WO2011078305A1 - 導電膜及びその製造方法、並びにタッチパネル - Google Patents

導電膜及びその製造方法、並びにタッチパネル Download PDF

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WO2011078305A1
WO2011078305A1 PCT/JP2010/073277 JP2010073277W WO2011078305A1 WO 2011078305 A1 WO2011078305 A1 WO 2011078305A1 JP 2010073277 W JP2010073277 W JP 2010073277W WO 2011078305 A1 WO2011078305 A1 WO 2011078305A1
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conductive film
metal nanowire
metal
producing
axis length
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PCT/JP2010/073277
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English (en)
French (fr)
Japanese (ja)
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規 宮城島
直井　憲次
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富士フイルム株式会社
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Priority to CN2010800525705A priority Critical patent/CN102667969A/zh
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/0545—Dispersions or suspensions of nanosized particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/0547—Nanofibres or nanotubes
    • G—PHYSICS
    • G06—COMPUTING; CALCULATING OR COUNTING
    • G06F—ELECTRIC DIGITAL DATA PROCESSING
    • G06F3/00—Input arrangements for transferring data to be processed into a form capable of being handled by the computer; Output arrangements for transferring data from processing unit to output unit, e.g. interface arrangements
    • G06F3/01—Input arrangements or combined input and output arrangements for interaction between user and computer
    • G06F3/03—Arrangements for converting the position or the displacement of a member into a coded form
    • G06F3/041—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means
    • G06F3/045—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means using resistive elements, e.g. a single continuous surface or two parallel surfaces put in contact
    • G—PHYSICS
    • G06—COMPUTING; CALCULATING OR COUNTING
    • G06F—ELECTRIC DIGITAL DATA PROCESSING
    • G06F3/00—Input arrangements for transferring data to be processed into a form capable of being handled by the computer; Output arrangements for transferring data from processing unit to output unit, e.g. interface arrangements
    • G06F3/01—Input arrangements or combined input and output arrangements for interaction between user and computer
    • G06F3/03—Arrangements for converting the position or the displacement of a member into a coded form
    • G06F3/041—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means
    • G06F3/047—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means using sets of wires, e.g. crossed wires
    • 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
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • G—PHYSICS
    • G06—COMPUTING; CALCULATING OR COUNTING
    • G06F—ELECTRIC DIGITAL DATA PROCESSING
    • G06F2203/00—Indexing scheme relating to G06F3/00 - G06F3/048
    • G06F2203/041—Indexing scheme relating to G06F3/041 - G06F3/045
    • G06F2203/04103—Manufacturing, i.e. details related to manufacturing processes specially suited for touch sensitive devices

Definitions

  • the present invention relates to a conductive film having greatly improved transparency and conductivity without causing film peeling, a method for producing the conductive film, and a touch panel.
  • a conductive film is formed by preparing a silver nanowire dispersion liquid, applying the silver nanowire dispersion liquid and drying it, and obtaining conductivity by reducing the interface between fine particles.
  • the amount of metal can be reduced, and a transparent conductive film can be formed.
  • An object of the present invention is to provide a conductive film, a method for producing the conductive film, and a touch panel that have greatly improved transparency and conductivity without causing film peeling.
  • the present invention is based on the above findings by the present inventors, and means for solving the above problems are as follows. That is, ⁇ 1> A metal nanowire-containing film production process for producing a metal nanowire-containing film containing a metal nanowire and a dispersant, An immersion step of immersing the metal nanowire-containing film in an immersion liquid. ⁇ 2> The method for producing a conductive film according to ⁇ 1>, wherein the immersion liquid is a solvent capable of dissolving the dispersant in the metal nanowire-containing film. ⁇ 3> The method for producing a conductive film according to any one of ⁇ 1> to ⁇ 2>, wherein the immersion liquid is at least one selected from ethanol, ethylene glycol, methanol, and water.
  • ⁇ 4> The method for producing a conductive film according to any one of ⁇ 1> to ⁇ 3>, wherein the dispersant is an ionic surfactant.
  • ⁇ 5> The method for producing a conductive film according to ⁇ 4>, wherein the ionic surfactant is a quaternary alkyl ammonium salt.
  • ⁇ 6> The method for producing a conductive film according to any one of ⁇ 1> to ⁇ 5>, wherein the metal nanowire contains silver.
  • All metal nanowires having an average minor axis length of 50 nm or less, an average major axis length of 5 ⁇ m or more, a minor axis length of 50 nm or less, and a major axis length of 5 ⁇ m or more It is a manufacturing method of the electrically conductive film in any one of said ⁇ 1> to ⁇ 6> which contains 50 mass% or more of metal amount in a metal particle.
  • ⁇ 8> The method for producing a conductive film according to any one of ⁇ 1> to ⁇ 7>, wherein the coefficient of variation of the minor axis length of the metal nanowire is 40% or less.
  • ⁇ 9> The method for producing a conductive film according to any one of ⁇ 1> to ⁇ 8>, wherein the cross-sectional shape of the metal nanowire is a shape with rounded corners.
  • the production of a metal nanowire-containing film is performed by applying a metal nanowire dispersion liquid containing a metal nanowire and a dispersant onto a substrate and drying the film. It is a manufacturing method of the electrically conductive film of description.
  • ⁇ 12> A conductive film manufactured by the method for manufacturing a conductive film according to any one of ⁇ 1> to ⁇ 11>.
