WO2017164209A1 - Film conducteur transparent stratifié, film de câblage stratifié, et procédé de fabrication d'un film de câblage stratifié - Google Patents

Film conducteur transparent stratifié, film de câblage stratifié, et procédé de fabrication d'un film de câblage stratifié Download PDF

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Publication number
WO2017164209A1
WO2017164209A1 PCT/JP2017/011343 JP2017011343W WO2017164209A1 WO 2017164209 A1 WO2017164209 A1 WO 2017164209A1 JP 2017011343 W JP2017011343 W JP 2017011343W WO 2017164209 A1 WO2017164209 A1 WO 2017164209A1
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Prior art keywords
film
transparent conductive
atomic
laminated
conductive oxide
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PCT/JP2017/011343
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English (en)
Japanese (ja)
Inventor
弘実 中澤
石井　博
悠人 歳森
齋藤　淳
林　雄二郎
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三菱マテリアル株式会社
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Priority claimed from JP2017024386A external-priority patent/JP6888318B2/ja
Application filed by 三菱マテリアル株式会社 filed Critical 三菱マテリアル株式会社
Priority to EP17770249.5A priority Critical patent/EP3435385B1/fr
Priority to US16/086,165 priority patent/US20190105872A1/en
Priority to CN201780019852.7A priority patent/CN108885922B/zh
Priority to KR1020187025939A priority patent/KR102333536B1/ko
Publication of WO2017164209A1 publication Critical patent/WO2017164209A1/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
    • H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
    • 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
    • B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables

Definitions

  • the present invention relates to a laminated transparent conductive film that can be used as a transparent electrode film such as a display or a touch panel, a laminated wiring film comprising the laminated transparent conductive film, and a method for producing the laminated wiring film.
  • a laminated transparent conductive film that can be used as a transparent electrode film such as a display or a touch panel
  • a laminated wiring film comprising the laminated transparent conductive film
  • a method for producing the laminated wiring film is based on Japanese Patent Application No. 2016-058937 filed in Japan on March 23, 2016, and Japanese Patent Application No. 2017-024386 filed in Japan on February 13, 2017. The contents are incorporated herein.
  • a transparent conductive film as shown in, for example, Patent Documents 1-4 is provided as a transparent electrode film.
  • This transparent conductive film is required to have high light transmittance in the visible light region and low electrical resistance.
  • Patent Document 1 an ITO film made of ITO (In 2 O 3 + Sn), which is a kind of transparent conductive oxide, is used as the transparent conductive film.
  • ITO film the electrical resistance is lowered.
  • the transmittance in the visible light region is lowered. Therefore, it has been difficult to achieve both high transmittance and low electrical resistance.
  • Patent Document 2 a metal mesh material such as Cu is used, but in order to reduce the electrical resistance in this metal mesh material, it is necessary to widen the width of the metal portion, and the transmittance is also low. There was a problem of being lowered. In addition, since the metal mesh material may be visually recognized due to light reflection, it is necessary to form a blackened film or the like on the surface of the metal mesh material.
  • Patent Documents 3 and 4 propose a laminated transparent conductive film in which an Ag film and a transparent conductive oxide film are laminated.
  • this laminated transparent conductive film since the conductivity is ensured by the Ag film, it is not necessary to form a thick transparent conductive oxide film in order to reduce the electrical resistance, and a relatively high transmittance can be obtained. It becomes possible.
  • the barrier property against moisture of the transparent conductive oxide film is low, moisture reaches the Ag film in a high humidity environment, Ag aggregation is promoted in the Ag film, and the transmittance and conductivity are reduced. There was a risk of it.
  • a wiring pattern is formed on the laminated transparent conductive film.
  • a wiring pattern is formed by etching, and then the resist film is removed.
  • an electrode pattern is obtained by etching. Since the Ag alloy film has a higher etching rate than that of the ITO film, the overetching of the Ag alloy film becomes large when the same etching solution is used. There was a risk of occurrence.
  • the present invention has been made in view of the above-described circumstances, and has a sufficiently high transmittance, a sufficiently low electrical resistance, excellent environmental resistance and alkali resistance, and forms a wiring pattern by an etching method. It is an object of the present invention to provide a laminated transparent conductive film in which over-etching is unlikely to occur, a laminated wiring film composed of the laminated transparent conductive film, and a method for manufacturing the laminated wiring film.
  • the laminated transparent conductive film of the present invention has an Ag film made of Ag or an Ag alloy, and a transparent conductive oxide film disposed on both sides of the Ag film, and the transparent conductive film
  • the oxide film is formed of an oxide containing Zn, Ga, and Ti.
  • the transparent conductive oxide film made of an oxide containing Zn, Ga and Ti is formed on both surfaces of the Ag film, the Ag film is formed by the transparent conductive oxide film on the lower surface.
  • the wettability of the Ag film is improved, and aggregation of Ag in the Ag film can be suppressed even when the Ag film is thinly formed.
  • the transparent conductive oxide film is excellent in environmental resistance (durability in a high-temperature and high-humidity environment), even when used in a high-humidity environment, the transparent conductive oxide film is formed on the upper surface of the Ag film.
