WO2013141278A1 - 導電性組成物、導電性部材、導電性部材の製造方法、タッチパネルおよび太陽電池 - Google Patents
導電性組成物、導電性部材、導電性部材の製造方法、タッチパネルおよび太陽電池 Download PDFInfo
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24802—Discontinuous or differential coating, impregnation or bond [e.g., artwork, printing, retouched photograph, etc.]
- Y10T428/24893—Discontinuous or differential coating, impregnation or bond [e.g., artwork, printing, retouched photograph, etc.] including particulate material
- Y10T428/24909—Free metal or mineral containing
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
Definitions
- the present invention relates to a conductive composition, a conductive member, a method for manufacturing a conductive member, a touch panel, and a solar cell.
- a touch panel is mounted on a display device such as a liquid crystal panel or electronic paper as an input device.
- a display device such as a liquid crystal panel or electronic paper
- Various touch panel configurations such as a resistive film method, a surface acoustic wave method, and a capacitance method are known, but a capacitance method is available as a method that allows multipoint touch and facilitates large area.
- a capacitive touch panel using ITO (indium tin oxide) as a transparent conductive material is disclosed.
- indium which is a raw material of ITO
- ITO indium
- a manufacturing process is high because a vacuum process is required for thin film production, and an ITO film is brittle and inferior in bending resistance.
- alternative materials such as metal nanowires, carbon nanotubes, PEDOT, and polyaniline have been proposed.
- a conductive member having a conductive layer including conductive fibers such as metal nanowires, carbon nanotubes, and composites of carbon nanotubes and metals has been proposed (see, for example, Patent Document 1).
- This conductive member is provided with a conductive layer containing a plurality of metal nanowires on a base material, and by exposing the photocurable composition as a matrix to the conductive layer, pattern exposure and Subsequent development can be easily processed into a conductive member having a conductive layer including a desired conductive region and a non-conductive region.
- a non-photocurable composition as a matrix is contained in the conductive layer, and drying and / or crosslinking by condensation reaction or polymerization reaction is performed as necessary.
- a method of performing an etching process after forming a resist layer imagewise on the conductive layer with an etching resist or the like, or in the uniformly formed transparent conductive layer The conductive network can be easily processed into a conductive member having a conductive layer including a desired conductive region and a non-conductive region by a method of partially disconnecting the conductive network by laser light irradiation (for example, a patent) Reference 2 and 3).
- a conductive layer including the conductive fiber is formed on the temporary support and transferred to a glass substrate or the like.
- a conductive layer transfer type conductive member that performs patterning by a method has also been proposed (see, for example, Patent Documents 4 and 5).
- the conductive fibers preferably used for the conductive member as described above include various materials such as metal nanowires and nanorods such as silver, gold, and copper, carbon nanotubes, carbon nanorods, and composites of carbon nanotubes and metals. It has been known. Among them, it is known that metal conductive fibers made of metals such as silver, gold, and copper more preferably give excellent conductive members with low resistance and high light transparency. Silver nanowires that are excellent in terms of price balance are particularly preferably used. However, the conductive members using these metal conductive fibers are presumed to be caused by metal oxidation or form change when exposed to harsh conditions such as high temperature, high humidity or ozone. In some cases, an increase in resistivity may occur, and depending on the application, improvement in weather resistance may be required.
- a method for improving the weather resistance of a transparent conductive material containing a metal conductive fiber a method using a metal adsorbing compound having a specific structure is disclosed (for example, see Patent Documents 6 and 7).
- this method is effective depending on specific storage conditions, the metal conductive fiber aggregates during the production of the transparent conductive material because the metal adsorbent compound exhibits strong adsorptivity to the metal conductive fiber.
- the homogeneity of the conductive layer is lowered, the conductivity and transparency of the conductive layer are reduced, or the contact resistance between the metal conductive fibers is increased, so that the conductivity of the conductive layer is increased. There were cases where problems such as lowering occurred.
- a method for producing an aqueous dispersion containing metal nanowires a method of adding a metal complex solution or a metal ion solution in an aqueous solvent containing a halogen compound and a reducing agent is disclosed (for example, see Patent Document 8).
- desalting treatment is preferably carried out for the purpose of improving the purity of the metal nanowires, and when the desalting (cleaning) treatment disclosed in the examples is performed, the metal nanowires are formed. It is estimated that most of the reducing agent that did not contribute has been removed. In this patent document, there is no description about intentionally leaving the reducing agent added when the metal complex is reduced and its effect.
- the problem to be solved by the present invention is a conductive composition containing metal conductive fibers that can maintain its conductivity over time even when exposed to severe conditions such as high temperature conditions, high humidity conditions, or the presence of ozone. It is providing the touch panel and solar cell using a thing, an electroconductive member, the manufacturing method of an electroconductive member, and the said electroconductive member.
- the manufacturing method of the electroconductive composition of this invention which solves the said subject, an electroconductive member, a touch panel, a solar cell, and an electroconductive member is as follows.
- the conductive composition of the present invention comprises at least (a) a metal conductive fiber having an average minor axis length of 1 nm to 150 nm, and (b) a compound represented by the following general formula (1) and the following general formula (2 At least one compound selected from the compounds represented by:
- R 1 and R 2 each independently represents an alkyl group, an aryl group, an alkoxy group, an aryloxy group or a halogen atom
- R 3 represents an alkyl group or an aryl group. At least two of R 1 , R 2 and R 3 may be linked to each other via a divalent or higher-valent organic group or a single bond.
- one hydrogen atom is removed from at least one of R 1 , R 2 and R 3 to form a monovalent group, and the monovalent group is divalent or higher.
- R 4 and R 5 each independently represents an alkyl group. R 4 and R 5 may be connected to each other via a divalent or higher-valent organic group or a single bond.
- the compound represented by the general formula (2) is a monovalent group by removing one hydrogen atom from at least one of R 4 and R 5 , and this monovalent group is a divalent or higher organic group or It includes a compound in which a plurality of structures represented by the general formula (2) connected to at least one of R 4 and R 5 through a single bond exist in one molecule.
- it further includes (c) a polymerizable compound capable of forming a matrix.
- the polymerizable compound capable of forming a matrix is a non-photosensitive compound.
- the polymerizable compound capable of forming a matrix is a compound capable of forming a sol-gel cured product.
- the content ratio ((c) / (a)) of (a) the polymerizable compound capable of forming a matrix with respect to the metal conductive fiber ((c) / (a)) is 0.001 / 1 to 100/1. is there.
- At least one compound selected from the compound represented by the general formula (1) and the compound represented by the general formula (2) is 0.005 mmol per 1 g of the metal conductive fiber (a). More than 30 mmol is contained.
- At least one of R 1 and R 2 in the general formula (1) is an alkoxy group or an aryloxy group, and R 3 is an aryl group.
- it further contains at least one compound represented by the following general formulas (3) to (11).
- V 3 represents a hydrogen atom or a substituent.
- V 4 represents a hydrogen atom or a substituent.
- V 5 represents a hydrogen atom or a substituent, and R 51 and R 52 each independently represent a hydrogen atom or a group that can be substituted with a nitrogen atom.
- V 6 represents a hydrogen atom or a substituent, and R 61 and R 62 each independently represent a hydrogen atom or a group that can be substituted with a nitrogen atom.
- V 7 represents a hydrogen atom or a substituent, and R 71 and R 72 each independently represent a hydrogen atom or a substituent.
- V 8 represents a hydrogen atom or a substituent
- R 81 and R 82 each independently represent a hydrogen atom or a substituent
- V 9 represents a hydrogen atom or a substituent
- R 91 , R 92 , R 93 and R 94 each independently represent a hydrogen atom or a group that can be substituted with a nitrogen atom.
- V 10 represents a hydrogen atom or a substituent
- R 101 , R 102 , R 103, and R 104 each independently represent a hydrogen atom or a group that can be substituted with a nitrogen atom.
- R 111 represents a hydrogen atom or a group capable of substituting for a nitrogen atom
- V 111 , V 112 , V 113 and V 114 each independently represents a hydrogen atom or a substituent
- 111 and V 112 , and V 113 and V 114 may be connected to each other to form a bicyclo ring or a tricyclo ring.
- the metal conductive fiber contains 50 mol% or more and 100 mol% or less of silver.
- the average short axis length of the metal conductive fiber is 1 nm or more and 30 nm or less.
- the conductive member of the present invention has a base material and a conductive layer formed from the conductive composition of the present invention provided on the base material.
- it further has a soluble protective layer containing at least a water-soluble polymer on the conductive layer.
- the surface resistance of the conductive layer is 1 ⁇ / ⁇ or more and 1000 ⁇ / ⁇ or less.
- the conductive layer includes a conductive region and a non-conductive region.
- At least one intermediate layer is further provided between the substrate and the conductive layer.
- the touch panel of the present invention is a touch panel including the conductive member of the present invention.
- the solar cell of the present invention is a solar cell including the conductive member of the present invention.
- the method for producing a conductive member of the present invention is represented by at least (a) a metal conductive fiber having an average minor axis length of 1 nm to 150 nm and (b) the following general formula (1) on a substrate. It includes a conductive layer forming step of forming a conductive layer using the conductive composition of the present invention containing a compound and at least one compound selected from the compounds represented by the following general formula (2).
- R 1 and R 2 each independently represents an alkyl group, an aryl group, an alkoxy group, an aryloxy group or a halogen atom
- R 3 represents an alkyl group or an aryl group. At least two of R 1 , R 2 and R 3 may be linked to each other via a divalent or higher-valent organic group or a single bond.
- one hydrogen atom is removed from at least one of R 1 , R 2 and R 3 to form a monovalent group, and the monovalent group is divalent or higher.
- R 4 and R 5 each independently represents an alkyl group. R 4 and R 5 may be connected to each other via a divalent or higher-valent organic group or a single bond.
- the compound represented by the general formula (2) is a monovalent group by removing one hydrogen atom from at least one of R 4 and R 5 , and this monovalent group is a divalent or higher organic group or It includes a compound in which a plurality of structures represented by the general formula (2) connected to at least one of R 4 and R 5 through a single bond exist in one molecule.
- the step of forming the conductive layer includes (a) a metal conductive fiber having an average minor axis length of 1 nm to 150 nm and (b) a compound represented by the general formula (1)
- a conductive composition containing at least one compound selected from the compounds represented by formula (2) (c) a matrix is added, and (a) component, (b) component, and (c ) A conductive layer containing the component is formed.
- the step of forming the conductive layer comprises: (a) a metal conductive fiber having an average minor axis length of 1 nm or more and 150 nm or less, (b) a compound represented by the general formula (1); At least one compound selected from the compounds represented by formula (2) and (c) a conductive composition containing a matrix are provided, and includes (a) component, (b) component, and (c) component A conductive layer is formed.
- a metal conductive fiber having an average minor axis length of 1 nm or more and 150 nm or less is provided on the substrate, and then (b) a compound represented by the following general formula (1) and the following general formula (A conductive layer containing (a) component, (b) component and (c) component by applying a composition containing at least one compound selected from the compounds represented by 2) and (c) matrix Form.
- R 1 and R 2 each independently represents an alkyl group, an aryl group, an alkoxy group, an aryloxy group or a halogen atom
- R 3 represents an alkyl group or an aryl group. At least two of R 1 , R 2 and R 3 may be linked to each other via a divalent or higher-valent organic group or a single bond.
- one hydrogen atom is removed from at least one of R 1 , R 2 and R 3 to form a monovalent group, and the monovalent group is divalent or higher.
- R 4 and R 5 each independently represents an alkyl group. R 4 and R 5 may be connected to each other via a divalent or higher-valent organic group or a single bond.
- the compound represented by the general formula (2) is a monovalent group by removing one hydrogen atom from at least one of R 4 and R 5 , and this monovalent group is a divalent or higher organic group or It includes a compound in which a plurality of structures represented by the general formula (2) connected to at least one of R 4 and R 5 through a single bond exist in one molecule.
- the step of providing a photoresist layer on the conductive member of the present invention having a substrate and a conductive layer, and exposing and developing the photoresist layer in a pattern form to form a patterned photoresist layer.
- a patterned conductive layer having at least a step and a step of etching the conductive layer through a patterned photoresist layer.
- a conductive composition containing metal conductive fibers which can maintain conductivity over time even when exposed to severe conditions such as high temperature conditions, high humidity conditions, or the presence of ozone,
- a member, a method for producing a conductive member, and a touch panel and a solar cell using the conductive member are provided.
- a numerical range expressed using “to” means a range including numerical values described before and after “to” as a lower limit value and an upper limit value.
- the term “light” is used as a concept including not only visible light but also high energy rays such as ultraviolet rays, X-rays, and gamma rays, particle rays such as electron beams, and the like.
- (meth) acrylic acid is used to indicate either or both of acrylic acid and methacrylic acid
- (meth) acrylate” is used to indicate either or both of acrylate and methacrylate.
- the content is expressed in terms of mass, and unless otherwise specified, mass% represents a ratio to the total amount of the composition, and “solid content” is a component excluding the solvent in the composition. Represents.
- the conductive composition of the present invention has at least (a) a metal conductive fiber (hereinafter referred to as “average short axis length” or “average diameter”) having an average minor axis length (hereinafter also referred to as “average minor axis length” or “average diameter”) of 1 nm to 150 nm. And (b) at least one compound selected from a compound represented by the following general formula (1) and a compound represented by the following general formula (2) (Hereinafter sometimes referred to as “(b) component compound”).
- R 1 and R 2 each independently represents an alkyl group, an aryl group, an alkoxy group, an aryloxy group or a halogen atom
- R 3 represents an alkyl group or an aryl group. At least two of R 1 , R 2 and R 3 may be linked to each other via a divalent or higher-valent organic group or a single bond.
- one hydrogen atom is removed from at least one of R 1 , R 2 and R 3 to form a monovalent group, and the monovalent group is divalent or higher. It includes a compound in which a plurality of structures represented by the general formula (1) connected to at least one of R 1 , R 2 and R 3 through an organic group or a single bond exist in one molecule.
- R 4 and R 5 each independently represents an alkyl group. R 4 and R 5 may be connected to each other via a divalent or higher-valent organic group or a single bond.
- the compound represented by the general formula (2) is a monovalent group by removing one hydrogen atom from at least one of R 4 and R 5 , and this monovalent group is a divalent or higher organic group or It includes a compound in which a plurality of structures represented by the general formula (2) connected to at least one of R 4 and R 5 through a single bond exist in one molecule.
- composition of the conductive composition of the present invention can suppress a decrease in conductivity even when exposed to severe conditions such as high temperature conditions, high humidity conditions, or the presence of ozone. The reason is not clear, but can be considered as follows.
- radical species are generated in the conductive layer containing metal conductive fibers or in the vicinity of the conductive layer.
- This radical species reacts with oxygen to generate peroxide and the like.