  • ⁇ 13> A touch panel using the conductive film according to ⁇ 12>.
  • ⁇ 14> A display element using the conductive film according to ⁇ 12>.
  • ⁇ 15> An integrated solar cell using the conductive film according to ⁇ 12>.
  • a conductive film a method for producing the conductive film, and a touch panel, which can solve the above-mentioned conventional problems, and have greatly improved transparency and conductivity without causing film peeling. be able to.
  • FIG. 1 is an explanatory diagram showing a method for determining the sharpness of metal nanowires.
  • FIG. 2 is a schematic cross-sectional view showing an example of a touch panel.
  • FIG. 3 is a schematic explanatory diagram illustrating another example of the touch panel.
  • FIG. 4 is a schematic plan view showing an example of arrangement of conductive films in the touch panel shown in FIG.
  • FIG. 5 is a schematic cross-sectional view showing still another example of the touch panel.
  • the manufacturing method of the electrically conductive film of this invention contains a metal nanowire containing film
  • the electrically conductive film of this invention is manufactured by the manufacturing method of the electrically conductive film of this invention.
  • the details of the conductive film of the present invention will be clarified through the description of the method of manufacturing the conductive film of the present invention.
  • membrane preparation process is a process of producing the metal nanowire containing film
  • the metal nanowire-containing film is produced by applying a metal nanowire dispersion liquid containing at least metal nanowires and a dispersing agent on a substrate and drying it.
  • the said metal nanowire dispersion liquid contains a metal nanowire and a dispersing agent at least, and contains a solvent and also another component as needed.
  • the metal nanowire has an average minor axis length (diameter) of 50 nm or less and an average major axis length (length) of 5 ⁇ m or more.
  • Metal nanowires having such a diameter and length are all The metal particles contain 50% by mass or more of metal.
  • the metal nanowire means metal fine particles having an aspect ratio (length / diameter) of 30 or more.
  • the average minor axis length of the metal nanowire is 50 nm or less, preferably 35 nm or less, and more preferably 20 nm or less. Note that if the average minor axis length is too small, the oxidation resistance deteriorates and the durability may deteriorate. Therefore, the minor axis length is preferably 5 nm or more. On the other hand, if the average minor axis length exceeds 50 nm, sufficient transparency may not be obtained because of scattering due to metal nanowires.
  • the average major axis length of the metal nanowire is 5 ⁇ m or more, preferably 10 ⁇ m or more, and more preferably 30 ⁇ m or more.
  • the length of the major axis of the metal nanowire is too long, it may be entangled during the production of the metal nanowire, or an aggregate may be generated in the production process, so the length of the major axis is 1 mm or less. Is preferred. If the average major axis length is less than 5 ⁇ m, it may be difficult to form a dense network, or sufficient conductivity may not be obtained.
  • the average minor axis length and the average major axis length of the metal nanowire can be determined by observing a TEM image or an optical microscope image using, for example, a transmission electron microscope (TEM) and an optical microscope. In the present invention, the short axis length and the long axis length of the metal nanowires are obtained by observing 300 metal nanowires with a transmission electron microscope (TEM) and calculating the average value thereof.
  • TEM transmission electron microscope
  • metal nanowires having a minor axis length of 50 nm or less and a major axis length of 5 ⁇ m or more are contained in all metal particles in an amount of 50% by mass or more, and 60% by mass or more. Is preferable, and 75 mass% or more is more preferable.
  • appropriate wire-forming ratio When the proportion of metal nanowires having a short axis length of 50 nm or less and a long axis length of 5 ⁇ m or more (hereinafter also referred to as “appropriate wire-forming ratio”) is less than 50% by mass,
  • the conductivity may decrease due to a decrease in the amount of metal that contributes to the resistance, and at the same time, voltage concentration may occur because a dense wire network cannot be formed, or durability may decrease.
  • the appropriate wire formation rate is obtained by filtering the silver nanowire aqueous dispersion to separate the silver nanowire and other particles, and an ICP emission spectrometer By measuring the amount of Ag remaining on the filter paper and the amount of Ag transmitted through the filter paper, respectively, an appropriate wire formation rate can be obtained.
  • the short axis length is 50 nm or less and the long axis length Is a metal nanowire having a thickness of 5 ⁇ m or more.
  • the filter paper has a short axis length of 50 nm or less in a TEM image and the longest axis of particles other than metal nanowires having a long axis length of 5 ⁇ m or more, and is 5 times or more of the longest axis. And it is preferable to use the thing of the diameter below 1/2 of the shortest length of a wire major axis.
  • the coefficient of variation of the short axis length (diameter) of the metal nanowire of the present invention is preferably 40% or less, more preferably 35% or less, and still more preferably 30% or less. If the coefficient of variation exceeds 40%, the voltage may be concentrated on a wire having a short axis length, or the durability may deteriorate.
  • the coefficient of variation of the short axis length of the metal nanowire is, for example, by measuring the short axis length of 300 nanowires from a transmission electron microscope (TEM) image, and calculating the standard deviation and average value thereof. Can be sought.
  • TEM transmission electron microscope
  • the shape of the metal nanowire of the present invention for example, a columnar shape, a rectangular parallelepiped shape, a columnar shape having a polygonal cross section, and the like, a columnar shape or A cross-sectional shape with rounded corners is preferable.
