embodiment can have a structure in which, for example, a copper layer and a blackened layer are laminated in that order from the transparent substrate side on at least one surface of the transparent substrate.
  • the copper layer 12 and the blackening layer 13 may be laminated one layer at a time on the one surface 11a side of the transparent base material 11. it can.
  • copper layer 12A, 12B and black layer are respectively provided in the one surface 11a side of the transparent base material 11, and the other surface (other surface) 11b side.
  • the layers 13A and 13B can be stacked one by one in that order.
  • an adhesion layer may be provided.
  • the adhesion layer 14, the copper layer 12, and the blackening layer 13 are laminated in that order on the one surface 11a side of the transparent base material 11. be able to.
  • a structure in which an adhesive layer, a copper layer, and a blackening layer are laminated on both surfaces of the transparent substrate 11 can be employed.
  • the adhesion layers 14A and 14B and the copper layers 12A and 12B are respectively formed on the one surface 11a side and the other surface 11b side of the transparent base material 11.
  • the blackening layers 13A and 13B can be stacked in that order.
  • FIG. 1B and FIG. 2B when a copper layer, a blackened layer, etc. are laminated on both sides of the transparent substrate, the layers laminated on the upper and lower sides of the transparent substrate 11 are symmetrical with the transparent substrate 11 as the symmetry plane.
  • the example which arranged in this way was shown, it is not limited to the form which concerns.
  • the configuration on the one surface 11a side of the transparent substrate 11 is the same as the configuration of FIG. 1B, in which the copper layer 12A and the blackening layer 13A are laminated in that order without providing the adhesion layer 14A.
  • the layers laminated on the top and bottom of the transparent substrate 11 may be asymmetrical.
  • substrate of this embodiment by providing a copper layer and a blackening layer on a transparent base material, reflection of the light by a copper layer is suppressed and the reflectance of an electroconductive board
  • the degree of reflectivity of the conductive substrate of the present embodiment is not particularly limited.
  • the reflectivity is lower. Is good.
  • the average reflectance of light having a wavelength of 400 nm to 700 nm is preferably 40% or less, and more preferably 35% or less.
  • the reflectance can be measured by irradiating the blackened layer of the conductive substrate with light. Specifically, for example, as shown in FIG. 1A, when the copper layer 12 and the blackened layer 13 are laminated in this order on the one surface 11 a side of the transparent substrate 11, the blackened layer 13 is irradiated so that the blackened layer 13 is irradiated with light.
  • the surface A can be irradiated with light and measured.
  • light having a wavelength of 400 nm or more and 700 nm or less is irradiated to the blackened layer 13 of the conductive substrate, for example, at a wavelength of 1 nm as described above, and the average value of the measured values is used as the reflectance of the conductive substrate. be able to.
  • the conductive substrate of this embodiment can be preferably used as a conductive substrate for a touch panel.
  • the conductive substrate can be configured to have mesh-like wiring.
  • the conductive substrate provided with the mesh-like wiring can be obtained by etching the copper layer and the blackening layer of the conductive substrate of the present embodiment described so far.
  • a mesh-like wiring can be formed by two-layer wiring.
  • FIG. 3 shows a view of the conductive substrate 30 provided with mesh-like wiring as viewed from the upper surface side in the stacking direction of the copper layer or the like.
  • the transparent substrate and the copper layer are patterned so that the wiring pattern can be easily understood. Description of layers other than the wirings 31A and 31B formed in the same manner is omitted.
  • the wiring 31B seen through the transparent base material 11 is also shown.
  • the conductive substrate 30 shown in FIG. 3 has a transparent base material 11, a plurality of wirings 31A parallel to the Y-axis direction in the drawing, and wirings 31B parallel to the X-axis direction.
  • the wirings 31A and 31B are formed by etching a copper layer, and a blackening layer (not shown) is formed on the upper or lower surface of the wirings 31A and 31B. The blackened layer is etched in the same shape as the wirings 31A and 31B.
  • the arrangement of the transparent substrate 11 and the wirings 31A and 31B is not particularly limited.