- at least one compound (component compound (b)) selected from the compound represented by the general formula (1) and the compound represented by the general formula (2) is the generated peroxide or the like. It is considered to have a function to deactivate. Therefore, in order to allow the component compound (b) to be present in the vicinity of the metal conductive fiber, by containing it in the conductive layer or a layer in contact with the conductive layer, the peroxide is reduced, and the metal conductive fiber is oxidized. It is presumed that the decrease in conductivity is suppressed as a result.
- the components of the conductive composition of the present invention will be described in detail.
- the conductive composition of the present invention contains a metal conductive fiber having an average minor axis length of 1 nm to 150 nm.
- the average minor axis length of the metal conductive fiber is 1 nm to 150 nm, preferably 1 nm to 70 nm, more preferably 1 nm to 50 nm, further preferably 1 nm to 40 nm, and more preferably 10 nm to 40 nm from the viewpoint of durability and optical properties. Particularly preferred.
- the average minor axis length (average diameter) of the metal conductive fiber, and the average major axis length (average major axis length) can be measured using a transmission electron microscope (TEM) and an optical microscope, for example, It can be determined by observing an optical microscope image.
- TEM transmission electron microscope
- the average minor axis length (average diameter) and average major axis length of the metal conductive fibers are 300 using a transmission electron microscope (TEM; JEM-2000FX, manufactured by JEOL Ltd.). The metal conductive fibers are observed, and the average value is defined as the average minor axis length and the average major axis length.
- the average short axis length when the short axis direction cross section of the metal conductive fiber is not circular is the length of the longest portion measured in the short axis direction as the average short axis length. Also. When the metal conductive fiber is bent, a circle having the arc as an arc is taken into consideration, and a value calculated from the radius and the curvature is defined as the average major axis length.
- the aspect ratio of the metal conductive fiber is preferably 50 or more.
- the aspect ratio generally means the ratio between the long side and the short side of the fibrous material (ratio of average major axis length / average minor axis length).
- ratio of average major axis length / average minor axis length There is no restriction
- the aspect ratio of the entire metal conductive fiber can be estimated by separately measuring the average major axis length and the average minor axis length of the metal conductive fiber.
- the said metal conductive fiber is a tube shape, the outer diameter of this tube is used as a diameter for calculating the said aspect ratio.
- the aspect ratio of the metal conductive fiber can be appropriately selected according to the purpose, but is preferably 50 to 1,000,000, and more preferably 100 to 1,000,000.
- the aspect ratio can be set to 50 or more, it becomes easy to form a network with the metal conductive fibers, and it becomes easy to ensure sufficient conductivity.
- the aspect ratio to 1,000,000 or less, a liquid that is stable and excellent in manufacturing suitability can be easily obtained without entanglement of the metal conductive fiber during the formation of the metal conductive fiber or in subsequent handling. can get.
- the metal conductive material that forms the fiber examples include metal oxides such as ITO, zinc oxide, and tin oxide, metallic carbon, a single metal element, a composite structure composed of a plurality of metal elements, and an alloy composed of a plurality of metals. Etc. Moreover, after making into fiber form, you may surface-treat, for example, the metal fiber etc. which were plated (plated) can be used.
- the metal conductive fiber may take any form of a solid structure, a porous structure, and a hollow structure, but preferably has a solid structure or a hollow structure.
- solid structure fibers may be referred to as “wires” and hollow structure fibers may be referred to as “tubes”.
- metal nanowires From the viewpoint of easily forming a transparent conductive film, it is preferable to use metal nanowires as the metal conductive fibers.
- the metal nanowires in the present invention preferably have an average minor axis length of 1 nm to 150 nm and an average major axis length of 1 ⁇ m to 100 ⁇ m.
- the average minor axis length (average diameter) of the metal nanowire is preferably 1 nm to 50 nm, more preferably 1 nm to 30 nm, still more preferably 5 nm to 30 nm, and more preferably 5 nm to 25 nm. It is particularly preferred.
- the average minor axis length is 1 nm or more, the oxidation resistance is excellent and the durability tends to be improved.
- the average minor axis length is 150 nm or less, deterioration of optical characteristics such as an increase in haze due to light scattering or the like can be suppressed.
- the average major axis length (sometimes referred to as “average length”) of the metal nanowire is preferably 1 ⁇ m to 40 ⁇ m, more preferably 3 ⁇ m to 35 ⁇ m, and particularly preferably 5 ⁇ m to 30 ⁇ m.
- the average major axis length of the metal nanowire is 40 ⁇ m or less, the formation of aggregates during the production of the metal nanowire is suppressed, and when the average major axis length is 1 ⁇ m or more, sufficient conductivity tends to be obtained. .
- the variation coefficient of the average minor axis length (diameter) of the metal nanowire used in the conductive layer according to the present invention is preferably 40% or less, more preferably 35% or less, and particularly preferably 30% or less. By setting the coefficient of variation to 40% or less, it becomes easy to ensure conductivity with excellent durability.
- the coefficient of variation of the average minor axis length (diameter) of the metal nanowire is, for example, the average minor axis length (diameter) of 300 metal nanowires measured from a transmission electron microscope (TEM) image, and the standard deviation and It can be obtained by calculating an average value.
- the shape of the metal nanowire can be any shape such as a columnar shape, a rectangular parallelepiped shape, or a columnar shape with a polygonal cross section.
- the columnar shape or the cross section is 5
- a polygon that is a polygon larger than a square and has a cross-sectional shape that does not have an acute angle is preferable.
- the cross-sectional shape of the metal nanowire can be detected by applying a metal nanowire aqueous dispersion on the substrate and observing the cross-section with a transmission electron microscope (TEM).
- TEM transmission electron microscope
- 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.
- 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 kind selected from Groups 2 to 14 Metal is more preferable, and at least one metal selected from Group 2, Group 8, Group 9, Group 10, Group 11, Group 12, Group 13, and Group 14 is more preferable. It is particularly preferable to include it as a component.
- the metal include copper, silver, gold, platinum, palladium, nickel, tin, cobalt, rhodium, iridium, iron, ruthenium, osmium, manganese, molybdenum, tungsten, niobium, tantalum, titanium, bismuth, and antimony. , Lead, or an alloy thereof.
- 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, particularly Silver or a silver-containing alloy containing 50 mol% or more and 100 mol% or less of silver (more preferably 90 mol% or more and 100 mol% or less of silver) is preferable.
- the solvent used for the production of the metal nanowire is preferably a hydrophilic solvent, and examples thereof include water, alcohols, ethers, and ketones. These may be used alone or in combination of two or more. May be used in combination.
- alcohols include methanol, ethanol, propanol, 2-propanol, butanol, ethylene glycol, and the like.
- ethers include dioxane and tetrahydrofuran.
- ketones include acetone.
- the temperature is preferably 250 ° C or lower, more preferably 20 ° C or higher and 200 ° C or lower, further preferably 30 ° C or higher and 180 ° C or lower, and particularly preferably 40 ° C or higher and 170 ° C or lower.
- the temperature is preferably 250 ° C or lower, more preferably 20 ° C or higher and 200 ° C or lower, further preferably 30 ° C or higher and 180 ° C or lower, and particularly preferably 40 ° C or higher and 170 ° C or lower.
- the temperature is preferably 250 ° C or lower, more preferably 20 ° C or higher and 200 ° C or lower, further preferably 30 ° C or higher and 180 ° C or lower, and particularly preferably 40 ° C or higher and 170 ° C or lower.
- the heating is preferably performed by adding a reducing agent.
- a reducing agent There is no restriction
- reducing sugars, sugar alcohols as derivatives thereof, and ethylene glycol are more preferable, and reducing sugars, sugar alcohols as derivatives thereof, and ethylene glycol are particularly preferable.
- the reducing agent there is a compound that functions as a dispersant or a solvent as a function, and can be preferably used in the same manner.
- the reducing agent used to form the metal nanowires is less than 0.1% by mass with respect to silver, after forming the metal nanowires, by ultrafiltration, dialysis, gel filtration, decantation, centrifugation, etc. It is preferable to remove.
- the metal nanowire it is preferable to add a dispersant and a halogen compound or metal halide fine particles.
- the timing of addition of the dispersant and the halogen compound may be before or after the addition of the reducing agent, and may be before or after the addition of the metal ions or metal halide fine particles, but a metal nanowire having better monodispersibility is obtained. Therefore, it is preferable to add the halogen compound in two or more stages.
- the dispersant may be added to the reaction solution before preparing the particles or after preparing the particles.
- the dispersant may be added in one step or divided into two or more steps.
- the dispersant include an amino group-containing compound, a mercapto group-containing compound, a sulfide-containing compound, an amino acid or a derivative thereof, a peptide compound, a polysaccharide, a natural polymer derived from a polysaccharide, a synthetic polymer, or a gel derived therefrom. And the like.
- polymer compound suitably used as the dispersant examples include gelatin, polyvinyl alcohol, methylcellulose, hydroxypropylcellulose, polyalkyleneamine, poly (meth) acrylic acid, a salt thereof, and a part thereof, which are protective colloidal polymers.
- Preferred examples include hydrophilic polymers such as alkyl esters, polyvinylpyrrolidone, copolymers containing a polyvinylpyrrolidone structure, and poly (meth) acrylic acid derivatives having an amino group or a mercapto group.
- the polymer used as the dispersant has a weight average molecular weight (Mw) measured by a gel permeation chromatography method of preferably 3000 or more and 300,000 or less, and more preferably 5000 or more and 100,000 or less.
- Mw weight average molecular weight measured by a gel permeation chromatography method
- the description of “Encyclopedia of Pigments” edited by Seijiro Ito, published by Asakura Shoin Co., Ltd., 2000
- the shape of the metal nanowire obtained can be controlled depending on the type of the dispersant used.
- halogen compound a compound containing bromide ion, chloride ion or iodide ion is preferable.
- metal halides such as sodium bromide, sodium chloride, sodium iodide, potassium iodide, potassium bromide, potassium chloride, potassium iodide, and onium salt halide ion salts that also function as dispersants listed below. Is preferred.
- silver halide fine particles may be used, and both a halogen compound and silver halide fine particles may be used.
- a single substance having both functions may be used as the dispersant and the halogen compound. That is, the function of both a dispersing agent and a halogen compound is expressed with one compound.
- Preferred examples of the halogen compound having a function as a dispersant include halide ion salts of onium (preferably ammonium or phosphonium).
- hexadecyltrimethylammonium bromide HTAB
- hexadecyltrimethylammonium chloride HTAC
- dodecyltrimethylammonium bromide dodecyltrimethylammonium chloride
- stearyltrimethylammonium bromide stearyltrimethylammonium chloride
- decyltrimethylammonium bromide decyltrimethylammonium chloride
- Examples include dimethyl distearyl ammonium bromide, dimethyl distearyl ammonium chloride, dilauryl dimethyl ammonium bromide, dilauryl dimethyl ammonium chloride, dimethyl dipalmityl ammonium bromide, dimethyl dipalmityl ammonium chloride, and the like.
- the metal nanowire preferably contains as little inorganic ions as possible, such as alkali metal ions, alkaline earth metal ions, and halide ions.
- the electrical conductivity when the metal nanowire is dispersed in an aqueous solution 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 at 20 ° C. when the metal nanowires are dispersed in water is preferably 0.5 mPa ⁇ s to 100 mPa ⁇ s, more preferably 1 mPa ⁇ s to 50 mPa ⁇ s.
- Metal nanotube examples of preferable metal conductive fibers other than metal nanowires include metal nanotubes that are hollow fibers. There is no restriction
- the shape of the metal nanotube may be a single layer or a multilayer, but a single layer is preferable from the viewpoint of excellent conductivity and thermal conductivity.
- the thickness (the difference between the outer diameter and the inner diameter) of the metal nanotube is preferably 3 nm to 80 nm, and more preferably 3 nm to 30 nm. When the thickness is 3 nm or more, sufficient oxidation resistance is obtained, and when the thickness is 80 nm or less, the occurrence of light scattering due to the metal nanotubes is suppressed.
- the average minor axis length of the metal nanotube is 1 nm to 150 nm as in the case of the metal nanowire.
- a preferable average minor axis length is the same as that of metal nanowires.
- the average major axis length is preferably 1 ⁇ m to 40 ⁇ m, more preferably 3 ⁇ m to 35 ⁇ m, and even more preferably 5 ⁇ m to 30 ⁇ m.
- the method for producing the metal nanotube is not particularly limited and may be appropriately selected depending on the intended purpose.
- the method described in US Patent Application Publication No. 2005/0056118 may be used.
- composition of the present invention contains at least one compound selected from the compound represented by the following general formula (1) and the compound represented by the following general formula (2).
- R 1 and R 2 each independently represents an alkyl group, an aryl group, an alkoxy group, an aryloxy group or a halogen atom
- R 3 represents an alkyl group or an aryl group. At least two of R 1 , R 2 and R 3 may be linked to each other via a divalent or higher-valent organic group or a single bond.
- one hydrogen atom is removed from at least one of R 1 , R 2 and R 3 to form a monovalent group, and the monovalent group is divalent or higher. It includes a compound in which a plurality of structures represented by the general formula (1) connected to at least one of R 1 , R 2 and R 3 through an organic group or a single bond exist in one molecule.
- R 4 and R 5 each independently represents an alkyl group. R 4 and R 5 may be connected to each other via a divalent or higher-valent organic group or a single bond.
- the compound represented by the general formula (2) is a monovalent group by removing one hydrogen atom from at least one of R 4 and R 5 , and this monovalent group is a divalent or higher organic group or It includes a compound in which a plurality of structures represented by the general formula (2) connected to at least one of R 4 and R 5 through a single bond exist in one molecule.
- the alkyl group represented by R 1 , R 2 and R 3 in the general formula (1) represents a linear, branched or cyclic substituted or unsubstituted alkyl group, preferably having 1 to 50 carbon atoms, more preferably Has 1 to 30 carbon atoms, particularly preferably 1 to 20 carbon atoms.
- Preferred examples include methyl, ethyl, n-propyl, isopropyl, cyclopropyl, butyl, isobutyl, t-butyl, sec-butyl, pentyl, isopentyl, neopentyl, t-pentyl, hexyl, cyclohexyl, heptyl, cyclopentyl, octyl, Examples include 2-ethylhexyl, nonyl, decyl, dodecyl, tetradecyl, hexadecyl, octadecyl, eicosyl, docosyl, triacontyl and the like.
- the alkyl group represented by R 1 , R 2 and R 3 may further have a substituent.
- Substituents include halogen atoms, alkyl groups (including cycloalkyl groups), alkenyl groups (including cycloalkenyl groups and bicycloalkenyl groups), alkynyl groups, aryl groups, cyano groups, hydroxyl groups, nitro groups, carboxyl groups, Alkoxy, aryloxy, acyloxy, carbamoyloxy, alkoxycarbonyloxy, aryloxycarbonyloxy, amino (including anilino), acylamino, aminocarbonylamino, alkoxycarbonylamino, aryloxycarbonylamino Groups, acyl groups, aryloxycarbonyl groups, alkoxycarbonyl groups, carbamoyl groups and the like.
- examples of the substituent include a halogen atom (for example, a chlorine atom, a bromine atom, an iodine atom), an alkyl group [(represents a linear, branched, cyclic substituted or unsubstituted alkyl group.