  • the cross-sectional shape of the metal nanowire can be examined by applying a metal nanowire aqueous dispersion on a substrate and observing the cross-section with a transmission electron microscope (TEM).
  • TEM transmission electron microscope
  • the corner of the cross section of the metal nanowire means a peripheral portion of a point that extends each side of the cross section and intersects with a perpendicular drawn from an adjacent side. Further, “each side of the cross section” is a straight line connecting these adjacent corners.
  • the ratio of the “outer peripheral length of the cross section” to the total length of the “each side of the cross section” was defined as the sharpness.
  • the sharpness can be represented by the ratio of the outer peripheral length of the cross section indicated by the solid line and the outer peripheral length of the pentagon indicated by the dotted line.
  • a cross-sectional shape having a sharpness of 75% or less is defined as a cross-sectional shape having rounded corners.
  • the sharpness is preferably 60% or less, and more preferably 50% or less. If the sharpness exceeds 75%, the electrons may be localized at the corners, and plasmon absorption may increase, or the transparency may deteriorate due to yellowing or the like.
  • the lower limit of the sharpness is preferably 30%, more preferably 40%.
  • metal in the said metal nanowire Any metal may be used, 2 or more types of metals may be used in combination other than 1 type of metal, and it can also be used as an alloy. . Among these, those formed from metals or metal compounds are preferable, and those formed from metals are more preferable.
  • the metal is preferably at least one metal selected from the group consisting of the fourth period, the fifth period, and the sixth period of the Long Periodic Table (IUPAC 1991), and at least one selected from Groups 2 to 14 More preferably, at least one metal selected from Group 2, Group 8, Group 9, Group 10, Group 11, Group 12, Group 13, Group 14 is more preferable, It is particularly preferable to include it as a main component.
  • the metal examples include copper, silver, gold, platinum, palladium, nickel, tin, cobalt, rhodium, iridium, iron, ruthenium, osmium, manganese, molybdenum, tungsten, niobium, tantel, titanium, bismuth, antimony, lead, Or these alloys etc. are mentioned.
  • copper, silver, gold, platinum, palladium, nickel, tin, cobalt, rhodium, iridium or alloys thereof are preferable, palladium, copper, silver, gold, platinum, tin and alloys thereof are more preferable, silver Or the alloy containing silver is especially preferable.
  • the content of the metal nanowire in the metal nanowire dispersion liquid is preferably 0.1% by mass to 99% by mass, and more preferably 0.3% by mass to 95% by mass.
  • the content is less than 0.1% by mass, the load in the drying process is great during production, and when it exceeds 99% by mass, particle aggregation may easily occur.
  • ionic surfactants such as a quaternary alkyl ammonium salt
  • Amino group containing compound, thiol group containing compound, sulfide group containing Examples thereof include compounds, amino acids or derivatives thereof, peptide compounds, polysaccharides, natural polymers derived from polysaccharides, synthetic polymers, and polymers such as gels derived therefrom.
  • a quaternary alkyl ammonium salt is particularly preferable because it can be easily washed at the time of immersion.
  • quaternary alkyl ammonium salt examples include hexadecyl trimethyl ammonium bromide (HTAB), hexadecyl trimethyl ammonium chloride, stearyl trimethyl ammonium bromide (STAB), stearyl trimethyl ammonium chloride, tetradecyl trimethyl ammonium bromide, tetradecyl trimethyl ammonium chloride. , Dilauryldimethylammonium bromide, dilauryldimethylammonium chloride and the like. These may be used individually by 1 type and may use 2 or more types together. Among these, hexadecyltrimethylammonium bromide (HTAB) is particularly preferable.
  • HTAB hexadecyltrimethylammonium bromide
  • polymers examples include a protective colloid polymer such as gelatin, polyvinyl alcohol, methyl cellulose, hydroxypropyl cellulose, polyalkyleneamine, partial alkyl ester of polyacrylic acid, polyvinylpyrrolidone (PVP), and polyvinylpyrrolidone copolymer. , Etc.
  • a protective colloid polymer such as gelatin, polyvinyl alcohol, methyl cellulose, hydroxypropyl cellulose, polyalkyleneamine, partial alkyl ester of polyacrylic acid, polyvinylpyrrolidone (PVP), and polyvinylpyrrolidone copolymer. , Etc.
  • PVP polyvinylpyrrolidone
  • Etc polyvinylpyrrolidone copolymer.
  • Etc for the structure that can be used as the dispersant, for example, the description of “Encyclopedia of Pigments” (edited by Seijiro Ito, published by Asshoin Co., Ltd
  • the content of the dispersant in the metal nanowire dispersion liquid can be determined by the following formula 1, and is not particularly limited as long as the metal nanowires can be dispersed, and can be appropriately selected according to the purpose. 20% by mass to 95% by mass is preferable, and 40% by mass to 90% by mass is more preferable.
  • ⁇ Formula 1> Content of dispersing agent in metal nanowire dispersion (mass%) (Metal content in metal nanowire dispersion) / (Metal content in metal nanowire dispersion + content of dispersant) ⁇ 100
  • the method for producing metal nanowires of (2) includes a step of adding and heating a metal complex solution in an aqueous solvent containing at least a halogen compound and a reducing agent, and preferably a desalting treatment step. Other steps are included as necessary.