  • positioning with the transparent base material 11 and wiring is shown to FIG. 4A and FIG. 4B.
  • 4A and 4B are cross-sectional views taken along line AA ′ of FIG.
  • wirings 31A and 31B may be arranged on the upper and lower surfaces of the transparent base material 11, respectively.
  • blackening layers 32A and 32B etched in the same shape as the wiring are arranged on the upper surface of the wiring 31A and the lower surface of 31B.
  • a pair of transparent base materials 11 is used, wirings 31A and 31B are arranged on the upper and lower surfaces across one transparent base material 11, and one wiring 31B is a transparent base material. 11 may be arranged. Also in this case, blackened layers 32A and 32B etched in the same shape as the wiring are disposed on the upper surfaces of the wirings 31A and 31B.
  • an adhesion layer can be provided in addition to the copper layer and the blackened layer. Therefore, in either case of FIG. 4A or FIG. 4B, for example, an adhesion layer can be provided between the wiring 31 ⁇ / b> A and / or the wiring 31 ⁇ / b> B and the transparent substrate 11. When the adhesion layer is provided, it is preferable that the adhesion layer is also etched in the same shape as the wirings 31A and 31B.
  • the conductive substrate having the mesh-like wiring shown in FIGS. 3 and 4A is, for example, a conductive substrate having copper layers 12A and 12B and blackening layers 13A and 13B on both surfaces of the transparent base 11 as shown in FIG. 1B. It can be formed from a conductive substrate.
  • the conductive substrate of FIG. 1B is used as an example.
  • the copper layer 12A and the blackened layer 13A on the one surface 11a side of the transparent base material 11 are parallel to the Y-axis direction in FIG. 1B.
  • Etching is performed so that a plurality of linear patterns are arranged at predetermined intervals along the X-axis direction.
  • the X-axis direction in FIG. 1B means a direction parallel to the width direction of each layer.
  • the Y-axis direction in FIG. 1B means a direction perpendicular to the paper surface in FIG. 1B.
  • a plurality of linear patterns parallel to the X-axis direction in FIG. 1B are arranged along the Y-axis direction at predetermined intervals on the copper layer 12B and the blackening layer 13B on the other surface 11b side of the transparent substrate 11. Etching is performed so as to be disposed.
  • the conductive substrate having the mesh-like wiring shown in FIGS. 3 and 4A can be formed.
  • the etching of both surfaces of the transparent substrate 11 can be performed simultaneously. That is, the etching of the copper layers 12A and 12B and the blackening layers 13A and 13B may be performed simultaneously.
  • the conductive substrate having an adhesion layer patterned in the same shape as the wirings 31A and 31B between the wirings 31A and 31B and the transparent base material 11 is the conductive substrate shown in FIG. 2B. It can be produced by etching in the same manner.
  • FIG. 3 can also be formed by using two conductive substrates shown in FIG. 1A or FIG. 2A.
  • a case where the two conductive substrates shown in FIG. 1A are used will be described as an example.
  • a plurality of copper layers 12 and blackened layers 13 are provided in parallel to the X-axis direction. Etching is performed so that the linear patterns are arranged along the Y-axis direction at a predetermined interval. Then, the conductive substrate having mesh-like wiring is obtained by bonding the two conductive substrates so that the linear patterns formed on the respective conductive substrates intersect with each other by the etching process. be able to.
  • the surface to be bonded when the two conductive substrates are bonded is not particularly limited.
  • the surface A in FIG. 1A in which the copper layer 12 or the like is laminated and the other surface 11b in FIG. 1A in which the copper layer 12 or the like is not laminated are bonded to form the structure shown in FIG. 4B. You can also.
  • the other surfaces 11b in FIG. 1A where the copper layer 12 or the like of the transparent base material 11 is not laminated can be bonded together so that the cross section has the structure shown in FIG. 4A.
  • FIG. 1A a conductive substrate having an adhesion layer patterned in the same shape as the wirings 31A and 31B between the wirings 31A and 31B and the transparent base material 11 is shown in FIG. 1A. It can be manufactured by using the conductive substrate shown in FIG. 2A instead of the conductive substrate.