  • the formed transparent conductive oxide film can suppress the intrusion of moisture into the Ag film and suppress the aggregation of Ag. Therefore, it is possible to provide a laminated transparent conductive film having a sufficiently high transmittance and a sufficiently low electric resistance.
  • an acidic mixed solution containing phosphoric acid and acetic acid is used as an etchant, the difference in etching rate between the Ag film and the transparent conductive oxide film is small, and the accuracy can be obtained even when the laminated transparent conductive film is collectively etched.
  • a wiring pattern can be formed well.
  • this transparent conductive oxide film has high alkali resistance, even when the resist film is removed using an alkaline resist removing solution when forming a wiring pattern, the deterioration of the characteristics of the laminated transparent conductive film is suppressed. Can do.
  • the atomic ratio of all metal elements contained in the transparent conductive oxide film is Ga: 0.5 atomic% to 30.0 atomic%, Ti: 0.1 It is preferable that the atomic percent is not less than 10.0 atomic percent and not more than Zn.
  • the Ga content in all the metal elements contained in the transparent conductive oxide film is in the range of 0.5 atomic% to 30 atomic%, the aggregation of the Ag film is suppressed, and the electric resistance Can be suppressed.
  • the Ti content is in the range of 0.1 atomic% or more and 10.0 atomic% or less, it is possible to improve alkali resistance and environmental resistance while suppressing an increase in electrical resistance.
  • the atomic ratio of all metal elements contained in the transparent conductive oxide film is Ga: 0.5 atomic% to 18.0 atomic%, Ti: 0.1 It is more preferable that the atomic percent is 10.0 atomic percent or less and the remaining Zn.
  • the Ga content in all the metal elements contained in the transparent conductive oxide film is in the range of 0.5 atomic% or more and 18.0 atomic% or less, the aggregation of the Ag film is further suppressed. The increase in electrical resistance can be further suppressed.
  • the Ti content is in the range of 0.1 atomic% or more and 10.0 atomic% or less, it is possible to improve alkali resistance and environmental resistance while suppressing an increase in electrical resistance.
  • the atomic ratio of all metal elements contained in the transparent conductive oxide film is Ga: 0.5 atomic% or more and 14.0 atomic% or less, Ti; More preferably, it is 1 atomic% or more and 10.0 atomic% or less and the remaining Zn.
  • the Ga content in all the metal elements contained in the transparent conductive oxide film is in the range of 0.5 atomic% to 14.0 atomic%, the aggregation of the Ag film is further suppressed. Further, the increase in electrical resistance can be further suppressed.
  • the Ti content is in the range of 0.1 atomic% or more and 10.0 atomic% or less, it is possible to improve alkali resistance and environmental resistance while suppressing an increase in electrical resistance.
  • the oxide forming the transparent conductive oxide film may further contain Y.
  • the oxide forming the transparent conductive oxide film contains Y, alkali resistance and environmental resistance can be further improved while suppressing an increase in electrical resistance.
  • the oxide forming the transparent conductive oxide film contains Y
  • the atomic ratio of all metal elements contained in the transparent conductive oxide film is Ga; It is preferable that 0 atomic% or less, Ti; 0.1 atomic% or more and 10.0 atomic% or less, Y: 0.1 atomic% or more and 10.0 atomic% or less, and the remaining Zn.
  • the Ga content in all the metal elements contained in the transparent conductive oxide film is in the range of 0.5 atomic% to 30 atomic%, the aggregation of the Ag film is suppressed, and the electric resistance Can be suppressed.
  • the Ti content is in the range of 0.1 atomic% or more and 10.0 atomic% or less, it is possible to improve alkali resistance and environmental resistance while suppressing an increase in electrical resistance. Furthermore, since the Y content is in the range of 0.1 atomic% to 10.0 atomic%, alkali resistance can be improved while suppressing an increase in electrical resistance.
  • the Ag film includes Cu, Sn, Sb, Ti, Mg, Zn, Ge, In, Al, Ga, Pd, Au, Pt, Bi, Mn, Sc, An Ag alloy containing one or more of Y, Nd, Sm, Eu, Gd, Tb, Er in a total of 0.2 atomic% to 10.0 atomic%, with the balance being Ag and inevitable impurities It is preferable that it is comprised.
  • the thickness of the Ag film is 10 nm or less.
  • the transmittance can be improved.
  • the above-described transparent conductive oxide film is formed on both surfaces of the Ag film, even if the thickness of the Ag film is 10 nm or less, the Ag film does not aggregate and becomes a continuous film. it can.
  • the average transmittance in the visible light region having a wavelength of 400 to 800 nm is 85% or more, and the sheet resistance value is 20 ⁇ / sq.
  • the average transmittance in the visible light region is 85% or more, and the sheet resistance value is 20 ⁇ / sq. Accordingly, the laminated transparent conductive film has a sufficiently high transmittance and a sufficiently low electrical resistance, and can be used as a miniaturized transparent electrode film or transparent wiring film.
  • the laminated wiring film of the present invention is composed of the above-mentioned laminated transparent conductive film and has a wiring pattern. Since the laminated wiring film of the present invention is composed of the above-described laminated transparent conductive film, it has low electrical resistance and high transmittance.