  • a silver complex is especially preferable.
  • the ligand of the silver complex include CN ⁇ , SCN ⁇ , SO 3 2 ⁇ , thiourea, and ammonia.
  • a silver ammonia complex is particularly preferable.
  • the metal complex is preferably added after the dispersant and the halogen compound. Probably because the wire core can be formed with high probability, there is an effect of increasing the proportion of metal nanowires having an appropriate minor axis length (diameter) and major axis length in the present invention.
  • the solvent is preferably a hydrophilic solvent
  • examples of the hydrophilic solvent include water, alcohols such as methanol, ethanol, propanol, isopropanol, and butanol; ethers such as dioxane and tetrahydrofuran; ketones such as acetone; And cyclic ethers such as dioxane.
  • the heating temperature is preferably 150 ° C. or lower, more preferably 20 ° C. or higher and 130 ° C. or lower, further preferably 30 ° C. or higher and 100 ° C. or lower, and particularly preferably 40 ° C. or higher and 90 ° C. or lower. If necessary, the temperature may be changed during the grain formation process, and changing the temperature during the process may have the effect of controlling nucleation, suppressing renucleation, and improving monodispersity by promoting selective growth. . If the heating temperature exceeds 150 ° C., the transmittance in the evaluation of the coating film may be low because the cross-sectional angle of the nanowire becomes steep.
  • borohydride metal salts such as sodium borohydride and potassium borohydride
  • Lithium aluminum hydride, hydrogen Aluminum hydride salts such as potassium aluminum hydride, cesium aluminum hydride, aluminum beryllium hydride, magnesium aluminum hydride, calcium aluminum hydride
  • alkanolamines such as diethylaminoethanol, ethanolamine, propanolamine, triethanolamine, dimethylaminopropanol
  • propylamine Aliphatic amines such as tilamine, dipropyleneamine, ethylenediamine and triethylenepentamine; heterocyclic
  • the timing of addition of the reducing agent may be before or after the addition of the dispersant, and may be before or after the addition of the halogen compound.
  • a halogen compound is not particularly limited as long as it is a compound containing bromine, chlorine, or iodine, and can be appropriately selected according to the purpose.
  • a halogen compound is not particularly limited as long as it is a compound containing bromine, chlorine, or iodine, and can be appropriately selected according to the purpose.
  • alkali halides such as potassium bromide, potassium chloride, and potassium iodide
  • the timing of adding the halogen compound may be before or after the addition of the dispersant, and may be before or after the addition of the reducing agent.
  • Some halogen compound species may function as a dispersant, but can be preferably used in the same manner.
  • metal halide fine particles may be used, or both a halogen compound and metal halide fine particles may be used.
  • the dispersant and the halogen compound or metal halide fine particles may be used in the same substance.
  • the compound in which the dispersant and the halogen compound are used in combination include, for example, hexadecyltrimethylammonium bromide (HTAB) containing amino group and bromide ion, stearyltrimethylammonium bromide (STAB), hexadecyltrimethylammonium containing amino group and chloride ion.
  • HTAC hexadecyltrimethylammonium bromide
  • the metal nanowire it is preferable to add a dispersant.
  • the shape of the metal nanowire obtained by the kind of dispersing agent to be used can be changed.
  • the step of adding the dispersant may be added before preparing the particles and may be added in the presence of the dispersed polymer, or may be added for controlling the dispersion state after adjusting the particles.
  • the amount needs to be changed according to the required length of the wire. This is considered to be due to the length of the wire by controlling the amount of core metal particles.
  • the dispersant those described above can be used.
  • the desalting treatment can be performed by a method such as ultrafiltration, dialysis, gel filtration, decantation, and centrifugation after forming metal nanowires.
  • a dispersion solvent in the metal nanowire dispersion liquid water is mainly used, and an organic solvent miscible with water can be used in a proportion of 80% by volume or less.
  • an organic solvent for example, an alcohol compound having a boiling point of 50 ° C. to 250 ° C., more preferably 55 ° C. to 200 ° C. is suitably used. By using such an alcohol compound in combination, it is possible to improve the coating in the coating process and reduce the drying load.
  • the alcohol compound is not particularly limited and may be appropriately selected depending on the intended purpose.
  • These may be used individually by 1 type and may use 2 or more types together.
  • the metal nanowire dispersion liquid preferably contains as little inorganic ions as possible, such as alkali metal ions, alkaline earth metal ions, and halide ions.
  • the electrical conductivity of the metal nanowire dispersion is preferably 1 mS / cm or less, more preferably 0.1 mS / cm or less, and even more preferably 0.05 mS / cm or less.
  • the viscosity of the metal nanowire dispersion at 20 ° C. is preferably 0.5 mPa ⁇ s to 100 mPa ⁇ s, and more preferably 1 mPa ⁇ s to 50 mPa ⁇ s.
  • a binder In the metal nanowire dispersion liquid, a binder, various additives, for example, a surfactant, a polymerizable compound, an antioxidant, an anti-sulfurizing agent, a corrosion inhibitor, a viscosity modifier, an antiseptic, etc., if necessary Can be contained.
  • a surfactant for example, a surfactant, a polymerizable compound, an antioxidant, an anti-sulfurizing agent, a corrosion inhibitor, a viscosity modifier, an antiseptic, etc., if necessary Can be contained.