  • the width of the wiring and the distance between the wirings in the conductive substrate having the mesh-like wiring shown in FIG. 3, FIG. 4A and FIG. 4B are not particularly limited. You can choose.
  • the conductive substrate of the present embodiment has a blackening layer formed using the blackening plating solution described above, and the blackening layer and the copper layer were simultaneously etched and patterned. Even in this case, the blackened layer and the copper layer can be patterned into a desired shape. Specifically, for example, a wiring having a wiring width of 10 ⁇ m or less can be formed. For this reason, it is preferable that the conductive substrate of this embodiment includes a wiring having a wiring width of 10 ⁇ m or less.
  • the lower limit value of the wiring width is not particularly limited, but can be 3 ⁇ m or more, for example.
  • 4 ⁇ / b> A, and 4 ⁇ / b> B show examples in which a mesh-like wiring (wiring pattern) is formed by combining linear wirings, but the present invention is not limited to such a form.
  • the wiring that constitutes can be of any shape.
  • the shape of the wiring constituting the mesh-like wiring pattern can be changed to various shapes such as jagged lines (zigzag straight lines) so that moire (interference fringes) does not occur between the images on the display.
  • a conductive substrate having a mesh-like wiring composed of two layers of wiring can be preferably used as a conductive substrate for a projected capacitive touch panel, for example.
  • the conductive substrate of the present embodiment described above has a structure in which a blackened layer is laminated on a copper layer formed on at least one surface of a transparent base material. Since the blackening layer is formed by using the blackening plating solution described above, the blackening layer can be easily formed when the copper layer and the blackening layer are patterned by etching as described above. It can be patterned into a desired shape.
  • the blackening layer included in the conductive substrate of the present embodiment can sufficiently suppress the reflection of light on the surface of the copper layer and can be a conductive substrate with a suppressed reflectance. Moreover, the visibility of a display can be improved when used for applications such as a touch panel.
  • the blackening layer can be formed by the wet method using the blackening plating solution described above, the conductive substrate can be formed with higher productivity than the case of forming the blackening layer using the conventional dry method. Can be produced. (Method for producing conductive substrate) Next, a configuration example of the method for manufacturing the conductive substrate according to the present embodiment will be described.
  • the manufacturing method of the conductive substrate of this embodiment can have the following processes.
  • the blackening plating solution includes the blackening plating solution described above, specifically, nickel ions, zinc ions, copper ions, amidosulfuric acid, and ammonia, and the zinc ion concentration is 0.34 g / l. As described above, a blackening plating solution having a copper ion concentration of 0.20 g / l or more can be used.
  • the conductive substrate described above can be suitably manufactured by the method for manufacturing a conductive substrate of the present embodiment. For this reason, since it can be set as the structure similar to the case of the electroconductive board
  • the transparent base material used for the copper layer forming step can be prepared in advance.
  • a transparent base material such as a resin substrate (resin film) that transmits visible light or a glass substrate can be preferably used as described above.
  • the transparent base material can be cut into an arbitrary size in advance if necessary.
  • the copper layer preferably has a copper thin film layer as described above.
  • the copper layer can also have a copper thin film layer and a copper plating layer.
  • a copper layer formation process can have a process of forming a copper thin film layer, for example with a dry plating method.
  • the copper layer forming step includes a step of forming a copper thin film layer by a dry plating method, a step of forming a copper plating layer by an electroplating method which is a kind of wet plating method, using the copper thin film layer as a power feeding layer, You may have.
  • the dry plating method used in the step of forming the copper thin film layer is not particularly limited, and for example, an evaporation method, a sputtering method, an ion plating method, or the like can be used.
  • a vapor deposition method a vacuum vapor deposition method can be used preferably.
  • the dry plating method used in the step of forming the copper thin film layer it is more preferable to use the sputtering method because the film thickness is particularly easy to control.
  • a copper plating layer can be formed by supplying a base material on which a copper thin film layer is formed in a plating tank containing a copper plating solution and controlling the current density and the conveyance speed of the base material.