  • the method for producing a laminated wiring film of the present invention is the above-described method for producing a laminated wiring film, wherein the laminated transparent conductive film including the Ag film and the transparent conductive oxide film is formed on a film formation surface of a substrate.
  • the difference in etching rate between the Ag film and the transparent conductive oxide film is small. Even if this laminated transparent conductive film is etched at once, it is possible to suppress the occurrence of overetching of the Ag film, the residue of the transparent conductive oxide film, and the like, and the wiring pattern can be formed with high accuracy. Further, since the alkali resistance of the transparent conductive oxide film is improved by addition of Ti or Ti and Y, even if the resist film is removed using an alkaline resist removing solution in the resist film removing step, the laminated wiring film The deterioration of the characteristics can be suppressed.
  • the manufacturing method of the laminated wiring film of the present invention is a manufacturing method of the above-described laminated wiring film, wherein a resist film forming step of forming a resist film having a reverse pattern of the wiring pattern on the film forming surface of the substrate; A laminated transparent conductive film forming step of forming the laminated transparent conductive film including the Ag film and the transparent conductive oxide film on a film forming surface of the base material on which the resist film is formed; and the resist film And a resist film removing step to be removed.
  • a resist film is formed in a reverse pattern of a wiring pattern on the film forming surface of the base material, and the layered film is formed on the film forming surface of the base material on which the resist film is formed.
  • a transparent conductive film is formed.
  • the alkali resistance of the transparent conductive oxide film is improved by addition of Ti or Ti and Y, even if the resist film is removed using an alkaline resist removing solution in the resist film removing step, the laminated wiring film The deterioration of the characteristics can be suppressed.
  • a laminated transparent conductive film having a sufficiently high transmittance, a sufficiently low electrical resistance, excellent environmental resistance and alkali resistance, and less prone to over-etching, and a laminate comprising this laminated transparent conductive film It is possible to provide a method for manufacturing a wiring film and a laminated wiring film.
  • the laminated transparent conductive film 10 in the present embodiment is used as a transparent electrode film of various displays and touch panels, and is particularly used in a capacitive type touch panel of tablet size or larger.
  • FIG. 1 shows a laminated transparent conductive film 10 according to this embodiment.
  • the laminated transparent conductive film 10 is formed, for example, on a first transparent conductive oxide film 11 formed as a base layer on one surface of a substrate 20 as a base material, and on the first transparent conductive oxide film 11.
  • An Ag film 12 and a second transparent conductive oxide film 13 formed on the Ag film 12 are provided.
  • substrate 20 a glass substrate, a resin film, etc. can be used, for example.
  • the laminated transparent conductive film 10 has an average transmittance of 85% or more and a sheet resistance value of 20 ⁇ / sq. It is as follows.
  • the average transmittance of the laminated transparent conductive film 10 in the visible light region with a wavelength of 400 to 800 nm is preferably 85% or more, and more preferably 86% or more. The higher the average transmittance, the better, so the upper limit is not particularly limited, but is preferably 95% and more preferably 90%.
  • the sheet resistance value of the laminated transparent conductive film 10 is 20 ⁇ / sq. Or less, preferably 5 ⁇ / sq. More preferably, it is as follows. Since the sheet resistance value of the laminated transparent conductive film 10 is preferably as low as possible, the lower limit value is not particularly limited, but 0.5 ⁇ / sq. Is preferable, and 1 ⁇ / sq. Is more preferable.
  • the Ag film 12 is made of Ag or an Ag alloy.
  • Ag or Ag alloy constituting the Ag film 12 may be pure Ag having a purity of 99.9% by mass or more, or Cu, Sn, Sb, Ti, Mg, Zn, Ge, In, Al, Ga, Pd, Au. , Pt, Bi, Mn, Sc, Y, Nd, Sm, Eu, Gd, Tb, and an Ag alloy containing an additive element such as Er may be used.
  • the content of the additive element is desirably limited to 10.0 atomic% or less from the viewpoint of suppressing an increase in the absorptivity (decrease in transmittance) of the Ag film 12 and an increase in electrical resistance. More preferably, it is at most atomic%.
  • the Ag film 12 is made of Cu, Sn, Sb, Ti, Mg, Zn, Ge, In, Al, Ga, Pd, Au, Pt, Bi, Mn, Sc, Y, Nd, Sm, One or two or more of Eu, Gd, Tb and Er are contained in a total of 0.2 atomic% to 10.0 atomic%, and the balance is made of an Ag alloy composed of Ag and inevitable impurities.
  • Nd, Sm, Eu, Gd, Tb, and Er are elements having an effect of improving the wettability of the Ag film 12 with respect to the first transparent conductive oxide film 11, and are cases where the Ag film 12 is formed thin. Also, Ag aggregation can be suppressed.
  • the transmittance of the Ag film 12 may decrease and the resistance value may increase.
  • the lower limit of the total content of one or more of Bi, Mn, Sc, Y, Nd, Sm, Eu, Gd, Tb, Er is 0.3 atomic% or more, 0.5 It is more preferable to set it to atomic% or more.
  • the upper limit of the total content of one or more is preferably 8.0 atomic% or less, and is preferably 5.0 atomic% or less More preferably, it is particularly preferably 2.0 atomic% or less.