  • the binder is not particularly limited and may be appropriately selected depending on the intended purpose.
  • gelatin, gelatin derivatives, casein, agar, starch, polyvinyl alcohol, polyacrylic acid copolymer, carboxymethyl cellulose, hydroxyethyl cellulose, polyvinyl Examples include pyrrolidone and dextran. These may be used individually by 1 type and may use 2 or more types together.
  • the content of the binder in the metal nanowire dispersion liquid is not particularly limited and may be appropriately selected depending on the intended purpose, but is preferably 0.01 parts by mass to 10 parts by mass with respect to 1 part by mass of silver. 0.1 to 5 parts by mass is more preferable.
  • the corrosion inhibitor is not particularly limited and may be appropriately selected depending on the intended purpose, and azoles are preferred.
  • the azoles include benzotriazole, tolyltriazole, mercaptobenzothiazole, mercaptobenzotriazole, mercaptobenzotetrazole, (2-benzothiazolylthio) acetic acid, 3- (2-benzothiazolylthio) propionic acid, and these And at least one selected from alkali metal salts, ammonium salts, and amine salts.
  • coats the said metal nanowire dispersion liquid there is no restriction
  • a pretreatment such as chemical treatment such as a silane coupling agent, plasma treatment, ion plat
  • the thickness of the metal nanowire-containing film produced as described above is preferably 0.02 ⁇ m to 1 ⁇ m, and more preferably 0.03 ⁇ m to 0.3 ⁇ m.
  • the immersion step is a step of immersing the metal nanowire-containing film in an immersion liquid.
  • the immersion is not particularly limited as long as the entire metal nanowire-containing film can be immersed in the immersion liquid, and can be appropriately selected depending on the purpose.
  • (1) the immersion liquid is placed in a container, And a method of immersing the metal nanowire-containing film in (2), a method of passing the coated material through the immersion liquid, and the like.
  • the immersion liquid is not particularly limited as long as it can dissolve the dispersant in the metal nanowire-containing film, and can be appropriately selected according to the purpose.
  • water, methanol, ethanol, ethylene glycol, acetone Etc for example, water, methanol, ethanol, and ethylene glycol are preferable, and water, ethanol, and ethylene glycol are particularly preferable.
  • the dipping conditions in the dipping step are not particularly limited and can be appropriately selected according to the purpose.
  • the dipping solution is ethanol
  • a range of 5 ° C. to 40 ° C. for 1 second to 30 minutes is preferable. More preferably, it is in the range of 10 ° C. to 30 ° C. for 3 seconds to 3 minutes.
  • the dispersant was removed from the metal nanowire-containing film, for example, when an ionic surfactant is used as the dispersant, after the immersion treatment This can be confirmed by measuring the conductivity of the immersion liquid.
  • the electrically conductive film of this invention is manufactured by the manufacturing method of the electrically conductive film of this invention.
  • the surface resistance of the conductive film of the present invention is preferably 1 ⁇ 10 7 ⁇ / ⁇ or less, more preferably 1 ⁇ 10 3 ⁇ / ⁇ or less.
  • the surface resistance can be measured by, for example, a four-terminal method.
  • the light transmittance of the conductive film of the present invention is preferably 70% or more, and more preferably 80% or more.
  • the transmittance can be measured by, for example, a self-recording spectrophotometer (UV2400-PC, manufactured by Shimadzu Corporation).
  • the conductive film of the present invention can greatly improve transparency and conductivity without causing film peeling, for example, a touch panel, a display electrode, an electromagnetic wave shield, an organic or inorganic EL display electrode, an electronic paper, It is widely applied to flexible display electrodes, integrated solar cells, display elements, and other various devices. Among these, a touch panel, a display element, and an integrated solar cell are particularly preferable.
  • a liquid crystal display element as a display element used in the present invention includes an element substrate provided with the conductive film of the present invention patterned on a substrate as described above, and a color filter substrate as a counter substrate. Are combined by heat treatment, injecting liquid crystal, and sealing the injection port. At this time, the conductive film of the present invention is also preferably used for the conductive film formed on the color filter. Further, after the liquid crystal is spread on the element substrate, the liquid crystal display element may be manufactured by superimposing the substrates and sealing the liquid crystal so as not to leak.
  • Integrated solar cell There is no restriction
  • GaAs gallium arsenide
  • InP indium phosphorus
  • Group III-V compound semiconductor solar cell devices II-VI compound semiconductor solar cell devices such as cadmium telluride (CdTe), copper / indium / selenium system (so-called CIS system), copper / indium / gallium / selenium system ( So-called CIGS-based), copper / indium / gallium / selenium / sulfur-based (so-called CIGS-based) I-III-VI group compound semiconductor solar cell devices, dye-sensitized solar cell devices, organic solar cell devices, etc. Can be mentioned.
  • CdTe cadmium telluride
  • CIS system copper / indium / selenium system
  • So-called CIGS-based copper / indium / gallium / selenium system
  • I-III-VI group compound semiconductor solar cell devices dye-sensitized solar cell devices, organic solar cell devices, etc.
  • the solar cell device is an amorphous silicon solar cell device constituted by a tandem structure type or the like, a copper / indium / selenium system (so-called CIS system), copper / indium / gallium / A selenium-based (so-called CIGS-based), copper / indium / gallium / selenium / sulfur-based (so-called CIGS-based) I-III-VI group compound semiconductor solar cell device is preferable.