  • the nickel ion, zinc ion, copper ion, amidosulfuric acid, and ammonia described above are included, the zinc ion concentration is 0.34 g / l or more, and the copper ion concentration is 0.20 g.
  • a blackened layer can be formed using a blackened plating solution that is at least 1 / l.
  • the blackened layer can be formed by a wet method. Specifically, for example, a blackened layer can be formed on the copper layer by an electrolytic plating method in a plating tank containing the blackened plating solution described above using a copper layer as a power feeding layer. In this way, by using the copper layer as a power feeding layer and forming the blackened layer by electrolytic plating, the blackened layer can be formed on the entire surface of the copper layer opposite to the surface facing the transparent substrate.
  • an optional step can be further performed in addition to the above-described steps.
  • an adhesion layer forming step of forming an adhesion layer on the surface of the transparent substrate on which the copper layer is formed can be performed.
  • the copper layer forming step can be carried out after the adhesion layer forming step, and in the copper layer forming step, copper is applied to the substrate on which the adhesion layer is formed on the transparent substrate in this step.
  • a thin film layer can be formed.
  • the method for forming the adhesion layer is not particularly limited, but it is preferable to form the film by a dry plating method.
  • a dry plating method for example, a sputtering method, an ion plating method, a vapor deposition method, or the like can be preferably used.
  • the adhesion layer is formed by a dry method, it is more preferable to use a sputtering method because the film thickness can be easily controlled.
  • one or more elements selected from carbon, oxygen, hydrogen, and nitrogen can be added to the adhesion layer, and in this case, the reactive sputtering method can be more preferably used.
  • the conductive substrate obtained by the conductive substrate manufacturing method of the present embodiment can be used for various applications such as a touch panel. And when using for various uses, it is preferable that the copper layer and blackening layer which are contained in the electroconductive board
  • the copper layer and the blackening layer, and in some cases, the adhesion layer can be patterned in accordance with, for example, a desired wiring pattern.
  • the copper layer and the blackening layer, and in some cases, the adhesion layer can be patterned in the same shape. It is preferable that
  • substrate of this embodiment can have the patterning process which patterns a copper layer and a blackening layer.
  • the patterning step can be a step of patterning the adhesion layer, the copper layer, and the blackening layer.
  • the specific procedure of the patterning step is not particularly limited, and can be performed by an arbitrary procedure.
  • a resist having a desired pattern is arranged on the surface A on the blackened layer 13.
  • a resist placement step can be performed.
  • an etching step of supplying an etching solution to the surface A on the blackened layer 13, that is, the surface side where the resist is disposed can be performed.
  • the etching solution used in the etching step is not particularly limited.
  • the blackened layer formed by the conductive substrate manufacturing method of the present embodiment exhibits almost the same reactivity to the etching solution as the copper layer.
  • the etching liquid used in an etching step is not specifically limited,
  • the etching liquid generally used for the etching of a copper layer can be used preferably.
  • etching solution for example, a mixed aqueous solution containing one or more selected from sulfuric acid, hydrogen peroxide (hydrogen peroxide solution), hydrochloric acid, cupric chloride, and ferric chloride can be preferably used.
  • the content of each component in the etching solution is not particularly limited.
  • the etching solution can be used at room temperature, but it can also be used by heating in order to increase the reactivity. For example, it can be used by heating to 40 ° C. or more and 50 ° C. or less.
  • a patterning process is performed to pattern the conductive substrate 10B in which the copper layers 12A and 12B and the blackening layers 13A and 13B are laminated on the one surface 11a and the other surface 11b of the transparent substrate 11.
  • a resist placement step of placing a resist having a desired pattern on the surface A and the surface B on the blackening layers 13A and 13B can be performed.
  • an etching step of supplying an etching solution to the surface A and the surface B on the blackening layers 13A and 13B, that is, the surface on which the resist is disposed can be performed.
  • the pattern formed in the etching step is not particularly limited, and can be an arbitrary shape.