  • the first transparent conductive oxide film 11 and the second transparent conductive oxide film 13 are made of an oxide containing Zn, Ga, Ti, or an oxide containing Zn, Ga, Ti, and Y.
  • the first transparent conductive oxide film 11 and the second transparent conductive oxide film 13 are made by adding Ga, Ti, or Ga, Ti, and Y to Zn oxide.
  • the first transparent conductive oxide film 11 and the second transparent conductive oxide film 13 are such that the atomic ratio of Ga, Ti, and Y in all metal elements contained in each transparent conductive oxide film is Ga.
  • the 1st transparent conductive oxide film 11 and the 2nd transparent conductive oxide film 13 do not need to be the same composition, and should just be set to the range of the above-mentioned composition.
  • the Ga content in all the metal elements contained in the first transparent conductive oxide film 11 and the second transparent conductive oxide film 13 is 0.5 atomic% or more.
  • the Ga content in the first transparent conductive oxide film 11 and the second transparent conductive oxide film 13 is 0.5 atomic% or more.
  • Ag aggregation in the Ag film 12 can be suppressed, and an increase in electrical resistance in the laminated transparent conductive film 10 can be suppressed.
  • the Ga content by setting the Ga content to 30.0 atomic% or less, an increase in electrical resistance in the first transparent conductive oxide film 11 and the second transparent conductive oxide film 13 can be suppressed.
  • the increase in the electrical resistance in the 1st transparent conductive oxide film 11 and the 2nd transparent conductive oxide film 13 can be suppressed further by making content of Ga into 18.0 atomic% or less.
  • the lower limit of the Ga content is preferably 1.0 atomic% or more, and more preferably 2.0 atomic% or more.
  • the upper limit of the Ga content should be 25.0 atomic% or less. It is preferably 20.0 atomic% or less, more preferably 18.0 atomic% or less, and even more preferably 14.0 atomic% or less.
  • the first transparent conductive oxide film is formed by setting the content of Ti in all metal elements contained in the first transparent conductive oxide film 11 and the second transparent conductive oxide film 13 to 0.1 atomic% or more.
  • 11 and the second transparent conductive oxide film 13 can be improved in alkali resistance and environmental resistance.
  • the Ti content is 10.0 atomic% or less, an increase in electrical resistance in the first transparent conductive oxide film 11 and the second transparent conductive oxide film 13 can be suppressed.
  • the lower limit of the Ti content is 0.2 atomic% or more. It is preferably 0.5 atomic% or more.
  • the upper limit of the Ti content should be 9.0 atomic% or less. Preferably, it is more preferably 8.0 atomic% or less.
  • the resistance of the transparent conductive oxide film is increased. Alkalinity can be improved.
  • the Y content is 10.0 atomic% or less, an increase in electrical resistance in the first transparent conductive oxide film 11 and the second transparent conductive oxide film 13 can be suppressed.
  • the lower limit of the Y content is preferably 0.2 atomic% or more, More preferably, it is 0.5 atomic% or more.
  • the upper limit of the Y content should be 9.0 atomic% or less. Preferably, it is more preferably 8.0 atomic% or less.
  • the total content of Ga, Ti, and Y shall be 35.0 atomic% or less. It is preferably 30.0 atomic% or less, more preferably 25.0 atomic% or less.
  • the film thickness t2 of the Ag film 12 is set to 10 nm or less in order to improve the transmittance.
  • the thickness t2 of the Ag film 12 is preferably 9 nm or less, and more preferably 8 nm or less.
  • the lower limit of the film thickness t2 of the Ag film 12 is preferably 3 nm or more, and more preferably 4 nm or more.
  • the film thickness t1 of the first transparent conductive oxide film 11 and the film thickness t3 of the second transparent conductive oxide film 13 are obtained by using optical constants (refractive index and extinction coefficient) in each single layer film.
  • An optical simulation is performed with a three-layer structure of 1 transparent conductive oxide film / Ag film (Ag alloy film) / second transparent conductive oxide film, and the film thickness is such that the transmittance in the visible light region is improved by the optical interference effect. .
  • the film thickness t1 (nm) of the first transparent conductive oxide film 11 and the film thickness t3 (nm) of the second transparent conductive oxide film 13 are preferably in the following ranges.
  • n1 and n3 are the refractive index (n1) of the first transparent conductive oxide film 11 and the refractive index (n3) of the second transparent conductive oxide film 13, respectively.
  • K1 and k3 are the coefficient (k1) of the first transparent conductive oxide film 11 and the coefficient (k3) of the second transparent conductive oxide film 13, respectively. That is, in the optical simulation, the film thickness is obtained by optimizing the values of the coefficients k1 and k3 so that the transmittance in the visible light region is improved.
  • the optimum values of the coefficients k1 and k3 differ depending on the transparent conductive oxide, but the coefficients k1 and k3 are preferably in the range of 0.2 to 0.8, and in the range of 0.4 to 0.7. More preferably. In particular, when the coefficients k1 and k3 are about 0.6, the transmittance in the visible light region is improved regardless of the type of the transparent conductive oxide.