- a halogen atom for example, a chlorine atom, a bromine atom, an iodine atom
- an alkyl group [(represents a linear, branched, cyclic substituted or unsubstituted alkyl group.
- cycloalkyl group (Preferably an alkyl group having 1 to 30 carbon atoms such as methyl, ethyl, n-propyl, isopropyl, t-butyl, n-octyl, eicosyl, 2-chloroethyl, 2-cyanoethyl, 2-ethylhexyl), cycloalkyl group ( Preferably, it is a substituted or unsubstituted cycloalkyl group having 3 to 30 carbon atoms, such as cyclohexyl, cyclopentyl, 4-n-dodecylcyclohexyl, or a bicycloalkyl group (preferably a substituted or unsubstituted group having 5 to 30 carbon atoms).
- a hydrogen atom from a bicycloalkyl group that is, a bicycloalkane having 5 to 30 carbon atoms.
- Monovalent groups removed such as bicyclo [1.2.2] heptan-2-yl, bicyclo [2.2.2] octane-3-yl), and tricyclo structures with more ring structures Among the substituents described below, an alkyl group (for example, an alkyl group of an alkylthio group also represents an alkyl group of such a concept), an alkenyl group (preferably a substituent having 2 to 30 carbon atoms) Or an unsubstituted alkenyl group such as vinyl, allyl, prenyl, geranyl, oleyl), a cycloalkenyl group (preferably a substituted or unsubstituted cycloalkenyl group having 3 to 30 carbon atoms, that is, having 3 to 30 carbon atoms)
- alkynyl group preferably a substituted or unsubstituted alkynyl group having 2 to 30 carbon atoms, such as ethynyl, propargyl, trimethylsilylethynyl group
- an aryl group preferably a substituted or unsubstituted aryl group having 6 to 30 carbon atoms, For example, phenyl, p-tolyl, naphthyl, m-chlorophenyl, o-hexadecanoylaminophenyl
- a heterocyclic group preferably a 5- or 6-membered substituted or unsubstituted aromatic or non-aromatic heterocyclic compound A monovalent group obtained by removing one hydrogen atom, and more preferably a 5- or 6-membered aromatic heterocyclic group having 3 to 30 carbon atoms, such as 2-furanyl, 2-thienyl, 2- Pyrimidinyl, 2-benzothiazolinyl), cyano group,
- amino group preferably an amino group, a substituted or unsubstituted alkylamino group having 1 to 30 carbon atoms, a substituted or unsubstituted anilino group having 6 to 30 carbon atoms, such as amino, methylamino, dimethylamino, anilino, N-methyl-anilino, diphenylamino), acylamino group (preferably formylamino group, substituted or unsubstituted alkylcarbonylamino group having 1 to 30 carbon atoms, substituted or unsubstituted arylcarbonylamino group having 6 to 30 carbon atoms) Groups such as formylamino, acetylamino, pivaloylamino, lauroylamino, benzoylamino, 3,4,5-tri-n-octyloxyphenylcarbonylamino), aminocarbonylamino groups (preferably substituted with 1 to 30 carbon atoms) Or unsubstituted
- alkylthio group preferably substituted or unsubstituted alkylthio group having 1 to 30 carbon atoms, such as methylthio, ethylthio, n-hexadecylthio
- arylthio group preferably substituted or unsubstituted arylthio group having 6 to 30 carbon atoms
- a heterocyclic thio group preferably a substituted or unsubstituted heterocyclic thio group having 2 to 30 carbon atoms, such as 2-benzothiazolylthio, 1 -Phenyltetrazol-5-ylthio
- a sulfamoyl group preferably a substituted or unsubstituted sulfamoyl group having 0 to 30 carbon atoms, such as N-ethylsulf
- Alkyl and arylsulfonyl groups preferably substituted or unsubstituted alkylsulfonyl groups having 1 to 30 carbon atoms, substituted or unsubstituted arylsulfonyl groups having 6 to 30 carbon atoms such as methylsulfonyl, ethylsulfonyl, phenylsulfonyl, p- Methylphenylsulfonyl
- acyl group preferably formyl group, substituted or unsubstituted alkylcarbonyl group having 2 to 30 carbon atoms, substituted or unsubstituted arylcarbonyl group having 7 to 30 carbon atoms, and substituted group having 4 to 30 carbon atoms
- a heterocyclic carbonyl group bonded to a carbonyl group with an unsubstituted carbon atom such as acetyl, pivaloyl, 2-chloroacetyl, stearoy
- a carbamoyl group (preferably a substituted or unsubstituted carbamoyl having 1 to 30 carbon atoms such as carbamoyl, N-methylcarbamoyl, N, N-dimethylcarbamoyl, N, N-di-n-octylcarbamoyl, N- (methyl Sulfonyl) carbamoyl), aryl and heterocyclic azo groups (preferably substituted or unsubstituted arylazo groups having 6 to 30 carbon atoms, substituted or unsubstituted heterocyclic azo groups having 3 to 30 carbon atoms, such as phenylazo, p- Chlorophenylazo, 5-ethylthio-1,3,4-thiadiazol-2-ylazo), imide group (preferably N-succinimide, N-phthalimide), phosphino group (preferably substituted or non-substituted having 2 to 30 carbon atoms) Substituted
- a substituted or unsubstituted phosphinylamino group such as dimethoxyphosphinylamino, dimethylaminophosphinylamino
- a silyl group preferably a substituted or unsubstituted silyl group having 3 to 30 carbon atoms, such as Trimethylsilyl, t-butyldimethylsilyl, phenyldimethylsilyl Representing the.
- those having a hydrogen atom may be substituted with the above groups by removing this.
- Examples of such functional groups include alkylcarbonylaminosulfonyl group, arylcarbonylaminosulfonyl group, alkylsulfonylaminocarbonyl group, arylsulfonylaminocarbonyl group, methylsulfonylaminocarbonyl, p-methylphenylsulfonylaminocarbonyl, acetylaminosulfonyl And benzoylaminosulfonyl group.
- the alkoxy group represented by R 1 and R 2 represents a linear, branched or cyclic substituted or alkoxy group. Preferably, it has 1 to 50 carbon atoms, more preferably 1 to 30 carbon atoms, and particularly preferably 1 to 20 carbon atoms.
- Preferred examples include methoxy, ethoxy, n-propoxy, isopropoxy, cyclopropoxy, butoxy, isobutoxy, t-butoxy, sec-butoxy, pentyloxy, isopentyloxy, neopentyloxy, t-pentyloxy, hexyloxy, Cyclohexyloxy, heptyloxy, cyclopentyloxy, octyloxy, 2-ethylhexyloxy, nonyloxy, decyloxy, dodecyloxy, tetradecyloxy, hexadecyloxy, octadecyloxy, eicosyloxy, docosyloxy, triacontyloxy, etc.
- the aryl group represented by R 1 , R 2 and R 3 represents a substituted or unsubstituted aryl group, preferably having 6 to 50 carbon atoms, more preferably 6 to 30 carbon atoms, and particularly preferably 6 to 6 carbon atoms. 20.
- Preferred examples include phenyl, 2-methylphenyl, 3-methylphenyl, 4-methylphenyl, 2-ethylphenyl, 4-ethylphenyl, 2,4-dimethylphenyl, 2,6-dimethylphenyl, 2,4, 6-trimethylphenyl, 1-naphthyl, 2-naphthyl, 2-chlorophenyl, 3-chlorophenyl, 4-chlorophenyl, 2-methoxyphenyl, 3-methoxyphenyl, 4-methoxyphenyl, 2-benzylphenyl, 4-benzylphenyl, Examples thereof include 2-methylcarbonylphenyl and 4-methylcarbonylphenyl.
- the aryl group represented by R 1 , R 2 and R 3 may further have a substituent.
- the aryloxy group represented by R 1 and R 2 represents a substituted or unsubstituted aryloxy group, preferably having 6 to 50 carbon atoms, more preferably 6 to 30 carbon atoms, and particularly preferably 6 to 20 carbon atoms. It is.
- Preferred examples include phenoxy, 2-methylphenoxy, 3-methylphenoxy, 4-methylphenoxy, 2-ethylphenoxy, 4-ethylphenoxy, 2,4-dimethylphenoxy, 2,4-di-t-butylphenoxy, 2,6-di-t-butylphenoxy, 2,6-dimethylphenoxy, 2,6-di-t-butyl-4-methylphenoxy, 2,4,6-trimethylphenoxy, 2,4,6-tri- t-butylphenoxy, 1-naphthyloxy, 2-naphthyloxy, 2-chlorophenoxy, 3-chlorophenoxy, 4-chlorophenoxy, 2-methoxyphenoxy, 3-methoxyphenoxy, 4-methoxyphenoxy, 2-benzylphenoxy, 4-benzylphenoxy, 2-methylcarbonylphenoxy, 4-methylcarbonylphen Or the like can be mentioned phenoxy.
- More preferable examples include phenyl, 2,4-di-t-butylphenoxy, 2,4,6-tri-t-butylphenoxy and the like.
- the aryloxy group represented by R 1 and R 2 may further have a substituent. Examples of the substituent include the substituents for the alkyl group represented by R 1, R 2 and R 3 described above.
- R 1 and R 2 are an alkoxy group or an aryloxy group
- R 3 is an aryl group.
- R 1 and R 2 are preferably an alkoxy group or an aryloxy group
- R 3 is preferably an alkyl group or an aryl group.
- R 1 , R 2 and R 3 may be linked to each other via a divalent or higher organic group or a single bond.
- one hydrogen atom is removed from at least one of R 1 , R 2 and R 3 to form a monovalent group, and the monovalent group is divalent or higher. It includes a compound in which a plurality of structures represented by the general formula (1) connected to at least one of R 1 , R 2 and R 3 through an organic group or a single bond exist in one molecule.
- an alkyl group, aryl group, alkoxy group or aryloxy group represented by at least one of R 1 , R 2 and R 3 an alkylene group, an arylene group, an oxyalkylene
- a compound linked to at least one of a group and an aryloxy group by removing one hydrogen atom from an alkyl group, aryl group, alkoxy group or aryloxy group represented by at least one of R 1 , R 2 and R 3 , an alkylene group, an arylene group, an oxyalkylene
- alkyl group, aryl group, alkoxy group, or aryloxy group represented by at least one of R 1 , R 2, and R 3 has the substituent
- one hydrogen atom is removed from the substituent.
- Examples of the divalent or higher organic group include groups that are divalent or higher by removing one or more hydrogen atoms from the substituents enumerated above for the alkyl groups represented by R 1 , R 2, and R 3. be able to.
- organic groups or single bonds a single bond, or one or more alkyl groups, aryl groups, bis-aryl groups, arylalkylaryl groups, aryloxyaryl groups, alkoxyalkyl groups, alkoxyaryl groups, or alkylaryl groups.
- a group that is divalent or higher by removing a hydrogen atom is preferred.
- the number of phosphorus atoms in one molecule is 2 or more and 20
- the number is preferably 2 or less, more preferably 2 or more and 10 or less, and even more preferably 2 or more and 5 or less.
- a phosphite compound described in JP-T-2011-527357 can be suitably used as a compound represented by the general formula (1).
- R 4 and R 5 each represents an alkyl group.
- the alkyl group represented by R 4 and R 5 represents a linear, branched or cyclic substituted or alkyl group. Preferably, it has 1 to 50 carbon atoms, more preferably 2 to 30 carbon atoms, and particularly preferably 2 to 20 carbon atoms.
- Preferred examples include methyl, ethyl, n-propyl, isopropyl, cyclopropyl, butyl, isobutyl, t-butyl, sec-butyl, pentyl, isopentyl, neopentyl, t-pentyl, hexyl, cyclohexyl, heptyl, cyclopentyl, octyl, Examples include 2-ethylhexyl, nonyl, decyl, dodecyl, tetradecyl, hexadecyl, octadecyl, eicosyl, docosyl, triacontyl and the like.
- the alkyl group represented by R 4 and R 5 may further have a substituent.
- Substituents include halogen atoms, alkyl groups (including cycloalkyl groups), alkenyl groups (including cycloalkenyl groups and bicycloalkenyl groups), alkynyl groups, aryl groups, cyano groups, hydroxyl groups, nitro groups, carboxyl groups, Alkoxy, aryloxy, acyloxy, carbamoyloxy, alkoxycarbonyloxy, aryloxycarbonyloxy, amino (including anilino), acylamino, aminocarbonylamino, alkoxycarbonylamino, aryloxycarbonylamino Examples thereof include a group, an acyl group, an aryloxycarbonyl group, an alkoxycarbonyl group, and a carbamoyl group.
- an alkoxycarbonylalkylene group is preferred.
- the alkoxycarbonyl group in the alkoxycarbonylalkylene group preferably has 2 to 50 carbon atoms, more preferably 5 to 30 carbon atoms, and particularly preferably 9 to 20 carbon atoms.
- R 4 and R 5 in the general formula (2) may be connected to each other via a divalent or higher-valent organic group or a single bond.
- the divalent or higher-valent organic group is the same as that described in the general formula (1), and the preferred range is also the same.
- the compound represented by the general formula (2) is a monovalent group by removing one hydrogen atom from at least one of R 4 and R 5 , and this monovalent group is a divalent or higher organic group or It includes a compound in which a plurality of structures represented by the general formula (2) connected to at least one of R 4 and R 5 through a single bond exist in one molecule.
- the divalent or higher-valent organic group is the same as that described in the general formula (1), and the preferred range is also the same.
- the content of the component compound (b) in the conductive composition of the present invention is 0 per 1 g of the metal conductive fiber (a). It is preferably 0.005 mmol or more and 30 mmol or less, and more preferably 0.01 mmol or more and 5 mmol or less.
- the addition amount is 0.005 mmol or more, a sufficient effect due to the addition of the component compound (b) tends to be obtained, and when the addition amount is 30 mmol or less, it is estimated that it is caused by contact inhibition between the metal conductive fibers. The deterioration of the resistance value tends to be suppressed.
- the molecular weight of the component compound is preferably 200 or more and 10,000 or less, more preferably 250 or more and 5000 or less, and further preferably 250 or more and 2000 or less.
- the molecular weight is 200 or more, volatility is suppressed and the heat resistance tends to be excellent.
- the molecular weight is 10,000 or less, a decrease in diffusibility in the film is suppressed, and a sufficient effect tends to be obtained.
- a conductive composition contains multiple types of compounds as (b) component compound, it is preferable that all those compounds are 200-10000.
- the compound represented by the general formula (2) is preferable from the viewpoint of conductivity under high temperature conditions, and the general formula (1) from the viewpoint of conductivity in the presence of ozone. ) Is preferred.
- the conductive composition of the present invention is applied on a substrate to form a conductive layer.
- the electrically conductive composition of this invention contains (b) component compound, as above-mentioned, (b) component compound is added to the electroconductive layer containing (a) metal conductive fiber, Even if it is added to the layer in contact with the conductive layer, the effect can be exhibited. Further, (a) the component compound (b) is added to another layer (for example, a soluble protective layer or an undercoat layer) in contact with the conductive layer containing the metal conductive fiber, and the conductive layer is transferred from this other layer.