  • CIS system copper / indium / selenium system
  • CIGS-based copper / indium / gallium / A selenium-based
  • I-III-VI group compound semiconductor solar cell device is preferable.
  • amorphous silicon solar cell device composed of a tandem structure type, etc.
  • amorphous silicon, a microcrystalline silicon thin film layer, a thin film containing Ge in these, and a tandem structure of these two or more layers is a photoelectric conversion layer Used as For film formation, plasma CVD or the like is used.
  • the transparent conductive layer as the conductive film of the present invention used for the solar cell can be applied to all the solar cell devices.
  • the transparent conductive layer may be included in any part of the solar cell device, but is preferably adjacent to the photoelectric conversion layer.
  • the following structure is preferable regarding the positional relationship with a photoelectric converting layer, it is not limited to this.
  • the structure described below does not describe all the parts that constitute the solar cell device, but describes the range in which the positional relationship of the transparent conductive layer can be understood.
  • A Substrate—Transparent conductive layer (Invention product) —Photoelectric conversion layer
  • B Substrate—Transparent conductive layer (Invention product) —Photoelectric conversion layer—Transparent conductive layer (Invention product)
  • C Substrate-electrode-photoelectric conversion layer-transparent conductive layer (product of the present invention)
  • D Back electrode-photoelectric conversion layer-transparent conductive layer (product of the present invention)
  • the transparent conductive layer used in the solar cell has high infrared wavelength transmittance and low sheet resistance, so that the solar cell has high absorption with respect to the infrared wavelength, for example, amorphous silicon composed of a tandem structure type or the like.
  • Solar cells copper / indium / selenium (so-called CIS), copper / indium / gallium / selenium (so-called CIGS), copper / indium / gallium / selenium / sulfur (so-called CIGSS), etc. It is suitably used for I-III-VI group compound semiconductor solar cells.
  • Touch panel When the conductive film of the present invention is used as a transparent conductor of a touch panel, it is excellent in visibility due to improved transmittance, and a character with at least one of a bare hand, a gloved hand, an indicator, etc. due to improved conductivity, etc.
  • a touch panel having excellent responsiveness to input or screen operation can be manufactured. Examples of the touch panel include widely known touch panels, and the conductive film of the present invention can be applied to what is known as a so-called touch sensor and touch pad.
  • the touch panel is not particularly limited as long as it has the conductive film, and can be appropriately selected according to the purpose.
  • a surface capacitive touch panel for example, a projection capacitive touch panel, a resistive touch panel, etc. Is mentioned.
  • the touch panel 10 includes a transparent conductive film 12 so as to uniformly cover the surface of the transparent substrate 11, and an external detection circuit (not shown) is formed on the transparent conductive film 12 at the end of the transparent substrate 11.
  • the electrode terminal 18 for electrical connection is formed.
  • reference numeral 13 denotes a transparent conductive film serving as a shield electrode
  • reference numerals 14 and 17 denote protective films
  • reference numeral 15 denotes an intermediate protective film
  • reference numeral 16 denotes an antiglare film.
  • the transparent conductive film 12 When an arbitrary point on the transparent conductive film 12 is touched with a finger or the like, the transparent conductive film 12 is grounded through the human body at the touched point, and changes to a resistance value between each electrode terminal 18 and the ground line. Occurs. The change of the resistance value is detected by the external detection circuit, and the coordinates of the touched point are specified.
  • the touch panel 20 includes a transparent conductive film 22 and a transparent conductive film 23 arranged to cover the surface of the transparent substrate 21, and an insulating layer 24 that insulates the transparent conductive film 22 and the transparent conductive film 23.
  • the insulating cover layer 25 that generates a capacitance between the contact object such as a finger and the transparent conductive film 22 or the transparent conductive film 23 detects the position of the contact object such as the finger.
  • the transparent conductive films 22 and 23 may be integrated.
  • the touch panel 20 as a projection capacitive touch panel will be schematically described through an arrangement in which the transparent conductive film 22 and the transparent conductive film 23 are viewed from the plane.
  • the touch panel 20 is provided with a plurality of transparent conductive films 22 capable of detecting positions in the X-axis direction and a plurality of transparent conductive films 23 in the Y-axis direction so as to be connectable to external terminals.
  • the transparent conductive film 22 and the transparent conductive film 23 are in contact with a plurality of contact objects such as fingertips, and contact information can be input at multiple points.
  • contact information can be input at multiple points.
  • the coordinates in the X-axis direction and the Y-axis direction are specified with high positional accuracy.
  • the structure of the said surface type capacitive touch panel can be selected suitably, and can be applied.
  • the example of the pattern of the transparent conductive film by the some transparent conductive film 22 and the some transparent conductive film 23 was shown in the touch panel 20, the shape, arrangement
  • the touch panel 30 can be in contact with the transparent conductive film 32 via the substrate 31 on which the transparent conductive film 32 is disposed, the spacers 36 disposed on the transparent conductive film 32, and the air layer 34.
  • a transparent conductive film 33 and a transparent film 35 disposed on the transparent conductive film 33 are supported and configured.
  • the touch panel 30 is touched from the transparent film 35 side, the transparent film 35 is pressed, the pressed transparent conductive film 32 and the transparent conductive film 33 come into contact with each other, and a potential change at this position is not illustrated.