  • the film thickness t1 of the first transparent conductive oxide film 11 and the film thickness t3 of the second transparent conductive oxide film 13 are set to 40 nm. These film thicknesses are the film thicknesses when the coefficients k1 and k3 are 0.6.
  • the laminated wiring film 30 according to the present embodiment has a wiring pattern formed on the laminated transparent conductive film 10 shown in FIG. 1.
  • the wiring pattern has a line width and a space width between the lines in the range of 1 ⁇ m to 900 ⁇ m.
  • the laminated wiring film 30 described above is manufactured as follows. First, the laminated transparent conductive film 10 according to the present embodiment is deposited on the deposition surface of the substrate 20 as a base material (laminated transparent conductive film deposition step S11). In the laminated transparent conductive film forming step S ⁇ b> 11, the first transparent conductive oxide film 11 is formed on the substrate 20 as a base layer. The first transparent conductive oxide film 11 is preferably formed by DC sputtering using a sintered target whose film composition can be easily controlled. Next, an Ag film 12 is formed on the formed first transparent conductive oxide film 11 by DC sputtering using an Ag target. This Ag target has a composition corresponding to the composition of the Ag film 12 to be formed.
  • the second transparent conductive oxide film 13 is formed on the formed Ag film 12 by DC sputtering using a transparent conductive oxide target.
  • the transparent conductive oxide target is preferably a sintered target whose film composition can be easily controlled. In this manner, the laminated transparent conductive film 10 according to this embodiment is formed.
  • a resist film 41 is formed on the laminated transparent conductive film 10 formed on the surface of the substrate 20, and the resist film 41 is exposed and developed to form a wiring pattern (resist film forming step S12). ).
  • the laminated transparent conductive film 10 on which the resist film 41 is formed is collectively etched using an acidic mixed solution containing phosphoric acid and acetic acid as an etchant (etching step S13).
  • the content of phosphoric acid is preferably 55% by volume or less, and the content of acetic acid is preferably 30% by volume or less.
  • the mixed solution may contain 20% by volume or less of nitric acid in addition to phosphoric acid and acetic acid.
  • the resist film 41 is removed using an alkaline resist removing solution (resist film removing step S14). Thereby, the laminated transparent conductive film 10 located below the wiring pattern-shaped resist film 41 remains, and the laminated wiring film 30 having the wiring pattern is formed.
  • a first transparent conductive oxide film 11 is formed on the surface of the substrate 20 as an underlayer, and the first transparent conductive oxide film 11 is formed. Since the Ag film 12 is formed thereon, the wettability of the Ag film 12 is improved, and aggregation of Ag is suppressed even when the Ag film 12 is thinly formed. Furthermore, since the first transparent conductive oxide film 11 and the second transparent conductive oxide film 13 are excellent in environmental resistance, even when used in a high humidity environment, Intrusion of moisture can be suppressed, and aggregation of Ag can be suppressed. Therefore, generation of surface plasmon absorption due to Ag aggregation in the Ag film 12 can be prevented, and high transmittance can be obtained. Further, since the Ag film 12 is a continuous film, the electrical resistance can be lowered.
  • the first transparent conductive oxide film 11 and the second transparent conductive oxide film 13 are made by adding Ga, Ti or Ga, Ti and Y to Zn oxide,
  • the atomic ratio of Ga, Ti and Y in all the metal elements contained in the transparent conductive oxide film is Ga: 0.5 atomic% to 30.0 atomic%, Ti; 0.1 atomic% to 10.0 Atomic% or less, Y; 0.1 atomic% or more and 10.0 atomic% or less. Therefore, the addition of Ga can suppress aggregation of Ag and suppress an increase in electrical resistance.
  • alkali resistance and environmental resistance can be improved by addition of Ti.
  • alkali resistance can be improved by addition of Y.
  • the thickness t2 of the Ag film 12 is set to 10 nm or less, the transmittance can be improved.
  • the first transparent conductive oxide film 11 is formed on the surface of the substrate 20 as an underlayer, even if the thickness of the Ag film 12 is 10 nm or less, Ag is not agglomerated and becomes a continuous film, and the electrical resistance is lowered. be able to.
  • the Ag film 12 is made of Cu, Sn, Sb, Ti, Mg, Zn, Ge, In, Al, Ga, Pd, Au, Pt, Bi, Mn, Sc, Y, Nd, Sm, Since one or more of Eu, Gd, Tb, and Er are contained in a total of 0.2 atomic% to 10.0 atomic%, and the balance is composed of an Ag alloy composed of Ag and inevitable impurities. Aggregation of the Ag film 12 is further suppressed, and even if the Ag film 12 is formed to be thinner, it becomes a continuous film and can achieve both high transmittance and low resistance.
  • the average transmittance of the laminated transparent conductive film 10 in the visible light region having a wavelength of 400 to 800 nm is 85% or more, and the sheet resistance value is 20 ⁇ / sq. Since it has a sufficiently high transmittance and low electrical resistance, it can be used as a miniaturized transparent electrode film or transparent wiring film.
  • the laminated wiring film 30 according to the present embodiment has a low electrical resistance and a high transmittance since the wiring pattern is formed on the laminated transparent conductive film 10 according to the present embodiment.