- Component compounds may be introduced by diffusing.
- V 3 represents a hydrogen atom or a substituent.
- V 4 represents a hydrogen atom or a substituent.
- V 5 represents a hydrogen atom or a substituent, and R 51 and R 52 each independently represent a hydrogen atom or a group that can be substituted with a nitrogen atom.
- V 6 represents a hydrogen atom or a substituent, and R 61 and R 62 each independently represent a hydrogen atom or a group that can be substituted with a nitrogen atom.
- V 7 represents a hydrogen atom or a substituent, and R 71 and R 72 each independently represent a hydrogen atom or a substituent.
- V 8 represents a hydrogen atom or a substituent
- R 81 and R 82 each independently represent a hydrogen atom or a substituent
- V 9 represents a hydrogen atom or a substituent
- R 91 , R 92 , R 93 and R 94 each independently represent a hydrogen atom or a group that can be substituted with a nitrogen atom.
- V 10 represents a hydrogen atom or a substituent
- R 101 , R 102 , R 103, and R 104 each independently represent a hydrogen atom or a group that can be substituted with a nitrogen atom.
- R 111 represents a hydrogen atom or a group capable of substituting for a nitrogen atom
- V 111 , V 112 , V 113 and V 114 each independently represents a hydrogen atom or a substituent
- 111 and V 112 , and V 113 and V 114 may be connected to each other to form a bicyclo ring or a tricyclo ring.
- the effect of using at least one compound selected from the compounds represented by the general formulas (3) to (11) together with the component compound (b) is not clear, it can be considered as follows. It can.
- the compounds represented by the general formulas (3) to (11) are considered to have a function of deactivating radical species generated in the conductive layer or in a layer in contact with the conductive layer. Therefore, the combined use of the compounds represented by the general formulas (3) to (11) capable of deactivating radical species and the component compound (b) capable of deactivating peroxide generated by the radical species is as follows: It is suitable from the viewpoint of suppressing the decrease in conductivity.
- V 3 represents a hydrogen atom or a substituent.
- the bonding mode of the group represented by V 3 in the general formula (3) any number in the range of 1 to 4 is bonded to any substitutable position of the cyclic structure included in the general formula (3).
- examples of the preferable group include the substituents described for the alkyl group represented by R 1 , R 2 and R 3 in the general formula (1).
- each group may be the same or different, and may be bonded to each other to form a ring. .
- the specific example of a compound represented by General formula (3) below is shown. However, the present invention is not limited to these.
- V 4 represents a hydrogen atom or a substituent.
- the bonding mode of the group represented by V 4 in the general formula (4) an arbitrary number of groups in the range of 1 to 4 is bonded to any substitutable position of the cyclic structure included in the general formula (4).
- examples of preferred groups include the substituents described for the alkyl groups represented by R 1 , R 2 and R 3 in the general formula (1).
- each group may be the same or different, and may be bonded to each other to form a ring. .
- the specific example of a compound represented by General formula (4) below is shown. However, the present invention is not limited to these.
- V 5 represents a hydrogen atom or a substituent.
- the bonding mode of the group represented by V 5 in the general formula (5) any number in the range of 1 to 4 is bonded to any substitutable position of the cyclic structure included in the general formula (5).
- examples of the preferable group include the substituents described for the alkyl group represented by R 1 , R 2 and R 3 in the general formula (1).
- each group may be the same or different, and may be bonded to each other to form a ring. .
- R 51 and R 52 each independently represent a hydrogen atom or a group that can be substituted with a nitrogen atom.
- Preferred examples of the group capable of substituting for a nitrogen atom include the substituents described for the alkyl group represented by R 1 , R 2 and R 3 in the general formula (1).
- V 6 represents a hydrogen atom or a substituent.
- the bonding mode of the group represented by V 6 in the general formula (6) any number in the range of 1 to 4 is bonded to any substitutable position of the cyclic structure included in the general formula (6).
- examples of the preferable group include the substituents described for the alkyl group represented by R 1 , R 2 and R 3 in the general formula (1).
- each group may be the same or different, and may be bonded to each other to form a ring. .
- R 61 and R 62 each independently represent a hydrogen atom or a group that can be substituted with a nitrogen atom.
- Preferred examples of the group capable of substituting for a nitrogen atom include the substituents described for the alkyl group represented by R 1 , R 2 and R 3 in the general formula (1).
- V 7 represents a hydrogen atom or a substituent.
- the bonding mode of the group represented by V 7 in the general formula (7) any number in the range of 1 to 4 is bonded to any substitutable position of the cyclic structure included in the general formula (7).
- examples of the preferred group include the substituents described for the alkyl group represented by R 1 , R 2 and R 3 in the general formula (1).
- each group may be the same or different, and may be bonded to each other to form a ring. .
- R 71 and R 72 examples include the substituents described for the alkyl group represented by R 1 , R 2 and R 3 described above, preferably an alkyl group, an alkenyl group, An alkynyl group or an aryl group, and preferred examples of each are the examples described for R 1 , R 2 and R 3 described above.
- R 71 or R 72 represents a substituent
- these groups may further have a substituent.
- the substituent demonstrated by the alkyl group represented by R ⁇ 1 >, R ⁇ 2 > and R ⁇ 3 > of the above-mentioned general formula (1) can be mentioned.
- V 8 represents a hydrogen atom or a substituent.
- the bonding mode of the group represented by V 8 in the general formula (8) an arbitrary number of 1 to 4 bonds can be bonded to any substitutable position of the cyclic structure included in the general formula (8).
- examples of the preferred group include the substituents described for the alkyl group represented by R 1 , R 2 and R 3 in the general formula (1).
- each group may be the same or different, and may be bonded to each other to form a ring. .
- R 81 and R 82 each independently represents a hydrogen atom or a substituent.
- substituent represented by R 81 and R 82 include the substituents described for the alkyl group represented by R 1 , R 2 and R 3 described above, preferably an alkyl group, an alkenyl group, An alkynyl group or an aryl group, and preferred examples of each are the examples described for R 1 , R 2 and R 3 described above.
- R 81 or R 82 represents a substituent, these groups may further have a substituent.
- the substituent demonstrated by the alkyl group represented by R ⁇ 1 >, R ⁇ 2 > and R ⁇ 3 > of the above-mentioned general formula (1) can be mentioned.
- V 9 represents a hydrogen atom or a substituent.
- the bonding mode of the group represented by V 9 in the general formula (9) any number in the range of 1 to 4 is bonded to any substitutable position of the cyclic structure included in the general formula (9).
- examples of preferred groups include the substituents described for the alkyl groups represented by R 1 , R 2 and R 3 in the general formula (1).
- each group may be the same or different, and may be bonded to each other to form a ring. .
- R 91 , R 92 , R 93 and R 94 each independently represent a hydrogen atom or a group capable of substituting for a nitrogen atom.
- Preferred examples of the group capable of substituting for a nitrogen atom include the substituents described for the alkyl group represented by R 1 , R 2 and R 3 in the general formula (1).
- V 10 represents a hydrogen atom or a substituent.
- the bonding mode of the group represented by V 10 in the general formula (10) an arbitrary number of groups in the range of 1 to 4 are bonded to any substitutable position of the cyclic structure included in the general formula (10).
- examples of preferred groups include the substituents described for the alkyl groups represented by R 1 , R 2 and R 3 in the general formula (1).
- each group may be the same or different, and may be bonded to each other to form a ring. .
- R 101 , R 102 , R 103 and R 104 each independently represent a hydrogen atom or a group capable of substituting for a nitrogen atom.
- Preferred examples of the group capable of substituting for a nitrogen atom include the substituents described for the alkyl group represented by R 1 , R 2 and R 3 in the general formula (1).
- R 111 represents a hydrogen atom or a group capable of substituting for a nitrogen atom
- V 111 , V 112 , V 113 and V 114 each independently represents a hydrogen atom or a substituent
- 111 and V 112 , and V 113 and V 114 may be connected to each other to form a bicyclo ring or a tricyclo ring.
- the preferred group is the substituent described for the alkyl group represented by R 1 , R 2 and R 3 in the general formula (1).
- V 111 , V 112 , V 113 and V 114 may be the same as or different from each other, and may be bonded to each other to form a ring.
- Any known method can be used for producing the compounds represented by the general formulas (3) to (11). Conditions for producing these compounds, such as temperature, selection of solvent, type and amount of reaction reagent, can be easily set by those skilled in the art and can be determined experimentally. Can be manufactured easily.
- the addition ratio is a molar ratio (general formulas (3) to (11) / (b) with respect to the component compound (b).
- Component compound) is preferably 1000 to 0.001, more preferably 100 to 0.01, and still more preferably 10 to 0.1.
- the compound represented by the general formula (1) or (2) and at least one of the general formulas (3) to (11) are used. It is preferable to combine the compounds represented by one type, and it is more preferable to combine the compound represented by the general formula (2) and the compound represented by at least one of the general formulas (3) to (11). Further, from the viewpoint of conductivity in the presence of ozone, it is represented by the compound represented by the general formula (1) or the compound represented by (2) and at least one of the general formulas (3) to (11).
- the compounds represented by general formula (1) are preferably combined with the compounds represented by at least one of general formulas (3) to (11).
- the conductive composition of the present invention may further contain a polymerizable compound capable of forming a matrix.
- the “matrix” is a general term for substances that include metal conductive fibers to form a layer, and has a function of stably maintaining the dispersion of the metal conductive fibers.
- the matrix may be non-photosensitive or photosensitive.
- the “polymerizable compound capable of forming a matrix” means, as exemplified below, when the matrix is a non-photosensitive matrix, methacrylates, acrylates, and the like that can form organic polymers, and inorganic polymers.
- a matrix it means an addition-polymerizable unsaturated compound contained in a photoresist composition described later.
- the content ratio of the polymerizable compound / metal conductive fiber capable of forming a matrix is 0.001 / 1 to 100/1 by mass ratio.
- the range of is preferable. By selecting in such a range, an appropriate adhesive strength and surface resistance of the conductive layer to the substrate can be obtained.
- the content ratio of the polymerizable compound / metal conductive fiber capable of forming the matrix is more preferably in the range of 0.01 / 1 to 20/1, more preferably in the range of 1/1 to 15/1, in terms of mass ratio. A range of / 1 to 8/1 is particularly preferred.
- a metal conductive fiber and the polymeric compound which can form a matrix are separately provided on a base material, and an electroconductive layer is formed. Also good. In this method, it is not necessary to contain a polymerizable compound capable of forming a matrix in the conductive composition.
- Non-photosensitive matrix The non-photosensitive matrix will be described. Suitable non-photosensitive matrices include those containing organic polymers or inorganic polymers.
- organic polymer examples include polymethacrylate (eg, a copolymer containing polymethyl methacrylate and polymethacrylic acid ester), polyacrylate (eg, a copolymer containing polymethyl acrylate and polyacrylic acid ester), and polyacrylonitrile.
- polymethacrylate eg, a copolymer containing polymethyl methacrylate and polymethacrylic acid ester
- polyacrylate eg, a copolymer containing polymethyl acrylate and polyacrylic acid ester
- polyacrylonitrile examples include polyacrylonitrile.
- Polyvinyl alcohol polyvinyl alcohol, polyester (eg, polyethylene terephthalate (PET), polyethylene naphthalate, polycarbonate), phenol or cresol-formaldehyde resin (eg, Novolacs®), polystyrene, polyvinyl toluene, polyvinyl xylene, polyimide, polyamide, polyamide Highly aromatic polymers such as imide, polyetherimide, polysulfide, polysulfone, polyphenylene, and polyphenyl ether, poly Retan (PU), epoxy resin, polyolefin (eg, polyethylene, polypropylene, polycycloolefin), acrylonitrile-butadiene-styrene copolymer (ABS), cellulose derivative, silicone, silicon-containing polymer (eg, polysilsesquioxane) And polysilane), polyvinyl chloride (PVC), polyacetate, polynorbornene, synthetic rubber (eg, E
- an alkoxide compound of an element selected from the group consisting of Si, Ti, Zr and Al (hereinafter, also referred to as “specific alkoxide compound”) is used as a polymerizable compound capable of forming a matrix, and this is hydrolyzed.
- specific alkoxide compound examples thereof include sol-gel cured products obtained by decomposition and polycondensation, and further heating and drying as desired.
- the sol-gel cured product is preferable because it can be easily manufactured with high resistance to scratches and abrasion.
- the specific alkoxide compound is preferably a compound represented by the following general formula (12).
- M represents an element selected from Si, Ti, Al and Zr
- R p and R q each independently represent a hydrogen atom or a hydrocarbon group
- a represents an integer of 2 to 4 Indicates.
- Each hydrocarbon group represented by R p and R q in the general formula (12) is preferably an alkyl group or an aryl group.
- the carbon number in the case of showing an alkyl group is preferably 1 to 18, more preferably 1 to 8, and still more preferably 1 to 4.
- a phenyl group is preferable.
- the alkyl group or aryl group may further have a substituent, and examples of the substituent that can be introduced are the alkyl groups represented by R 1 , R 2, and R 3 in the general formula (1).
- a substituent can be mentioned.
- This compound preferably has a molecular weight of 1000 or less. Specific examples of the compound represented by the general formula (12) are shown below, but the present invention is not limited thereto.
- Alkoxysilane When M is Si and a is 2, that is, as dialkoxysilane, for example, dimethyldimethoxysilane, diethyldimethoxysilane, propylmethyldimethoxysilane, dimethyldiethoxysilane, diethyldiethoxysilane, dipropyldiethoxysilane, ⁇ -Chloropropylmethyldiethoxysilane, acetoxymethylmethyldiethoxysilane, acetoxymethylmethyldimethoxysilane, phenylmethyldimethoxysilane, phenylethyldiethoxysilane, phenylmethyldipropoxysilane, vinylmethyldimethoxysilane, vinylmethyldiethoxysilane, vinyl Examples include methyldibutoxysilane, isopropenylmethyldimethoxysilane, isopropenylmethyldiethoxysilane, and isopropenylmethyldibutoxy
- Rukoto can be given from the viewpoint of easy availability and adhesiveness with the hydrophilic layer.
- M is Si and a is 3, that is, as trialkoxysilane, for example, methyltrimethoxysilane, ethyltrimethoxysilane, propyltrimethoxysilane, methyltriethoxysilane, ethyltriethoxysilane, propyltriethoxysilane, Examples include chloromethyltriethoxysilane, vinyltrimethoxysilane, isopropenyltrimethoxysilane, isopropenyltriethoxysilane, and the like.
- methyltrimethoxysilane ethyltrimethoxysilane, methyltriethoxysilane, ethyltriethoxysilane, and the like from the viewpoint of easy availability and the adhesion to the hydrophilic layer. .