  • the coordinates of the touched point are specified.
  • TEM transmission electron microscope
  • Each silver nanowire aqueous dispersion is filtered to separate silver nanowires and other particles, and the amount of Ag remaining on the filter paper using an ICP emission spectrometer (ICPS-8000, manufactured by Shimadzu Corporation), The amount of Ag permeated through the filter paper is measured, and the amount of metal in all metal particles of the silver nanowire (appropriate wire) whose minor axis length (diameter) is 50 nm or less and whose major axis length is 5 ⁇ m or more. (Mass%) was determined.
  • the appropriate silver wire separation for obtaining an appropriate wire conversion rate was performed using a membrane filter (Millipore, FALP02500, pore size: 1.0 ⁇ m).
  • the cross-sectional shape of the silver nanowire was obtained by applying a silver nanowire aqueous dispersion on a substrate, observing the cross section with a transmission electron microscope (TEM; JEM-2000FX, JEM-2000FX), and about 300 cross sections. Then, the outer peripheral length of the cross section and the total length of each side of the cross section were measured, and the sharpness, which is the ratio of the “outer peripheral length of the cross section” to the total length of “each side of the cross section”, was obtained. When the sharpness is 75% or less, the cross-sectional shape is rounded.
  • a silver nanowire aqueous dispersion was prepared as follows. 410 mL of pure water was placed in a three-necked flask, and 82.5 mL of additive solution H and 206 mL of additive solution G were added using a funnel while stirring at 20 ° C. (first stage). To this solution, 206 mL of additive solution A was added at a flow rate of 2.0 mL / min and a stirring rotation speed of 800 rpm (second stage). Ten minutes later, 82.5 mL of additive liquid H was added (third stage). Thereafter, the internal temperature was raised to 75 ° C. at 3 ° C./min. Then, the stirring rotation speed was reduced to 200 rpm and heated for 5 hours.
  • an ultrafiltration module SIP1013 manufactured by Asahi Kasei Co., Ltd., molecular weight cut off 6,000
  • a magnet pump a magnet pump
  • a stainless steel cup was connected with a silicone tube to obtain an ultrafiltration device.
  • the silver nanowire dispersion (aqueous solution) was put into a stainless steel cup, and ultrafiltration was performed by operating a pump.
  • the filtrate from the module reached 50 mL
  • 950 mL of distilled water was added to the stainless steel cup for washing.
  • concentration is performed.
  • a silver nanowire aqueous dispersion of 101 was prepared.
  • the obtained sample No. Table 1 shows the average minor axis length (diameter), average major axis length, appropriate wire formation rate, variation coefficient of silver nanowire diameter, and sharpness of the cross-sectional angle of 101 silver nanowires.
  • Preparation Example 2 Sample No. Preparation of 102
  • sample No. 1 was prepared in the same manner as in Preparation Example 1, except that the initial temperature 20 ° C. of the first stage mixed solution was changed to 30 ° C.
  • a silver nanowire aqueous dispersion of 102 was prepared.
  • the obtained sample No. Table 1 shows the average minor axis length (diameter) of 102 silver nanowires, the average major axis length, the appropriate wire formation rate, the variation coefficient of the silver nanowire diameter, and the sharpness of the cross-sectional angle.
  • Preparation Example 3 (Preparation Example 3) -Sample No. Preparation of 103-
  • the same procedure as in Preparation Example 1 was conducted except that the amount of the additive liquid H added in the first stage was changed from 82.5 mL to 65.0 mL.
  • a silver nanowire aqueous dispersion of 103 was prepared.
  • the obtained sample No. Table 1 shows the average minor axis length (diameter) of 103 silver nanowires, the average major axis length, the appropriate wire formation rate, the coefficient of variation of the silver nanowire diameter, and the sharpness of the cross-sectional angle.
  • Preparation Example 4 Sample No. 1 was prepared in the same manner as in Preparation Example 1, except that hexadecyltrimethylammonium bromide (HTAB) added to additive liquid H was replaced with equimolar stearyltrimethylammonium bromide (STAB). 104 aqueous silver nanowire dispersions were prepared.
  • the obtained sample No. Table 1 shows the average minor axis length (diameter), average major axis length, appropriate wire formation rate, variation coefficient of silver nanowire diameter, and sharpness of the cross-sectional angle of 104 silver nanowires.
  • Example 1 Formation of undercoat layer-
  • a commercially available biaxially stretched heat-fixed polyethylene terephthalate (PET) substrate having a thickness of 100 ⁇ m is subjected to a corona discharge treatment of 8 W / m 2 ⁇ min, and a coating liquid for an undercoat layer having the following composition is applied to a dry thickness of 0.8 ⁇ m.
  • a subbing layer was formed.
  • the surface of the undercoat layer was subjected to a corona discharge treatment of 8 W / m 2 ⁇ min, and hydroxyethyl cellulose was coated as a hydrophilic polymer layer so that the dry thickness was 0.2 ⁇ m.
  • sample No. 101 silver nanowire aqueous dispersion was applied onto the hydrophilic polymer layer and dried.
  • the amount of coated silver was measured with a fluorescent X-ray analyzer (SEA1100, manufactured by SII), the amount of coated silver was adjusted to 0.02 g / m 2, and a silver nanowire-containing coated film having a thickness of 0.1 ⁇ m was obtained. Formed.