  • the Ag film 12, the first transparent conductive oxide film 11, and the second transparent conductive oxide are used. Since the difference in etching rate with the film 13 is small, even if the laminated transparent conductive film 10 is etched at once, overetching of the Ag film 12, the first transparent conductive oxide film 11, and the second transparent conductive oxide film 13 are performed. It is possible to suppress the generation of residues and the like, and to form a wiring pattern with high accuracy. Further, in this embodiment, the alkali resistance of the first transparent conductive oxide film 11 and the second transparent conductive oxide film 13 is improved by adding Ti or Ti and Y. Therefore, in the resist film removing step S14, the alkaline resistance Even if the resist film is removed using the resist removing solution, the deterioration of the characteristics of the laminated wiring film 30 can be suppressed.
  • the Ag film 12 is made of Cu, Sn, Sb, Ti, Mg, Zn, Ge, In, Al, Ga, Pd, Au, Pt, Bi, Mn, Sc, Y, Nd, Sm, Eu. , Gd, Tb, and Er are included as a total of 0.2 atomic% to 10.0 atomic%, with the balance being composed of an Ag alloy composed of Ag and inevitable impurities.
  • the Ag film 12 is not limited to this, and may be pure Ag or an Ag alloy containing another metal element that is dissolved in Ag.
  • the first transparent conductive oxide film 11 and the second transparent conductive oxide film 13 have been described as having a thickness of about 40 nm.
  • the present invention is not limited to this, and other film thicknesses are possible. It is good.
  • the laminated wiring film 30 is described as being manufactured by an etching method.
  • the present invention is not limited to this, and as shown in FIGS. 5 and 6, the laminated wiring film 30 is formed by a lift-off method. It may be manufactured.
  • a resist film 41 is formed on the film forming surface of the substrate 20, and the resist film 41 is exposed and developed to reverse the wiring pattern. The reversed pattern thus formed is formed (resist film forming step S21).
  • the first transparent conductive oxide film 11, the Ag film 12, and the second transparent conductive oxide film 13 are sequentially formed on the substrate 20 on which the resist film 41 having the reverse pattern is formed by sputtering.
  • the laminated transparent conductive film 10 is formed on the resist film 41 and the substrate 20 (laminated transparent conductive film forming step S22).
  • the resist film 41 is removed using an alkaline resist removing solution (resist film removing step S23).
  • resist film removing step S23 As a result, the laminated transparent conductive film 10 formed on the resist film 41 having the inverted pattern is removed, and a laminated wiring film 30 having a wiring pattern is formed.
  • the wiring pattern can be formed with high accuracy without performing the etching process. Further, since the alkali resistance of the first transparent conductive oxide film 11 and the second transparent conductive oxide film 13 is improved by the addition of Ti or Ti and Y, an alkaline resist removal solution is used in the resist film removal step S23. Even if the resist film is removed by using, the deterioration of the characteristics of the laminated wiring film 30 can be suppressed.
  • a laminated transparent conductive film having a structure shown in Tables 1, 2, 3, and 4 was formed on the surface of a glass substrate (non-alkali glass: 50 mm ⁇ 50 mm ⁇ 1 mmt) by a sputtering method.
  • a glass substrate non-alkali glass: 50 mm ⁇ 50 mm ⁇ 1 mmt
  • an ITO single layer film was formed by sputtering.
  • the glass substrate was heated to 200 ° C. to form a film.
  • the film thickness of the transparent conductive oxide film is the optical simulation described in the embodiment, and the film thickness at which the transmittance in the visible light region is improved by the optical interference effect is selected. All were 40 nm.
  • membrane and the transparent conductive oxide film in the Example of this invention and a comparative example was measured using the film thickness meter (DEKTAK by ULVAC).
  • the compositions of the transparent conductive oxide film and the Ag alloy film were determined by quantitative analysis of elements using an ICP emission spectrometer (ICP emission spectrometer STS-3500DD manufactured by Hitachi High-Tech Science Co., Ltd.).
  • oxide sintered compact targets having the compositions described in Tables 1, 2, 3, and 4 were used.
  • Ag targets having the compositions described in Tables 1, 2, 3, and 4 were used.
  • the film forming conditions for each film are shown below.
  • the composition of the ITO film (oxide obtained by adding Sn to In 2 O 3 ) was In: 35.6 atomic%, Sn: 3.6 atomic%, and O: 60.8 atomic%. It was.
  • the composition of the GZO film (oxide obtained by adding Ga to ZnO) was Zn: 47.3 atomic%, Ga: 2.2 atomic%, and O: 50.5 atomic%.
  • Sputtering device DC magnetron sputtering device (CS-200 manufactured by ULVAC) Magnetic field intensity: 1000 Gauss (directly above the target, vertical component) Ultimate vacuum: 5 ⁇ 10 ⁇ 5 Pa or less
  • Sputtering gas Ar + O 2 mixed gas (O 2 mixing ratio: 1%)
  • Sputtering gas pressure 0.4 Pa
  • Sputtering power DC100W
  • Sputtering device DC magnetron sputtering device (CS-200 manufactured by ULVAC) Magnetic field intensity: 1000 Gauss (directly above the target, vertical component) Ultimate vacuum: 5 ⁇ 10 ⁇ 5 Pa or less Sputtering gas: Ar Sputtering gas pressure: 0.5 Pa Sputtering power: DC100W
  • permeability after film-forming were evaluated.