- M is Si and a is 4, that is, as tetraalkoxysilane, for example, tetramethoxysilane, tetraethoxysilane, tetrapropoxysilane, tetrabutoxysilane, methoxytriethoxysilane, ethoxytrimethoxysilane, methoxytripropoxysilane Ethoxytripropoxysilane, propoxytrimethoxysilane, propoxytriethoxysilane, dimethoxydiethoxysilane and the like.
- tetramethoxysilane, tetraethoxysilane and the like are particularly preferable.
- Alkoxy titanate When M is Ti and a is 2, that is, as dialkoxytitanate, for example, dimethyldimethoxytitanate, diethyldimethoxytitanate, propylmethyldimethoxytitanate, dimethyldiethoxytitanate, diethyldiethoxytitanate, dipropyldiethoxytitanate, phenyl Examples thereof include ethyl diethoxy titanate, phenyl methyl dipropoxy titanate, and dimethyl dipropoxy titanate.
- M is Ti and a is 3, that is, as trialkoxy titanate, for example, methyl trimethoxy titanate, ethyl trimethoxy titanate, propyl trimethoxy titanate, methyl triethoxy titanate, ethyl triethoxy titanate, propyl triethoxy titanate, Examples thereof include chloromethyl triethoxy titanate, phenyl trimethoxy titanate, phenyl triethoxy titanate, and phenyl tripropoxy titanate.
- trialkoxy titanate for example, methyl trimethoxy titanate, ethyl trimethoxy titanate, propyl trimethoxy titanate, methyl triethoxy titanate, ethyl triethoxy titanate, propyl triethoxy titanate.
- examples of the tetraalkoxy titanate include tetramethoxy titanate, tetraethoxy titanate, tetrapropoxy titanate, tetraisopropoxy titanate, and tetrabutoxy titanate.
- M Zr, that is, as an alkoxide of zirconium, for example, zirconate corresponding to the compounds exemplified as containing titanium can be exemplified.
- M Al
- the alkoxide of aluminum includes, for example, trimethoxy aluminate, triethoxy aluminate, tripropoxy aluminate, tetraethoxy aluminate and the like.
- the conductive layer having a sol-gel cured product as a matrix is formed by applying an aqueous solution containing a specific alkoxide compound as a coating liquid (hereinafter also referred to as “sol-gel coating liquid”) on a substrate to form a coating liquid film,
- a coating liquid film a reaction of hydrolysis and polycondensation of the specific alkoxide compound (hereinafter, the reaction of hydrolysis and polycondensation is also referred to as “sol-gel reaction”) is performed, and further heated as necessary to produce water. It is preferable to form by evaporating and drying.
- a dispersion of metal conductive fibers may be prepared separately and mixed with a specific alkoxide compound. Furthermore, after preparing a solution containing the specific alkoxide compound, the solution is heated to hydrolyze and polycondensate at least a part of the specific alkoxide compound to form a sol state. The solution in the sol state and the metal conductive fiber A mixture of the dispersion and the sol-gel coating liquid may be used.
- catalyst When the conductive composition of the present invention contains the specific alkoxide, it is preferable to add an acidic catalyst or a basic catalyst in order to promote the sol-gel reaction.
- an acidic catalyst or a basic catalyst in order to promote the sol-gel reaction.
- Any catalyst can be used as long as it promotes hydrolysis and polycondensation reactions of the alkoxide compound.
- Such a catalyst includes an acid or a basic compound and is used as it is or dissolved in a solvent such as water or alcohol (hereinafter, these are comprehensively referred to as an acidic catalyst and a basic compound, respectively). Also referred to as catalyst).
- the concentration at which the acid or basic compound is dissolved in the solvent is not particularly limited, and may be appropriately selected depending on the characteristics of the acid or basic compound used, the desired content of the catalyst, and the like.
- concentration of the acid or basic compound constituting the catalyst is high, the hydrolysis and polycondensation rates tend to increase.
- a basic catalyst having a too high concentration is used, a precipitate may be generated and appear as a defect in the conductive layer. Therefore, when a basic catalyst is used, the concentration is 1 N in terms of concentration in an aqueous solution. The following is preferable.
- the type of acidic catalyst or basic catalyst is not particularly limited, but when it is necessary to use a highly concentrated catalyst, a compound that hardly remains in the conductive layer after drying is preferable.
- the acidic catalyst include hydrogen halides such as hydrochloric acid, nitric acid, sulfuric acid, sulfurous acid, hydrogen sulfide, perchloric acid, hydrogen peroxide, carbonic acid, carbonic acid such as formic acid and acetic acid, and the structure represented by RCOOH.
- Examples thereof include substituted carboxylic acids in which R in the formula is substituted with other elements or substituents, sulfonic acids such as benzenesulfonic acid, etc., and basic catalysts include ammoniacal bases such as aqueous ammonia and amines such as ethylamine and aniline Is mentioned.
- a Lewis acid catalyst comprising a metal complex can also be preferably used.
- a particularly preferred catalyst is a metal complex catalyst, a metal element selected from Group 2, Group 13, Group 4 and Group 5 of the periodic table and ⁇ -diketone, ketoester, hydroxycarboxylic acid or ester thereof, It is a metal complex composed of an oxo- or hydroxy-oxygen-containing compound selected from amino alcohols and enolic active hydrogen compounds.
- Group 2 elements such as Mg, Ca, St and Ba; Group 13 elements such as Al and Ga; Group 4 elements such as Ti and Zr; and Group 2 elements such as V, Nb and Ta Group 5 elements are preferable, and each form a complex having an excellent catalytic effect. Of these, complexes obtained from Zr, Al and Ti are excellent and preferred.
- an oxo- or hydroxy-oxygen-containing compound constituting the ligand of the metal complex is a ⁇ -diketone such as acetylacetone (2,4-pentanedione) or 2,4-heptanedione, methyl acetoacetate, acetoacetic acid Ketoesters such as ethyl and butylacetoacetate, lactic acid, methyl lactate, salicylic acid, ethyl salicylate, phenyl salicylate, malic acid, tartaric acid, methyl tartrate and other hydroxycarboxylic acids and esters thereof, 4-hydroxy-4-methyl-2-pentanone , 4-hydroxy-2-pentanone, 4-hydroxy-4-methyl-2-heptanone, ketoalcohols such as 4-hydroxy-2-heptanone, monoethanolamine, N, N-dimethylethanolamine, N-methyl- Monoethanolamine, diethano Amino alcohols such as amine and triethanolamine, enol
- a preferred ligand is an acetylacetone derivative.
- the acetylacetone derivative refers to a compound having a substituent on the methyl group, methylene group or carbonyl carbon of acetylacetone.
- Substituents for substitution on the methyl group of acetylacetone are all straight-chain or branched alkyl groups having 1 to 3 carbon atoms, acyl groups, hydroxyalkyl groups, carboxyalkyl groups, alkoxy groups, alkoxyalkyl groups, and acetylacetone
- the substituents that substitute for the methylene group are carboxyl groups, both straight-chain or branched carboxyalkyl groups and hydroxyalkyl groups having 1 to 3 carbon atoms, and the substituent that substitutes for the carbonyl carbon of acetylacetone is carbon number Is an alkyl group of 1 to 3, in which case a hydrogen atom is added to the carbonyl oxygen to form a hydroxyl group.
- acetylacetone derivatives include ethylcarbonylacetone, n-propylcarbonylacetone, i-propylcarbonylacetone, diacetylacetone, 1-acetyl-1-propionyl-acetylacetone, hydroxyethylcarbonylacetone, hydroxypropylcarbonylacetone, acetoacetate Acetopropionic acid, diacetacetic acid, 3,3-diacetpropionic acid, 4,4-diacetbutyric acid, carboxyethylcarbonylacetone, carboxypropylcarbonylacetone, diacetone alcohol. Of these, acetylacetone and diacetylacetone are particularly preferred.
- the complex of the above acetylacetone derivative and the above metal element is a mononuclear complex in which 1 to 4 molecules of the acetylacetone derivative are coordinated per metal element, and the coordinateable bond of the acetylacetone derivative is the coordinateable bond of the metal element.
- ligands commonly used for ordinary complexes such as water molecules, halogen ions, nitro groups, and ammonio groups may coordinate.
- Examples of preferred metal complexes include tris (acetylacetonato) aluminum complex, di (acetylacetonato) aluminum / aco complex, mono (acetylacetonato) aluminum / chloro complex, di (diacetylacetonato) aluminum complex, ethylacetate Acetate aluminum diisopropylate, aluminum tris (ethylacetoacetate), cyclic aluminum oxide isopropylate, tris (acetylacetonato) barium complex, di (acetylacetonato) titanium complex, tris (acetylacetonato) titanium complex, di-i -Propoxy bis (acetylacetonato) titanium complex salt, zirconium tris (ethyl acetoacetate), zirconium tris (benzoic acid) complex salt, etc.
- ethyl acetoacetate aluminum diisopropylate, aluminum tris (ethyl acetoacetate), di ( Acetylacetonato) titanium complex and zirconium tris (ethylacetoacetate) are preferred.
- the type of the counter salt is arbitrary as long as it is a water-soluble salt that maintains the neutrality of the charge as the complex compound, such as nitrate, Salt forms such as halogenates, sulfates, phosphates, etc., that ensure stoichiometric neutrality are used.
- nitrate nitrate
- Salt forms such as halogenates, sulfates, phosphates, etc., that ensure stoichiometric neutrality are used.
- the metal complex in the coating solution, has a coordinated structure and is stable, and in the dehydration condensation reaction that starts in the heat drying process after coating, it is considered that crosslinking is promoted by a mechanism similar to an acid catalyst.
- this metal complex by using this metal complex, it is possible to obtain a coating solution having excellent stability over time, film surface quality of the conductive layer, and high durability.
- the above metal complex catalyst can be easily obtained as a commercial product, and can also be obtained by a known synthesis method, for example, reaction of each metal chloride with an alcohol.
- the catalyst according to the present invention is used in the sol-gel coating solution in an amount of preferably 0 to 50% by mass, more preferably 5 to 25% by mass, based on the nonvolatile components.
- a catalyst may be used independently or may be used in combination of 2 or more type.
- the sol-gel coating liquid may contain a solvent as desired in order to ensure the formation of a uniform coating liquid film on the substrate.
- solvents include water, ketone solvents (eg, acetone, methyl ethyl ketone, diethyl ketone, etc.), alcohol solvents (eg, methanol, ethanol, 2-propanol, 1-propanol, 1-butanol, tert- Butanol, etc.), chlorinated solvents (eg, chloroform, dichloromethane, etc.), aromatic solvents (eg, benzene, toluene, etc.), ester solvents (eg, ethyl acetate, butyl acetate, isopropyl acetate, etc.), ether solvents ( For example, diethyl ether, tetrahydrofuran, dioxane, etc.), glycol ether solvents (for example, ethylene glycol monomethyl ether, ethylene glycol, ethylene
- the coating liquid film of the sol-gel coating liquid formed on the substrate hydrolysis and condensation reactions of the specific alkoxide compound occur.
- the coating liquid film is heated and dried.
- the heating temperature for promoting the sol-gel reaction is suitably in the range of 30 ° C. to 200 ° C., more preferably in the range of 50 ° C. to 180 ° C.
- the heating and drying time is preferably 10 seconds to 300 minutes, more preferably 1 minute to 120 minutes.
- the above-mentioned sol-gel cured product is preferable in that a conductive layer having high film strength can be obtained.
- the photosensitive matrix includes photoresist compositions suitable for lithographic processes.
- a photoresist composition is included as a matrix, a conductive layer having a conductive region and a non-conductive region in a pattern can be formed by a lithographic process.
- a photopolymerizable composition is particularly preferable because a conductive layer having excellent transparency and flexibility and excellent adhesion to a substrate can be obtained. It is done.
- this photopolymerizable composition will be described.
- the photopolymerizable composition comprises (I) an addition-polymerizable unsaturated compound and (II) a photopolymerization initiator that generates radicals when irradiated with light as basic components. (IV) In addition, additives other than the above components (I) to (III) are included. Hereinafter, these components will be described.
- the addition polymerizable unsaturated compound of component (I) (hereinafter also referred to as “polymerizable compound”) is polymerized by causing an addition polymerization reaction in the presence of a radical.
- a compound having at least one, more preferably two or more, more preferably four or more ethylenically unsaturated bonds at the molecular terminals is used. These have chemical forms such as monomers, prepolymers, i.e. dimers, trimers and oligomers, or mixtures thereof.
- Various kinds of such polymerizable compounds are known, and they can be used as component (I).
- particularly preferred polymerizable compounds are trimethylolpropane tri (meth) acrylate, pentaerythritol tetra (meth) acrylate, dipentaerythritol hexa (meth) acrylate, dipentaerythritol penta (meth) from the viewpoint of film strength.
- Acrylate is particularly preferred.
- the content of component (I) is preferably 2.6% by mass or more and 37.5% by mass or less, and 5.0% by mass or more and 20.0% by mass based on the total mass of the solid content of the conductive composition. It is more preferable that the amount is not more than mass%.
- the photopolymerization initiator of component (II) is a compound that generates radicals when irradiated with light.
- examples of such a photopolymerization initiator include a compound that generates an acid radical that finally becomes an acid upon irradiation with light and a compound that generates another radical.
- the former is referred to as “photoacid generator”, and the latter is referred to as “photoradical generator”.
- Photoacid generators include photoinitiators for photocationic polymerization, photoinitiators for photoradical polymerization, photodecolorants for dyes, photochromic agents, irradiation with actinic rays or radiation used in microresists, etc.
- photoinitiators for photocationic polymerization photoinitiators for photoradical polymerization
- photodecolorants for dyes photochromic agents, irradiation with actinic rays or radiation used in microresists, etc.
- known compounds that generate acid radicals and mixtures thereof can be appropriately selected and used.
- Such a photoacid generator is not particularly limited and may be appropriately selected depending on the intended purpose.
- examples thereof include a triazine compound having at least one di- or tri-halomethyl group or 1,3,4-oxaxene.
- examples thereof include diazole, naphthoquinone-1,2-diazide-4-sulfonyl halide, diazonium salt, phosphonium salt, sulfonium salt, iodonium salt, imide sulfonate, oxime sulfonate, diazodisulfone, disulfone, and o-nitrobenzyl sulfonate.
- imide sulfonate, oxime sulfonate, and o-nitrobenzyl sulfonate which are compounds that generate sulfonic acid
- imide sulfonate, oxime sulfonate, and o-nitrobenzyl sulfonate which are compounds that generate sulfonic acid
- a group that generates an acid radical upon irradiation with actinic rays or radiation, or a compound in which a compound is introduced into the main chain or side chain of the resin for example, US Pat. No. 3,849,137, German Patent 3914407.
- JP-A-63-26653, JP-A-55-164824, JP-A-62-69263, JP-A-63-146038, JP-A-63-163452, JP-A-62-153853 And compounds described in JP-A-63-146029, etc. can be used. Furthermore, compounds described in each specification such as US Pat. No. 3,779,778 and European Patent 126,712 can also be used as an acid radical generator.
- the photoradical generator is a compound that has a function of generating radicals by directly absorbing light or being photosensitized to cause a decomposition reaction or a hydrogen abstraction reaction.