  • the pattern is formed so that the copper layer 12 and the blackened layer 13 include a plurality of straight lines or jagged lines (zigzag straight lines) as described above. Can do.
  • a pattern can be formed so as to form a mesh-like wiring with the copper layer 12A and the copper layer 12B.
  • a lamination step of laminating two or more patterned conductive substrates can be performed.
  • laminating for example, by laminating so that the pattern of the copper layer of each conductive substrate intersects, it is also possible to obtain a laminated conductive substrate provided with mesh-like wiring.
  • the method of fixing two or more laminated conductive substrates is not particularly limited, but can be fixed by, for example, an adhesive.
  • the conductive substrate obtained by the above-described method for manufacturing a conductive substrate according to this embodiment has a structure in which a blackening layer is stacked on a copper layer formed on at least one surface of a transparent base material. . Since the blackening layer is formed by using the blackening plating solution described above, the blackening layer can be easily formed when the copper layer and the blackening layer are patterned by etching as described above. It can be patterned into a desired shape.
  • the blackening layer included in the conductive substrate obtained by the method for manufacturing the conductive substrate of the present embodiment is a conductive substrate that sufficiently suppresses reflection of light on the surface of the copper layer and suppresses reflectance. Can do. For this reason, when it uses for uses, such as a touch panel, for example, the visibility of a display can be improved.
  • the blackening layer can be formed by the wet method using the blackening plating solution described above, the conductive substrate can be formed with higher productivity than the case of forming the blackening layer using the conventional dry method. Can be produced.
  • a conductive substrate having the structure shown in FIG. 1A was produced.
  • the reflectance measurement is performed with an incident angle of 5 ° and a light receiving angle of 5 ° with respect to the surface A of the blackened layer 13 of the conductive substrate 10A shown in FIG.
  • the regular reflectance was measured by irradiation, and the average value was defined as the reflectance (average reflectance) of the conductive substrate.
  • Etching characteristics a dry film resist (Hitachi Kasei RY3310) was attached to the blackened layer surface of the conductive substrate obtained in the following experimental examples by a laminating method.
  • the sample was immersed in an etching solution of 10% by weight sulfuric acid and 3% by weight of hydrogen peroxide at 30 ° C. for 40 seconds, and then the dry film resist was stripped and removed with an aqueous sodium hydroxide solution.
  • the obtained sample was observed with a 200-fold microscope, and the minimum value of the wiring width of the metal wiring remaining on the conductive substrate was determined.
  • Experimental Examples 1 to 13 are examples, and Experimental Examples 14 and 15 are comparative examples.
  • [Experimental Example 1] (1) Blackening plating solution In Experimental Example 1, a blackening plating solution containing nickel ions, zinc ions, copper ions, amidosulfuric acid, and ammonia was prepared. In addition, nickel ion, zinc ion, and copper ion were supplied to the blackening plating solution by adding nickel sulfate hexahydrate, zinc sulfate heptahydrate, and copper sulfate pentahydrate.
  • the concentration of nickel ions in the blackening plating solution is 9.9 g / l
  • the concentration of zinc ions is 1.09 g / L
  • the concentration of copper ions is 0.20 g / l
  • the concentration of amidosulfuric acid is 11 g / l.
  • a copper layer was formed on one side of a long transparent substrate made of polyethylene terephthalate resin (PET) having a length of 100 m, a width of 500 mm, and a thickness of 100 ⁇ m.
  • PET polyethylene terephthalate resin
  • the transparent base material made of polyethylene terephthalate resin used as the transparent base material was evaluated to have a total light transmittance of 97% when evaluated by the method defined in JIS K 7361-1.
  • a copper thin film layer forming step and a copper plating layer forming step were performed.
  • the above-mentioned transparent base material was used as a base material, and a copper thin film layer was formed on one surface of the transparent base material.
  • the above-mentioned transparent base material which was previously heated to 60 ° C. to remove moisture, was placed in the chamber of the sputtering apparatus.