  • the sheet resistance and transmittance after the constant temperature and humidity test, and the sheet resistance and transmittance after the alkali resistance test were evaluated.
  • the obtained laminated transparent conductive film was subjected to a patterning test by an etching method and a patterning test by a lift-off method. The evaluation method is shown below.
  • Sheet resistance was measured by a four-probe method using a surface resistance measuring instrument (Loresta AP MCP-T400 manufactured by Mitsubishi Yuka Co., Ltd.). The sheet resistance measurement results are shown in Tables 5, 6, 7, and 8, respectively.
  • ⁇ Transmissivity> Using a spectrophotometer (U4100 manufactured by Hitachi High-Technologies Corporation), a transmittance spectrum in a wavelength range of 400 nm to 800 nm was measured, and an average transmittance (transmittance) was obtained. The measurement results of transmittance are shown in Tables 9, 10, 11, and 12, respectively.
  • ⁇ Constant temperature and humidity test> The sample was left in a constant temperature and humidity chamber of 85 ° C. and 85% humidity for 250 hours, and the transmittance and sheet resistance after the test were measured to evaluate the rate of change from before the test.
  • ⁇ Alkali resistance test> The film was immersed in an alkaline resist removing solution (pH 9, TOK-104 manufactured by Tokyo Ohka Kogyo Co., Ltd.) at a temperature of 40 ° C. for 10 minutes, and the transmittance and sheet resistance after immersion were measured to evaluate the rate of change from before immersion.
  • an alkaline resist removing solution pH 9, TOK-104 manufactured by Tokyo Ohka Kogyo Co., Ltd.
  • ⁇ Patterning test by etching method About the above-mentioned laminated transparent conductive film, a resist film was formed on the laminated transparent conductive film in a wiring pattern shape of line width / space width: 30 ⁇ m / 30 ⁇ m by a photolithography method (photolithography method). This was subjected to batch etching using a mixed solution containing phosphoric acid and acetic acid (SEA-5 manufactured by Kanto Chemical Co., Inc.) as an etchant. The etching was performed without heating and with an appropriate etching time (20 seconds to 120 seconds). Further, the phosphoric acid content in the mixed solution was 55% by volume or less, and the acetic acid content was 30% by volume or less.
  • SEA-5 manufactured by Kanto Chemical Co., Inc.
  • FIGS. 7A and 7B a line is denoted by a symbol P, a space by a symbol S, an overetch by a symbol O, and the residue by a symbol R.
  • a cross section of the pattern before removing the resist film (a cross section perpendicular to the line and space and perpendicular to the film formation surface of the substrate 20) is scanned at a magnification of 50000 using a scanning electron microscope (SU8000 manufactured by Hitachi High-Technologies Corporation). Observed at double. The observation result of the cross-sectional shape of Example 3 of the present invention is shown in FIG.
  • the length L was measured with the point farthest from the end of the resist film 41 in the direction parallel to the film formation surface of the substrate 20 among the inner ends of the transparent conductive film 10 as the end of the laminated transparent conductive film 10.
  • Tables 5, 6, 7, and 8 show the lengths of overetching of the samples of the present invention and the comparative example, respectively. Note that the length of overetching in Tables 5, 6, 7, and 8 is the value of the length L obtained by observing one cross section. Moreover, the resist was peeled off and the surface of the laminated film was visually observed.
  • ⁇ Patterning test by lift-off method First, a resist solution is applied to the substrate, a photomask on which a wiring pattern of line width / space width: 30 ⁇ m / 30 ⁇ m is formed, exposed to ultraviolet rays with an exposure machine, and then the portion exposed to the developer is removed. Then, a reversal pattern was formed by photolithography. Next, a laminated transparent conductive film was formed on the substrate on which the reverse pattern was formed using the sputtering apparatus as described above.
  • the formed wiring pattern was subjected to an optical microscope (KEYENCE).
  • the accuracy of the electrode pattern was confirmed by observing at a magnification of 50 times with a laser microscope VK-X200 manufactured by the company.
  • the average transmittance after film formation exceeds 85%, and the sheet resistance after film formation is 20 ⁇ / sq. It was confirmed that a laminated transparent conductive film having excellent transmittance and sufficiently low resistance was obtained.
  • the average transmittance after film formation is 85% or less, and the sheet resistance after film formation is higher than that of the present invention example when compared with samples having the same film thickness of the Ag film. It was. It is presumed that Ag aggregation occurred in the Ag film.
  • the sheet resistance is 10 ⁇ / sq.
  • the sheet resistance is 10 ⁇ / sq.
  • the average transmittance was greatly deteriorated to 76.4%.
  • Comparative Example B by heating the glass substrate to 200 ° C., the film thickness is 180 nm and the sheet resistance is 10 ⁇ / sq. The average transmittance was 85% or less.
  • the overetching length of the laminated film is 1 ⁇ m or less, and the transparent conductive oxide film It was confirmed that a wiring pattern having no residue can be formed with high accuracy.