- the photo radical generator is preferably one having absorption in a wavelength region of 200 nm to 500 nm.
- Many compounds are known as such photo radical generators. For example, carbonyl compounds, ketal compounds, benzoin compounds, acridine compounds, organic peroxide compounds as described in JP-A-2008-268884 are known.
- Azo compounds, coumarin compounds, azide compounds, metallocene compounds, hexaarylbiimidazole compounds, organic boric acid compounds, disulfonic acid compounds, oxime ester compounds, and acylphosphine (oxide) compounds can be appropriately selected according to the purpose.
- benzophenone compounds, acetophenone compounds, hexaarylbiimidazole compounds, oxime ester compounds, and acylphosphine (oxide) compounds are particularly preferable from the viewpoint of exposure sensitivity.
- benzophenone compound examples include benzophenone, Michler's ketone, 2-methylbenzophenone, 3-methylbenzophenone, N, N-diethylaminobenzophenone, 4-methylbenzophenone, 2-chlorobenzophenone, 4-bromobenzophenone, 2-carboxybenzophenone, and the like. Can be mentioned. These may be used individually by 1 type and may use 2 or more types together.
- acetophenone compound examples include 2,2-dimethoxy-2-phenylacetophenone, 2,2-diethoxyacetophenone, 2- (dimethylamino) -2-[(4-methylphenyl) methyl] -1- [4- (4-morpholinyl) phenyl] -1-butanone, 1-hydroxycyclohexyl phenyl ketone, ⁇ -hydroxy-2-methylphenylpropanone, 1-hydroxy-1-methylethyl (p-isopropylphenyl) ketone, 1-hydroxy- 1- (p-dodecylphenyl) ketone, 2-methyl-1- (4-methylthiophenyl) -2-morpholinopropan-1-one, 1,1,1-trichloromethyl- (p-butylphenyl) ketone, 2-Benzyl-2-dimethylamino-1- (4-morpholinophenyl) -butanone 1, and the like. Specific examples of commercially available products are Irgacure
- Examples of the hexaarylbiimidazole compound include JP-B-6-29285, US Pat. No. 3,479,185, US Pat. No. 4,311,783, US Pat. No. 4,622,286, and the like.
- Examples of the oxime ester compound include JCSPerkin II (1979) 1653-1660), JCSPerkin II (1979) 156-162, Journal of Photopolymer Science and Technology (1995) 202-232, and JP 2000-66385 A. And the compounds described in JP-A No. 2000-80068 and JP-T No. 2004-534797. Specific examples include Irgacure OXE-01 and OXE-02 manufactured by BASF. These may be used individually by 1 type and may use 2 or more types together.
- acylphosphine (oxide) compound examples include Irgacure 819, Darocur 4265, and Darocur TPO manufactured by BASF.
- 2- (dimethylamino) -2-[(4-methylphenyl) methyl] -1- [4- (4-morpholinyl) phenyl] -1- is used from the viewpoint of exposure sensitivity and transparency.
- Butanone, 2-benzyl-2-dimethylamino-1- (4-morpholinophenyl) -butanone-1,2-methyl-1- (4-methylthiophenyl) -2-morpholinopropan-1-one, 2, 2′-bis (2-chlorophenyl) -4,4 ′, 5,5′-tetraphenylbiimidazole, N, N-diethylaminobenzophenone, Irgacure OXE-01] is particularly preferred.
- Component (II) photopolymerization initiators may be used alone or in combination of two or more.
- the content is preferably 0.1% by mass to 50% by mass, more preferably 0.5% by mass to 30% by mass based on the total mass of the solid content of the conductive composition, and 1% by mass More preferred is 20% by mass.
- 1% by mass More preferred is 20% by mass.
- the binder is a linear organic high molecular polymer having at least one alkali-soluble component in a molecule (preferably a molecule having an acrylic copolymer or a styrene copolymer as a main chain). It can be appropriately selected from alkali-soluble resins having a group to be promoted (for example, carboxyl group, phosphoric acid group, sulfonic acid group, etc.). Among these, those that are soluble in an organic solvent and soluble in an aqueous alkali solution are preferable, and those that have a dissociable group and become alkali-soluble when the dissociable group is dissociated by the action of a base are particularly preferable.
- the dissociable group represents a functional group that can be dissociated in the presence of a base.
- a known radical polymerization method For the production of the binder, for example, a known radical polymerization method can be applied. Polymerization conditions such as temperature, pressure, type and amount of radical initiator, type of solvent, etc. when producing an alkali-soluble resin by the radical polymerization method can be easily set by those skilled in the art, and experimental conditions are set. Can be determined.
- a polymer having a carboxylic acid in the side chain is preferable.
- the polymer having a carboxylic acid in the side chain include, for example, JP-A-59-44615, JP-B-54-34327, JP-B-58-12777, JP-B-54-25957, JP-A-59-53836, As described in JP-A-59-71048, methacrylic acid copolymer, acrylic acid copolymer, itaconic acid copolymer, crotonic acid copolymer, maleic acid copolymer, partial ester A maleic acid copolymer, etc., an acidic cellulose derivative having a carboxylic acid in the side chain, a polymer having a hydroxyl group with an acid anhydride added, and a polymer having a (meth) acryloyl group in the side chain Polymers are also preferred.
- benzyl (meth) acrylate / (meth) acrylic acid copolymers and multi-component copolymers composed of benzyl (meth) acrylate / (meth) acrylic acid / other monomers are particularly preferable.
- a high molecular polymer having a (meth) acryloyl group in the side chain and a multi-component copolymer composed of (meth) acrylic acid / glycidyl (meth) acrylate / other monomers are also useful.
- the polymer can be used by mixing in an arbitrary amount.
- 2-hydroxypropyl (meth) acrylate / polystyrene macromonomer / benzyl methacrylate / methacrylic acid copolymer 2-hydroxy-3-phenoxypropyl acrylate / polymethyl described in JP-A-7-140654 Methacrylate macromonomer / benzyl methacrylate / methacrylic acid copolymer, 2-hydroxyethyl methacrylate / polystyrene macromonomer / methyl methacrylate / methacrylic acid copolymer, 2-hydroxyethyl methacrylate / polystyrene macromonomer / benzyl methacrylate / methacrylic acid copolymer Coalescence, etc.
- (meth) acrylic acid and other monomers copolymerizable with the (meth) acrylic acid are suitable.
- Examples of other monomers copolymerizable with the (meth) acrylic acid include alkyl (meth) acrylates, aryl (meth) acrylates, and vinyl compounds. In these, the hydrogen atom of the alkyl group and aryl group may be substituted with a substituent.
- Examples of the alkyl (meth) acrylate or aryl (meth) acrylate include methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, butyl (meth) acrylate, isobutyl (meth) acrylate, and pentyl (meth).
- vinyl compound examples include styrene, ⁇ -methylstyrene, vinyl toluene, glycidyl methacrylate, acrylonitrile, vinyl acetate, N-vinyl pyrrolidone, tetrahydrofurfuryl methacrylate, polystyrene macromonomer, polymethyl methacrylate macromonomer, CH 2 ⁇ CR. 1 R 2 , CH 2 ⁇ C (R 1 ) (COOR 3 ) [wherein R 1 represents a hydrogen atom or an alkyl group having 1 to 5 carbon atoms, and R 2 represents an aromatic hydrocarbon ring having 6 to 10 carbon atoms. R 3 represents an alkyl group having 1 to 8 carbon atoms or an aralkyl group having 6 to 12 carbon atoms. ] And the like. These may be used individually by 1 type and may use 2 or more types together.
- the weight average molecular weight of the binder is preferably from 1,000 to 500,000, more preferably from 3,000 to 300,000, and even more preferably from 5,000 to 200,000, from the viewpoints of alkali dissolution rate, film physical properties and the like.
- the weight average molecular weight can be determined by a gel permeation chromatography method and obtained using a standard polystyrene calibration curve.
- the content of the component (III) binder is preferably 5% by mass to 90% by mass, more preferably 10% by mass to 85% by mass, based on the total mass of the solid content of the conductive composition. More preferred is from 80% by weight. When the content is within the preferable range, both developability and conductivity of the metal conductive fiber can be achieved.
- the matrix it is possible to use, as at least a part of the components constituting the matrix, a polymer compound as a dispersant used in the production of the metal conductive fibers described above.
- the photopolymerizable composition may contain other additives other than the components (I) to (III).
- Other additives include, for example, sensitizers, chain transfer agents, crosslinking agents, dispersants, solvents, surfactants, antioxidants, sulfurization inhibitors, metal corrosion inhibitors, viscosity modifiers, preservatives, etc. Various additives are mentioned.
- chain transfer agent is used for improving the exposure sensitivity of the photopolymerizable composition.
- chain transfer agents include N, N-dialkylaminobenzoic acid alkyl esters such as N, N-dimethylaminobenzoic acid ethyl ester, 2-mercaptobenzothiazole, 2-mercaptobenzoxazole, and 2-mercaptobenzoic acid.
- Aliphatic polyfunctional compounds such as mercapto compounds having a heterocyclic ring, pentaerythritol tetrakis (3-mercaptopropionate), pentaerythritol tetrakis (3-mercaptobutyrate), 1,4-bis (3-mercaptobutyryloxy) butane Examples include mercapto compounds. These may be used individually by 1 type and may use 2 or more types together.
- the content of the chain transfer agent is preferably 0.01% by mass to 15% by mass, preferably 0.1% by mass to 10% by mass based on the total mass of the solid content of the photopolymerizable composition containing the above-described metal conductive fibers. % By mass is more preferable, and 0.5% by mass to 5% by mass is still more preferable.
- crosslinking agent is a compound that forms a chemical bond with a free radical or acid and heat and cures the conductive layer.
- the crosslinking agent is at least one selected from a methylol group, an alkoxymethyl group, and an acyloxymethyl group.
- a compound having an ethylenically unsaturated group containing a methacryloyl group or an acryloyl group are particularly preferable in terms of film properties, heat resistance, and solvent resistance.
- the said oxetane resin can be used individually by 1 type or in mixture with an epoxy resin.
- the reactivity is high, which is preferable from the viewpoint of improving film properties.
- the said crosslinking agent is also included by said (I) polymeric compound,
- the content is (I) polymerization in this invention. It should be considered that it is included in the content of the active compound.
- the content of the crosslinking agent is preferably 1 part by weight to 250 parts by weight, and more preferably 3 parts by weight to 200 parts by weight, based on the total weight of the solid content of the photopolymerizable composition containing the above-described metal conductive fiber. .
- the dispersant is used to disperse the above-described metal conductive fibers in the photopolymerizable composition while preventing aggregation.
- the dispersant is not particularly limited as long as the metal conductive fibers can be dispersed, and can be appropriately selected according to the purpose.
- a commercially available dispersant can be used as a pigment dispersant, and a polymer dispersant having a property of adsorbing to metal conductive fibers is particularly preferable.
- polystyrene resin examples include polyvinyl pyrrolidone, BYK series (manufactured by Big Chemie), Solsperse series (manufactured by Nippon Lubrizol Co., Ltd.), and Ajisper series (manufactured by Ajinomoto Co., Inc.).
- the polymer dispersant when a polymer dispersant is added as a dispersant other than the one used for the production of the metal conductive fiber, the polymer dispersant is also included in the binder of the component (III), It should be considered that the content is included in the content of the component (III) described above.
- the content of the dispersant is preferably 0.1 part by weight to 50 parts by weight, more preferably 0.5 part by weight to 40 parts by weight, with respect to 100 parts by weight of the binder of component (III), and 1 part by weight to 30 parts by weight. Part by mass is particularly preferred.
- the content of the dispersant By setting the content of the dispersant to 0.1 parts by mass or more, aggregation of the metal conductive fibers in the dispersion is effectively suppressed, and by setting the content to 50 parts by mass or less, a stable liquid in the coating process. It is preferable because a film is formed and the occurrence of coating unevenness is suppressed.
- the solvent is a component used to form a coating solution for forming the photopolymerizable composition containing the above-described metal conductive fibers on the surface of the base material in a film form, depending on the purpose.
- PGME propylene glycol monomethyl ether
- PMEA propylene glycol monomethyl ether acetate
- methanol ethanol, 1-propanol, 2-propanol, butanol, 1-methoxy-2-propanol, 3 -Methoxybutanol, acetone, methyl ethyl ketone, methyl isobutyl ketone, cyclohexanone, methyl acetate, ethyl acetate, propyl acetate, isopropyl acetate, butyl acetate, ethyl 3-ethoxypropionate, methyl 3-methoxypropionate, ethyl lactate, ⁇ -butyrolactone, Carbon dioxide Pyrene, PGME),
- the conductive composition of the present invention further contains a compound capable of adsorbing to a metal or a compound capable of coordinating to a metal ion. May be. There is no restriction
- azole compounds (benzotriazole, 4-methylbenzotriazole, 5-methylbenzotriazole, 4-ethylbenzotriazole, 5,6-dimethylbenzobenzotriazole, tolyltriazole, benzyltriazole, 5,6-dimethylbenzimidazole, thiadiazole, Tetrazole, etc.), triazine compounds, ammonium compounds, phosphonium compounds, mercapto compounds (2-mercaptobenzoxazole, 2-mercaptobenzothiazole, 2-mercaptotetrazole, 2-mercaptopyrimidine, 2-mercaptobenzimidazole, dithiothiadiazole, alkyldithiothiadiazole And alkylthiols), sulfide compounds, disulfide compounds and the like are suitable.
- the method for adding the compound capable of adsorbing to the metal or the compound capable of coordinating to the metal ion can be selected from any method.
- the conductive layer after preparation may be immersed in a solution of a compound capable of adsorbing to a metal or a compound capable of coordinating to a metal ion.
- a preferable addition amount of the compound capable of adsorbing to the metal or the compound capable of coordinating to the metal ion is preferably 0.1% or more and 100% or less, more preferably 1% or more and 50% per mass of the metal conductive fiber. % Or less, particularly preferably 2% or more and 25% or less. By setting it to 0.1% or more and 100% or less, high conductivity is maintained while effectively preventing the occurrence of corrosion or rust of the metal conductive fibers.
- the conductive composition of the present invention preferably contains a solvent in order to form it on a desired substrate by coating.
- a solvent in order to form it on a desired substrate by coating.
- the component (b) described above is added to the aqueous dispersion. What is necessary is just to add and contain a compound.
- the component compound (b) is added in an amount of 0.005 mmol or more and 30 mmol or less per 1 g of the metal conductive fiber.
- a solvent for the coating liquid of the conductive composition a solvent different from the solvent (for example, water) used in the production of the metal conductive fiber, for example, an organic solvent such as propylene glycol monomethyl ether or propylene glycol monomethyl ether acetate is used.
- the solvent (for example, water) used in the production of the metal conductive fiber is subjected to solvent substitution that partially or completely replaces the desired solvent (for example, propylene glycol monomethyl ether acetate).
- the component compound (b) is added in an amount of 0.005 mmol or more and 30 mmol or less per 1 g of the metal conductive fiber.