  • Electric power was supplied to a copper target set in advance on the cathode of the sputtering apparatus, and a copper thin film layer was formed on one surface of the transparent substrate so as to have a thickness of 0.2 ⁇ m.
  • a copper plating layer was formed in the copper plating layer forming step.
  • the copper plating layer was formed by electroplating so that the thickness of the copper plating layer was 0.3 ⁇ m.
  • a copper layer having a thickness of 0.5 ⁇ m was formed as a copper layer.
  • the substrate formed in the copper layer forming step and having a 0.5 ⁇ m thick copper layer formed on the transparent substrate was immersed in 20 g / l sulfuric acid for 30 sec and washed, and then the following blackened layer forming step was performed. .
  • Blackening layer forming process a blackened layer was formed on one surface of the copper layer by electrolytic plating using the blackened plating solution of the above-described experimental example.
  • the blackening layer was formed by performing electrolytic plating under the conditions that the temperature of the blackening plating solution was 40 ° C., the current density was 0.2 A / dm 2 , and the plating time was 100 sec.
  • the film thickness of the formed blackened layer was 70 nm.
  • Tables 2 and 3 show the evaluation results of the etching characteristics, and shows the minimum resist width in which the metal wiring remains.
  • Table 3 shows the evaluation results of the reflectance.
  • the zinc ion concentration is 0.34 g / l and the copper ion concentration is 0.31 g / l.
  • a conductive substrate was prepared and evaluated in the same manner as in Experimental Example 1 except that the blackening plating solution prepared in each experimental example was used when forming the blackened layer.
  • the conductive substrate having the blackened layer formed using the blackened plating solution of Experimental Examples 1 to 13 has an average value of the regular reflectance of light having a wavelength of 400 nm to 700 nm. It was confirmed that the (reflectance) was 40% or less.
  • Experimental Examples 14 and 15 which are comparative examples, it was confirmed that a metal wiring having a wiring width of 10 ⁇ m could not be formed. Therefore, it was confirmed that when a blackened layer was formed using these blackened plating solutions and etched together with the copper layer, it was difficult to pattern the blackened layer into a desired shape. Moreover, about the experiment example 15, it has confirmed that the average value (reflectance) of the regular reflectance of light with a wavelength of 400 nm or more and 700 nm or less exceeded 40%.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrochemistry (AREA)
  • Mechanical Engineering (AREA)
  • Laminated Bodies (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
  • Manufacturing Of Printed Wiring (AREA)

Abstract

L'invention concerne une solution de noircissement pour dépôt électrolytique contenant des ions nickel, des ions zinc, des ions cuivre, de l'acide amidosulfurique et de l'ammoniac, la concentration en ions zinc étant égale ou supérieure à 0,34 g/l et la concentration en ions cuivre étant égale ou supérieure à 0,20 g/l.
PCT/JP2017/002018 2016-01-29 2017-01-20 Solution de noircissement pour dépôt électrolytique et procédé de fabrication d'un substrat conducteur WO2017130869A1 (fr)

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CN201780008194.1A CN108603302A (zh) 2016-01-29 2017-01-20 黑化镀液、导电性基板的制造方法
JP2017564219A JP7003665B2 (ja) 2016-01-29 2017-01-20 黒化めっき液、導電性基板の製造方法
KR1020187020868A KR102631091B1 (ko) 2016-01-29 2017-01-20 흑화 도금액 및 도전성 기판 제조방법

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WO2019163070A1 (fr) * 2018-02-22 2019-08-29 コニカミノルタ株式会社 Procédé de formation de motif

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CN111727669A (zh) * 2018-02-22 2020-09-29 柯尼卡美能达株式会社 图案形成方法
JPWO2019163070A1 (ja) * 2018-02-22 2021-02-04 コニカミノルタ株式会社 パターン形成方法
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JP7003665B2 (ja) 2022-01-20
JPWO2017130869A1 (ja) 2018-11-22
KR102631091B1 (ko) 2024-01-29
TW201739968A (zh) 2017-11-16
TWI791429B (zh) 2023-02-11
CN108603302A (zh) 2018-09-28

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