  • the length of the overetching O of the laminated film is larger than 1 ⁇ m, and the residue R of the transparent conductive oxide film is also generated. Depending on the etching, it is difficult to form a wiring pattern with high accuracy.
  • the laminated transparent conductive film of the present invention has a sufficiently high transmittance, a sufficiently low electrical resistance, excellent environmental resistance and alkali resistance, and is unlikely to cause over-etching. It is suitable for.

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Abstract

Ce film conducteur transparent stratifié comporte : un film d'Ag formé à partir d'Ag ou d'un alliage d'Ag; et des films d'oxyde conducteur transparents disposés sur les deux surfaces du film d'Ag. Les films d'oxyde conducteur transparent sont formés à partir d'un oxyde comprenant Zn, Ga et Ti.
PCT/JP2017/011343 2016-03-23 2017-03-22 Film conducteur transparent stratifié, film de câblage stratifié, et procédé de fabrication d'un film de câblage stratifié WO2017164209A1 (fr)

Priority Applications (4)

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EP17770249.5A EP3435385B1 (fr) 2016-03-23 2017-03-22 Film conducteur transparent stratifié, film de câblage stratifié, et procédé de fabrication d'un film de câblage stratifié
US16/086,165 US20190105872A1 (en) 2016-03-23 2017-03-22 Multilayer transparent conductive film, multilayer wiring film, and method of forming multilayer wiring film
CN201780019852.7A CN108885922B (zh) 2016-03-23 2017-03-22 层叠透明导电膜、层叠布线膜及层叠布线膜的制造方法
KR1020187025939A KR102333536B1 (ko) 2016-03-23 2017-03-22 적층 투명 도전막, 적층 배선막 및 적층 배선막의 제조 방법

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JP2016-058937 2016-03-23
JP2016058937 2016-03-23
JP2017-024386 2017-02-13
JP2017024386A JP6888318B2 (ja) 2016-03-23 2017-02-13 積層透明導電膜、積層配線膜及び積層配線膜の製造方法

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Citations (9)

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Publication number Priority date Publication date Assignee Title
JP2004156070A (ja) * 2002-11-01 2004-06-03 Kanto Chem Co Inc 透明導電膜を含む積層膜のエッチング液組成物
JP2007250430A (ja) * 2006-03-17 2007-09-27 Sumitomo Metal Mining Co Ltd 透明導電膜、およびこれを用いた透明導電性フィルム
JP2009298649A (ja) * 2008-06-13 2009-12-24 Sumitomo Metal Mining Co Ltd 酸化物焼結体、ターゲット、およびそれを用いて得られる透明導電膜、導電性積層体
WO2011122497A1 (fr) * 2010-03-31 2011-10-06 リンテック株式会社 Film conducteur transparent, son procédé de production et dispositif électronique utilisant un film conducteur transparent
WO2011126074A1 (fr) * 2010-04-08 2011-10-13 東ソー株式会社 Film d'oxyde de zinc conducteur transparent, son procédé de fabrication et son utilisation
JP2012054006A (ja) * 2010-08-31 2012-03-15 Gunze Ltd 透明導電性ガスバリヤフィルム及びその製造方法
WO2014097963A1 (fr) * 2012-12-17 2014-06-26 住友化学株式会社 Film conducteur transparent à base d'oxyde de zinc
WO2016024615A1 (fr) * 2014-08-12 2016-02-18 三菱マテリアル株式会社 Film stratifié, film de câblage stratifié, et procédé de fabrication d'un film de câblage stratifié
WO2016111202A1 (fr) * 2015-01-09 2016-07-14 三菱マテリアル株式会社 Film multicouche

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004156070A (ja) * 2002-11-01 2004-06-03 Kanto Chem Co Inc 透明導電膜を含む積層膜のエッチング液組成物
JP2007250430A (ja) * 2006-03-17 2007-09-27 Sumitomo Metal Mining Co Ltd 透明導電膜、およびこれを用いた透明導電性フィルム
JP2009298649A (ja) * 2008-06-13 2009-12-24 Sumitomo Metal Mining Co Ltd 酸化物焼結体、ターゲット、およびそれを用いて得られる透明導電膜、導電性積層体
WO2011122497A1 (fr) * 2010-03-31 2011-10-06 リンテック株式会社 Film conducteur transparent, son procédé de production et dispositif électronique utilisant un film conducteur transparent
WO2011126074A1 (fr) * 2010-04-08 2011-10-13 東ソー株式会社 Film d'oxyde de zinc conducteur transparent, son procédé de fabrication et son utilisation
JP2012054006A (ja) * 2010-08-31 2012-03-15 Gunze Ltd 透明導電性ガスバリヤフィルム及びその製造方法
WO2014097963A1 (fr) * 2012-12-17 2014-06-26 住友化学株式会社 Film conducteur transparent à base d'oxyde de zinc
WO2016024615A1 (fr) * 2014-08-12 2016-02-18 三菱マテリアル株式会社 Film stratifié, film de câblage stratifié, et procédé de fabrication d'un film de câblage stratifié
WO2016111202A1 (fr) * 2015-01-09 2016-07-14 三菱マテリアル株式会社 Film multicouche

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