- the coating liquid of the electrically conductive composition of this invention can be prepared.
- the solvent for such a coating solution include alcohols such as methanol, ethanol, 1-propanol, 2-propanol, butanol, 1-methoxy-2-propanol, and 3-methoxybutanol in addition to the solvents listed above.
- ketone solvents such as acetone, methyl ethyl ketone, methyl isobutyl ketone, cyclohexanone, methyl acetate, ethyl acetate, propyl acetate, isopropyl acetate, butyl acetate, ethyl 3-ethoxypropionate, methyl 3-methoxypropionate, ethyl lactate, ⁇ -Ester solvents such as butyrolactone and propylene carbonate, amide solvents such as N-methyl-2-pyrrolidinone and N-ethyl-2-pyrrolidinone, benzene solvents such as toluene and xylene, and mixed solvents thereof It is done.
- concentration of the metal electroconductive fiber in said coating liquid is suitably selected according to the thickness of the desired electroconductive layer from the range of 0.001 mass% or more and 50 mass% or less.
- the conductive composition of the present invention and the conductive member described later are, for example, a touch panel, a display electrode, an electromagnetic wave shield, an organic EL display electrode, an inorganic EL display electrode, an electronic paper, a flexible display electrode, and an integrated solar cell. It can be widely used for liquid crystal display devices, display devices with a touch panel function, and other various devices.
- the conductive member of the present invention has at least a conductive layer containing (a) a metal conductive fiber having an average minor axis length of 1 nm to 150 nm and (b) a component compound on a substrate.
- the conductive layer may be provided directly on the substrate, or may be provided on one or more other layers such as an undercoat layer, an intermediate layer, or a cushion layer provided on the substrate.
- other layers such as a surface protective layer (such as a soluble protective layer), a hard coat layer, an oxygen blocking layer, and an antistatic layer may be further provided on the conductive layer.
- an adhesive layer is previously provided on the substrate, and the conductive layer is formed of the conductive composition on the adhesive layer.
- An embodiment provided with a conductive layer is preferable.
- the shape, structure, size and the like are not particularly limited and can be appropriately selected according to the purpose.
- the shape, , Plate, film, and sheet examples include a single layer structure and a laminated structure.
- the substrate may be transparent or opaque. There is no restriction
- the transparent glass substrate examples include white plate glass, blue plate glass, and silica-coated blue plate glass. Further, a thin glass substrate having a thickness of 10 ⁇ m to several hundred ⁇ m developed recently may be used.
- synthetic resin sheets include polyethylene terephthalate (PET) sheets, polycarbonate sheets, triacetyl cellulose (TAC) sheets, polyethersulfone sheets, polyester sheets, acrylic resin sheets, vinyl chloride resin sheets, aromatic polyamide resin sheets, Examples thereof include a polyamideimide sheet and a polyimide sheet.
- the metal substrate examples include an aluminum plate, a copper plate, a nickel plate, and a stainless plate.
- the base material can be subjected to pretreatment such as chemical treatment such as a silane coupling agent, plasma treatment, ion plating, sputtering, gas phase reaction method, and vacuum deposition.
- chemical treatment such as a silane coupling agent, plasma treatment, ion plating, sputtering, gas phase reaction method, and vacuum deposition.
- the base material used in the present invention is applied to the conductive layer of the present invention, for the purpose of improving the adhesion of the functional layer and improving the wettability of the coating liquid, hydrophilic treatment, uneven treatment, etc. on one side or both sides It is preferable to perform the pretreatment.
- the pretreatment include corona discharge treatment, glow discharge treatment, plasma treatment, atmospheric pressure plasma treatment, flame treatment, hot air treatment, ozone / ultraviolet irradiation treatment, chromic acid treatment (wet), and saponification treatment (wet). Corona discharge treatment and plasma treatment (vacuum glow discharge and atmospheric pressure glow discharge treatment) are particularly preferred.
- Examples of the plasma treatment used in the present invention include vacuum glow discharge, atmospheric pressure glow discharge, and the like, and other methods include flame plasma treatment and the like.
- the methods described in, for example, JP-A-6-123062, JP-A-11-293011, and JP11-5857 can be used.
- the plasma treatment is a method in which a gas is plasma-excited by applying a high-frequency voltage to cause glow discharge between electrodes, and the surface of the substrate is modified by irradiating the substrate surface with a plasma-excited gas. is there.
- chlorofluorocarbons such as argon, helium, neon, krypton, xenon, nitrogen, carbon dioxide, tetrafluoromethane, and mixtures thereof are preferable, and inert gases such as argon and neon are preferable.
- a reactive gas capable of imparting a polar functional group such as a carboxyl group, a hydroxyl group or a carbonyl group to the surface of the plastic film.
- oxygen, nitrogen, and other gases such as water vapor and ammonia
- low-boiling organic compounds such as lower hydrocarbons and ketones can be used as the reactive gas if necessary.
- Gases such as oxygen, carbon dioxide, nitrogen and water vapor are preferred.
- a gas obtained by bubbling other gas through water can be used.
- water vapor may be mixed.
- the frequency of the applied high frequency voltage is preferably 1 kHz to 100 kHz, more preferably 1 kHz to 40 kHz.
- an inert gas such as helium or argon
- an inert gas is not necessarily required, and the reactive gas concentration can be increased and the reaction rate can be increased.
- Corona discharge treatment can be performed by any conventionally known method, for example, Japanese Patent Publication Nos. 48-5043, 47-51905, Japanese Patent Publication Nos. 47-28067, 49-83767, and 51-41770. Can be achieved by the method disclosed in JP-A-51-131576.
- Various commercially available corona treatment machines can be used as the treatment machine.
- a corona treatment machine having a multi-knife electrode manufactured by SOFTAL (Sophthal) is composed of a large number of electrodes, and the film is heated by sending air between the electrodes. This is useful because it can prevent or remove small molecules from the film surface.
- a dielectric covering electrode In order to avoid the spark between an electrode and a conductive layer with respect to the surface which has not provided the conductive layer of the base material which provided the conductive layer on one side, as a discharge electrode, it is a dielectric covering electrode. (Ceramic electrode, quartz electrode, etc.) is preferably subjected to corona treatment using a metal roll such as stainless steel as the counter electrode.
- the corona treatment conditions vary depending on the type of substrate used, the type of coating matrix, the type of corona treatment machine used, and the like, but the corona surface treatment has an irradiation energy of 0.1 J / m 2 or more and 10 J / m. It is preferably carried out in m 2 or less in the range, 0.5 J / m 2 or more 5 J / m 2 or less is more preferable.
- the contact angle of the substrate surface with water is preferably 0 ° to 40 °, more preferably 0 ° to 20 °, and still more preferably. It is in the range of 0 ° to 10 °.
- the average thickness of the substrate is not particularly limited and can be appropriately selected depending on the purpose. In general, it is preferably selected from the range of 1 ⁇ m to 500 ⁇ m, more preferably 3 ⁇ m to 400 ⁇ m, and particularly preferably 5 ⁇ m to 300 ⁇ m.
- the average thickness of the substrate is 1 ⁇ m or more, the handling of the conductive member becomes easy, and when it is 500 ⁇ m or less, the flexibility of the substrate becomes appropriate, the handling is easy, and the transfer mold Even when used as a conductive member, it is easy to ensure transfer uniformity.
- the total visible light transmittance of the substrate is preferably 70% or more, more preferably 85% or more, and particularly preferably 90% or more.
- the base material that has been colored to the extent that does not interfere with the object of the present invention can also be used.
- the conductive layer according to the present invention contains at least (a) a metal conductive fiber having an average minor axis length of 1 nm to 150 nm and (b) a component compound.
- the average thickness of the conductive layer of the present invention is preferably 0.01 ⁇ m to 2 ⁇ m, more preferably 0.02 ⁇ m to 1 ⁇ m, still more preferably 0.03 ⁇ m to 0.8 ⁇ m, and particularly preferably 0.05 ⁇ m to 0.5 ⁇ m.
- the average thickness of the conductive layer is 0.01 ⁇ m or more, it becomes easy to achieve sufficient durability and film strength, and the in-plane distribution of conductivity becomes uniform. Further, by setting the average thickness of the conductive layer to 2 ⁇ m or less, a material having high transmittance and transparency can be easily obtained.
- the method for forming the conductive layer on the substrate can be performed by a general coating method using the above-described conductive composition coating liquid, and is not particularly limited and is appropriately selected depending on the purpose. For example, roll coating method, bar coating method, dip coating method, spin coating method, casting method, die coating method, blade coating method, gravure coating method, curtain coating method, spray coating method, doctor coating method, etc. It is done.
- the (a) metal conductive fiber and the (b) component compound may be added to different layers, in which case (a) the metal conductive fiber and ( b) It is not necessary to use the electroconductive composition of this invention containing a component compound.
- the ratio of the metal conductive fibers described above is preferably 50% or more, more preferably 60% or more, and particularly preferably 75% or more in volume ratio in the conductive layer.
- the ratio of these metal conductive fibers may be referred to as “the ratio of metal conductive fibers”.
- the ratio of the metal conductive fibers By setting the ratio of the metal conductive fibers to 50% or more, it becomes easy to ensure sufficient conductivity and to make the durability good. Further, particles having a shape other than the metal conductive fiber are not preferable because they do not greatly contribute to conductivity and have absorption. In particular, when the particles other than the metal conductive fibers are metal and the plasmon absorption such as a spherical shape is strong, the transparency may be deteriorated.
- the ratio of the metal conductive fiber is, for example, when the metal conductive fiber is a silver nanowire, the silver nanowire aqueous dispersion is filtered, and the silver nanowire and other particles are filtered.
- the ratio of metal conductive fibers can be determined by measuring the amount of silver remaining on the filter paper and the amount of conductive material that has passed through the filter paper using an ICP emission analyzer. This is detected by observing the metal conductive fibers remaining on the filter paper with a TEM, observing the average minor axis length of 300 metal conductive fibers, and examining their distribution. The method for measuring the average minor axis length and the average major axis length of the metal conductive fiber is as described above.
- the conductive member of the present invention preferably has a soluble protective layer containing at least a water-soluble polymer on the conductive layer.
- the soluble protective layer contains a water-soluble polymer, and further contains other components as necessary.
- the availability protection layer of the present invention may contain the component compound (b) according to the present invention.
- the water-soluble polymer is not particularly limited and may be appropriately selected depending on the intended purpose.
- polyvinyl pyrrolidone, polyvinyl alcohol, and water-soluble cellulose derivatives are particularly preferable.
- the polyvinyl pyrrolidone may be a copolymer having a polymer unit other than the vinyl pyrrolidone unit. Examples of such a copolymer include a vinyl pyrrolidone / vinyl acetic acid copolymer.
- the polyvinyl alcohol may be a copolymer having a polymer unit other than the vinyl alcohol unit. Examples of such a copolymer include a vinyl alcohol / vinyl pyrrolidone copolymer.
- the water-soluble cellulose derivative include carboxymethylcellulose, hydroxyethylcellulose, hydroxypropylmethylcellulose and the like.
- Examples of the polyalkylene glycol include polyethylene glycol and ethylene glycol / propylene glycol copolymer, and polyalkylene glycol having a weight average molecular weight of 5,000 to 100,000 is preferable.
- the other components are not particularly limited and may be appropriately selected depending on the intended purpose.
- fillers for example, fillers, surfactants, antioxidants, sulfurization inhibitors, metal corrosion inhibitors, viscosity modifiers, preservatives And various other additives.
- the average thickness of the soluble protective layer is preferably 0.1 ⁇ m to 5 ⁇ m, more preferably 0.2 ⁇ m to 2 ⁇ m, and still more preferably 0.5 ⁇ m to 1 ⁇ m.
- the average thickness is 0.1 ⁇ m or more, an effect of improving scratch resistance is easily obtained.
- the average thickness is 5 ⁇ m or less, the removal time of the soluble protective layer is easily shortened, and the remaining of the soluble protective layer is easily suppressed.
- it is 5 micrometers or less it is suppressed that the binder of a protective layer mixes in a conductive fiber content layer, and the density of a conductive fiber falls, and it exists in the tendency for a conductive fall to be suppressed.
- the average thickness of the soluble protective layer can be measured, for example, by observing the cross section of the protective layer with a scanning electron microscope (SEM).
- the soluble protective layer can be formed by applying a composition for a soluble protective layer containing at least a water-soluble polymer on the conductive layer.
- the composition for a soluble protective layer contains at least the aforementioned water-soluble polymer, and contains a solvent and, if necessary, other components.
- the solvent is not particularly limited and may be appropriately selected depending on the purpose.
- the coating method is not particularly limited and may be appropriately selected depending on the purpose.
- the printing method include letterpress (letterpress) printing, stencil (screen) printing, lithographic (offset) printing, and intaglio (gravure) printing.
- the soluble protective layer may be removed by applying a solvent.
- the removal of the soluble protective layer may be performed during pattern formation of the conductive layer, or may be performed together with pattern formation on the user side.
- the solvent used for removing the soluble protective layer is preferably either water or an alkaline solution.
- water there is no restriction
- the alkali contained in the alkaline solution is not particularly limited and may be appropriately selected depending on the intended purpose.
- Examples thereof include tetramethylammonium hydroxide, tetraethylammonium hydroxide, 2-hydroxyethyltrimethylammonium hydroxide, sodium carbonate, Examples thereof include sodium hydrogen carbonate, potassium carbonate, potassium hydrogen carbonate, sodium hydroxide, potassium hydroxide and the like.
- the immersion time of the water and alkaline solution is not particularly limited and can be appropriately selected depending on the purpose, but is preferably 10 seconds to 5 minutes.
- the conductive member according to the present invention is preferably adjusted so that the surface resistance is 1 ⁇ / ⁇ or more and 1000 ⁇ / ⁇ or less.
- the surface resistance of the conductive member according to the present invention is more preferably in the range of 1 ⁇ / ⁇ to 500 ⁇ / ⁇ , particularly preferably in the range of 1 ⁇ / ⁇ to 250 ⁇ / ⁇ , and 1 ⁇ / ⁇ to 200 ⁇ / ⁇ .
- the range of ⁇ is most preferable.
- the surface resistance is a value measured by a four-probe method on the surface of the conductive member according to the present invention on the side opposite to the base material side.
- the surface resistance measurement method by the four-probe method can be measured in accordance with, for example, JIS K 7194: 1994 (resistivity test method by the four-probe method for conductive plastics), and a commercially available surface resistivity meter. Can be easily measured.
- Resistivity test method by the four-probe method for conductive plastics can be easily measured.
- at least one of the kind and content ratio of the metal conductive fibers contained in the conductive layer may be adjusted. More specifically, for example, a conductive layer having a surface resistance in a desired range can be formed by adjusting the content ratio of the matrix and the metal conductive fiber.
- the conductive member according to the present invention preferably has a total light transmittance of 70% or more, more preferably 85% or more, and particularly preferably 90% or more.
- the conductive member according to the present invention preferably has a haze of 10% or less, more preferably 5% or less, and particularly preferably 2% or less.