  • ⁇ Immersion treatment> About the produced silver nanowire containing coating film, the immersion process was performed on the following immersion conditions. -Immersion conditions- Ethanol was used as the dipping solution, dipped at a temperature of 25 ° C., and held for 15 seconds.
  • ⁇ Surface resistance (conductive) of coating film The surface resistance of the obtained metal nanowire-containing film (conductive film) after the immersion treatment was measured using a surface resistance meter (Loresta-GP MCP-T600, manufactured by Mitsubishi Chemical Corporation). evaluated. ⁇ Evaluation criteria ⁇ A: The surface resistance is less than 100 ⁇ / ⁇ , which is a practically acceptable level. ⁇ : The surface resistance is less than 500 ⁇ / ⁇ , which is a level that is not problematic in practice. (Triangle
  • Examples 2 to 11 and Comparative Examples 1 to 8 In Example 1, except that the silver nanowire-containing coating film (sample No. 101 to sample No. 106) shown in Table 2 was changed to the presence or absence of immersion treatment, the immersion liquid, and the presence or absence of centrifugation. Similarly, a silver nanowire-containing coating film after the immersion treatment was prepared, and various characteristics were evaluated in the same manner as in Example 1. The results are shown in Table 2. In addition, the centrifugation in Examples 10 and 11 and Comparative Examples 7 and 8 is sample No. 101 and sample no. After producing 106, before coating, it was performed at 4,500 rpm for 10 minutes.
  • Example 12 -Fabrication of touch panel- Using the conductive film produced in Example 1, "Latest Touch Panel Technology” (issued July 6, 2009, Techno Times Co., Ltd.), supervised by Yuji Mitani, “Touch Panel Technology and Development”, CM Publishing (2004) Published in December), “FPD International 2009 Forum T-11 Lecture Textbook”, “Cypress Semiconductor Corporation Application Note AN2292”, etc., were used to produce a touch panel. When using the manufactured touch panel, it improves visibility by improving transmittance, and responds to input of characters, etc. or screen operations with at least one of bare hands, hands with gloves, or pointing tools by improving conductivity It was found that a touch panel with excellent performance can be produced.
  • the conductive film manufactured by the conductive film manufacturing method of the present invention has greatly improved transparency and conductivity without causing film peeling, for example, a touch panel, a display electrode, an electromagnetic wave shield, an organic or inorganic EL display It is widely used for electrodes, electronic paper, electrodes for flexible displays, integrated solar cells, display elements, and other various devices.

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  • Theoretical Computer Science (AREA)
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JP2013225499A (ja) * 2012-03-23 2013-10-31 Fujifilm Corp 導電性部材、その製造方法、タッチパネル、及び太陽電池
CN103843074A (zh) * 2011-09-29 2014-06-04 富士胶片株式会社 透明导电性涂布膜、透明导电性墨水、及使用其的触控式面板
CN105382265A (zh) * 2015-11-13 2016-03-09 云南常道科技股份有限公司 一种光刻触摸屏银浆用高分散银粉的制备方法
US20210046544A1 (en) * 2018-06-07 2021-02-18 Nuovo Film Suzhou China Inc. Preparation Method of Silver Nanowire with Circular Cross Section

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WO2013141065A1 (ja) * 2012-03-21 2013-09-26 リンテック株式会社 熱電変換材料及びその製造方法
JP2013225296A (ja) * 2012-03-23 2013-10-31 Fujifilm Corp 導電性部材、それを用いたタッチパネル、表示装置、及び入力装置
KR101414560B1 (ko) * 2013-01-09 2014-07-04 한화케미칼 주식회사 전도성 필름의 제조방법
TWI500048B (zh) * 2013-12-30 2015-09-11 Ind Tech Res Inst 透明導電膜組合物及透明導電膜
CN103680766B (zh) * 2013-12-31 2016-08-17 复旦大学 导电薄膜的制备方法
CN104299721B (zh) * 2014-09-05 2018-01-23 中国科学院合肥物质科学研究院 一种通过清洗处理提高金属纳米线透明导电薄膜光学性质的方法
CN108602119B (zh) * 2016-03-14 2020-09-01 尤尼吉可株式会社 纳米线及其制造方法、纳米线分散液以及透明导电膜
CN107342115A (zh) * 2016-05-03 2017-11-10 上海大学 一种透明导电和低发射率微网及其制备方法

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CN103843074A (zh) * 2011-09-29 2014-06-04 富士胶片株式会社 透明导电性涂布膜、透明导电性墨水、及使用其的触控式面板
JP2013201007A (ja) * 2012-03-23 2013-10-03 Fujifilm Corp 導電性部材及びその製造方法、並びにタッチパネル
JP2013225499A (ja) * 2012-03-23 2013-10-31 Fujifilm Corp 導電性部材、その製造方法、タッチパネル、及び太陽電池
WO2013146509A1 (ja) * 2012-03-26 2013-10-03 富士フイルム株式会社 金属ナノワイヤ分散液の製造方法、金属ナノワイヤ分散液、金属ナノワイヤ分散液を用いて形成された導電性部材、及びその導電性部材を用いたタッチパネル、及び太陽電池
CN105382265A (zh) * 2015-11-13 2016-03-09 云南常道科技股份有限公司 一种光刻触摸屏银浆用高分散银粉的制备方法
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