- a first preferred embodiment of the present invention is a conductive member in which a conductive layer containing metal conductive fibers is provided on a base material, and when the conductive layer is observed from a direction perpendicular to the base material surface, This is an embodiment in which the entire region is a conductive region (hereinafter, this conductive layer is also referred to as “non-patterned conductive layer”).
- the electroconductive member which concerns on a 1st aspect can be preferably used for the transparent electrode of a solar cell, an electromagnetic wave shielding material, an antistatic material etc., for example.
- a second preferred embodiment of the present invention is a conductive member in which a conductive layer containing metal conductive fibers is provided on a substrate, and the conductive layer includes a conductive region and a non-conductive region (hereinafter referred to as a conductive layer).
- This conductive layer is also referred to as a “patterned conductive layer”).
- the non-conductive region may or may not contain metal conductive fibers. When the metal conductive fiber is included in the non-conductive region, the metal conductive fiber included in the non-conductive region is disconnected or the contact resistance between the metal conductive fibers is extremely high. It becomes non-conductive.
- the electroconductive member which concerns on a 2nd preferable aspect is used, for example when producing a touch panel and wiring material.
- a conductive region and a non-conductive region having a desired shape are formed, and examples thereof include an electrode shape applied with an existing ITO transparent conductive film.
- a third preferred embodiment of the present invention is a conductive member in which at least a cushion layer and a conductive layer containing metal conductive fibers are provided in this order on a first base material, the conductive layer being A conductive member that is transferred onto a second base material for use.
- the base material is peeled after the conductive member is transferred to the transfer target, and the cushion layer and the conductive layer are transferred to the transfer target.
- the entire region of the conductive layer may be conductive (non-patterned conductive layer) or a patterned conductive layer having a conductive region and a non-conductive region.
- the preferred use in the case of the non-patterned conductive layer is the same as the first preferred embodiment of the present invention, and the preferred use and shape in the case of the patterned conductive layer are the same as those in the first aspect of the present invention. This is the same as the two preferred embodiments.
- the 1st preferable aspect of this invention and the 2nd preferable aspect are the electroconductive members which provided the electroconductive layer containing a metal electroconductive fiber on a base material, From the above-mentioned base material and an electroconductive layer, Any combination can be selected according to the purpose.
- the above-described sol-gel cured product is preferably used as the matrix of the conductive layer.
- the patterned conductive layer according to the second preferred embodiment of the present invention is produced, for example, by the following patterning method.
- a non-patterned conductive layer is formed in advance, and a high-energy laser beam such as a carbon dioxide laser or a YAG laser is irradiated to the metal conductive fiber contained in a desired region of the non-patterned conductive layer. Then, a patterning method in which a part of the metal conductive fiber is disconnected or disappeared to make the desired region a non-conductive region. This method is described in, for example, Japanese Patent Application Laid-Open No. 2010-496.
- a negative-type or positive-type photoresist layer is provided on a previously formed non-patterned conductive layer, and a desired pattern exposure and development are performed on this photoresist layer to form the patterned cured resist layer.
- the metal conduction in the conductive layer in areas that are not protected by the hardened resist layer either by a wet process where the metal conductive fibers are treated with an etchable etchant or by a dry process such as reactive ion etching. Patterning method for etching away conductive fibers. This method is described, for example, in JP-T-2010-507199 (particularly, paragraphs 0212 to 0217).
- a patterned photoresist layer is formed on a non-patterned conductive layer formed in advance, and the photoresist layer is subjected to desired exposure and development as necessary to form a patterned cured resist layer.
- a metal conductive fiber in a conductive layer in a region not protected by a cured resist layer by a wet process in which the metal conductive fiber is treated with an etchable etchant or by a dry process such as reactive ion etching.
- a patterning method for removing the etching is provided.
- a pre-formed non-patterned conductive layer is provided with a photo-etching layer containing a compound that can be made non-conductive by reacting with metal conductive fibers by exposure to a pattern, and the photo-etched layer has a desired exposure.
- the patterning method is characterized in that the metal conductive fiber in the region irradiated with light is insulated by oxidation, disconnection or the like.
- the methods (1), (2), (4) and (5) are performed when the conductive layer is composed of metal conductive fibers alone, and when the metal conductive fibers and the non-photosensitive matrix are used. Is a convenient patterning method.
- the light source used for the exposure described in (2), (3), (4) and (5) is selected in relation to the photosensitive wavelength range of the photoresist composition. Ultraviolet rays such as h-line, i-line, and j-line are preferably used. A blue LED may be used.
- the pattern exposure method is not particularly limited, and may be performed by surface exposure using a photomask, or may be performed by scanning exposure using a laser beam or the like. At this time, refractive exposure using a lens or reflection exposure using a reflecting mirror may be used, and exposure methods such as contact exposure, proximity exposure, reduced projection exposure, and reflection projection exposure can be used.
- the resist used for the photoresist layer is arbitrarily selected from a negative type and a positive type.
- the negative resist examples include a photopolymerization initiator and a photocuring material (monofunctional or polyfunctional monomer, oligomer, or crosslinkable group-containing polymer), a binder, a filler, a sensitizer, a polymerization inhibitor, a dye, Additives such as pigments, surfactants, thickeners, leveling agents, crosslinking agents, adhesion improvers, solvents and the like can optionally be included.
- a photopolymerization initiator known compounds and mixtures thereof can be appropriately selected and used as a photoinitiator for photoradical polymerization.
- the type of the photopolymerization initiator is not particularly limited, and examples thereof include alkylphenone compounds (for example, benzyldimethyl ketal compound, ⁇ -hydroxyalkylphenone compound, ⁇ -aminoalkylphenone compound, etc.), oxime compounds (for example, Oxime ester compounds) and the like can be used. Moreover, a photoinitiator may be used independently or may be used in combination of 2 or more type.
- alkylphenone compounds for example, benzyldimethyl ketal compound, ⁇ -hydroxyalkylphenone compound, ⁇ -aminoalkylphenone compound, etc.
- oxime compounds for example, Oxime ester compounds
- a photoinitiator may be used independently or may be used in combination of 2 or more type.
- Positive resists include, for example, photoacid generators and curing agents, binders, fillers, sensitizers, polymerization inhibitors, dyes, pigments, surfactants, thickeners, leveling agents, crosslinking agents, and adhesion improvers. Additives such as agents and solvents can optionally be included.
- the coating method is not particularly limited.
- a roll coating method, a bar coating method, a dip coating method, a spin coating method, a casting method, a die coating method, a blade coating method, a bar coating method, a gravure coating method, a curtain coating method examples thereof include a spray coating method and a doctor coating method.
- the printing method include letterpress (letterpress) printing, stencil (screen) printing, lithographic (offset) printing, and intaglio (gravure) printing.
- the solution for dissolving the metal conductive fiber can be appropriately selected according to the metal conductive fiber.
- the metal conductive fibers are silver nanowires
- bleach-fixing solutions strong acids, oxidizing agents, peroxides used mainly in the bleach-fixing process of photographic papers of silver halide color light-sensitive materials
- Examples include hydrogen.
- bleach-fixing solution, diluted nitric acid, and hydrogen peroxide are more preferable, and bleach-fixing solution and diluted nitric acid are particularly preferable.
- the dissolution of the silver nanowires with the solution for dissolving the metal conductive fibers may not completely dissolve the portion of the silver nanowires to which the solution is applied, and partly if the conductivity is lost. May remain.
- the concentration of the diluted nitric acid is preferably 1% by mass to 20% by mass.
- the concentration of the hydrogen peroxide is preferably 3% by mass to 30% by mass.
- Examples of the bleach-fixing solution include, for example, page 26, lower right column, line 1 to page 34, upper right column, line 9 of JP-A-2-207250, and page 5, upper-left column, line 17 of JP-A-4-97355.
- the processing materials and processing methods described in the 20th page, lower right column, line 20 can be preferably applied.
- the bleach-fixing time is preferably 180 seconds or shorter, more preferably 120 seconds or shorter and 1 second or longer, and further preferably 90 seconds or shorter and 5 seconds or longer.
- the washing time or the stabilization time is preferably 180 seconds or shorter, more preferably 120 seconds or shorter and 1 second or longer.
- the bleach-fixing solution is not particularly limited as long as it is a photographic bleach-fixing solution, and can be appropriately selected according to the purpose.
- CP-48S, CP-49E color paper bleaching manufactured by FUJIFILM Corporation. Fixing agent), Kodak Ektacolor RA bleach-fixing solution, Dai Nippon Printing Co., Ltd. bleach-fixing solution D-J2P-02-P2, D-30P2R-01, D-22P2R-01, and the like.
- CP-48S and CP-49E are particularly preferable.
- the viscosity of the solution for dissolving the metal conductive fibers is preferably 5 mPa ⁇ s to 300,000 mPa ⁇ s at 25 ° C., more preferably 10 mPa ⁇ s to 150,000 mPa ⁇ s.
- the viscosity is preferably 5 mPa ⁇ s to 300,000 mPa ⁇ s at 25 ° C., more preferably 10 mPa ⁇ s to 150,000 mPa ⁇ s.
- the application of the pattern of the solution for dissolving the metal conductive fibers is not particularly limited as long as the solution can be applied in a pattern, and can be appropriately selected according to the purpose.
- screen printing, inkjet printing Examples thereof include a method in which an etching mask is formed with a resist agent or the like, and a solution is coated thereon by coater coating, roller coating, dipping coating or spray coating.
- screen printing, ink jet printing, coater coating, and dip coating are particularly preferable.
- the ink jet printing for example, both a piezo method and a thermal method can be used.
- etching agent that generates an etching chemical species such as a photo radical generator
- the etching agent described in (5) can be removed by any method after exposure.
- the photoradical generator is a compound having a function of generating radicals by directly absorbing light or being photosensitized to cause a decomposition reaction or a hydrogen abstraction reaction.
- the photopolymerization initiator preferably has an absorption in a wavelength range of 200 nm to 900 nm, preferably 200 nm to 600 nm, more preferably 250 nm to 500 nm, and particularly preferably 300 nm to 500 nm.
- photo radical generators A large number of compounds are known as such photo radical generators.
- carbonyl compounds, acetal compounds, benzoin compounds, acridine compounds, organic peroxide compounds as described in JP-A-2008-268884 are disclosed.
- Azo compounds, coumarin compounds, azide compounds, metallocene compounds, hexaarylbiimidazole compounds, organic boric acid compounds, disulfonic acid compounds, oxime ester compounds, and acylphosphine (oxide) compounds These can be appropriately selected according to the purpose.
- the photo radical generator may be used alone, or appropriately diluted with a solvent, added with a polymer, a thickening agent, or inorganic fine particles to impart coating suitability, inkjet discharge suitability, screen printing suitability, or improve visibility. Therefore, it may be colored by adding a pigment or a dye.
- middle layer About the 1st preferable aspect of this invention, and a 2nd preferable aspect, it is preferable to have an intermediate
- the intermediate layer includes an adhesive layer for improving the adhesive force between the base material and the conductive layer, and a functional layer for improving functionality by interaction with components contained in the conductive layer. Depending on the situation, it is appropriately provided.
- the component used in the intermediate layer is not particularly limited as long as it improves at least one of the above characteristics.
- an intermediate layer in contact with the conductive layer (that is, if the intermediate layer is a single layer, the intermediate layer, and if the intermediate layer includes a plurality of layers, an intermediate layer in contact with the conductive layer) Is a functional layer containing a compound having a functional group capable of interacting with the metal conductive fibers contained in the conductive layer, a conductive layer excellent in total light transmittance, haze, and film strength. Since it is obtained, it is preferable. In the case of having such an intermediate layer, even if the conductive layer contains metal conductive fibers and a matrix, a conductive layer having excellent film strength can be obtained.
- the metal conductive fiber and the intermediate layer contained in the conductive layer are provided.
- the interaction with the compound having the above functional group contained in the above the aggregation of the conductive material in the conductive layer is suppressed, the uniform dispersibility is improved, and the transparency resulting from the aggregation of the conductive material in the conductive layer It is considered that the improvement of the film strength is achieved due to the adhesiveness while the deterioration of the property and haze is suppressed.
- the intermediate layer capable of exhibiting such interaction may be referred to as a functional layer.
- the functional group capable of interacting with the metal conductive fiber for example, when the metal conductive fiber is a silver nanowire, an amide group, an amino group, a mercapto group, a carboxylic acid group, a sulfonic acid group, a phosphoric acid group More preferably at least one selected from the group consisting of phosphonic acid groups or salts thereof.
- An amino group, a mercapto group, a phosphoric acid group, a phosphonic acid group or a salt thereof is more preferable, and an amino group is most preferable.
- Examples of the compound having a functional group as described above include compounds having an amide group such as ureidopropyltriethoxysilane, polyacrylamide, poly (N-methylacrylamide) and the like, for example, N- ⁇ (aminoethyl) ⁇ -amino.
- an amide group such as ureidopropyltriethoxysilane, polyacrylamide, poly (N-methylacrylamide) and the like, for example, N- ⁇ (aminoethyl) ⁇ -amino.
- the metal conductive fibers interact with the functional groups contained in the intermediate layer, and the metal conductive fibers are dried when drying. Can be suppressed, and a conductive layer in which metal conductive fibers are uniformly dispersed can be formed.
- the intermediate layer can be formed by applying a solution in which the compound constituting the intermediate layer is dissolved, dispersed, or emulsified on a substrate and drying, and the application method may be a general method. it can.
- the method is not particularly limited and can be appropriately selected depending on the purpose. For example, roll coating method, bar coating method, dip coating method, spin coating method, casting method, die coating method, blade coating method, gravure coating method. , Curtain coating method, spray coating method, doctor coating method, and the like.
- FIG. 1 and FIG. 2 are schematic cross-sectional views showing conductive members (1) and (2) according to a first preferred embodiment and a second preferred embodiment of the present invention, respectively.
- FIG. 1 between the base material 10 and the electroconductive layer 20, the 1st contact bonding layer 31 excellent in affinity with the base material 10, and the 2nd adhesion excellent in affinity with the electroconductive layer 20 are shown.
- An intermediate layer 30 including a layer 32 is provided between the base material 10 and the electroconductive layer 20 .
- the conductive layer 20 is adjacent between the substrate 10 and the conductive layer 20.
- the intermediate layer 30 having the functional layer 33 is provided.
- the intermediate layer 30 in this specification refers to a layer including at least one layer selected from the first adhesive layer 31, the second adhesive layer 32, and the functional layer 33.
- FIGS. 3 and 4 are schematic cross-sectional views showing a third preferred embodiment of the present invention and conductive members (3) and (4) according to modifications of the third preferred embodiment.
- the conductive member (3) of FIG. 3 has the base material 1 and the cushion layer 2 and the conductive layer 3 in this order on one surface of the base material 1.
- the conductive member (4) in FIG. 4 is obtained by providing the adhesive layer 4 on the conductive layer 3 in the conductive member (3) in FIG.
- the conductive member 3 according to the third preferred embodiment of the present invention will be described in detail.
- the conductive member 3 has a cushion layer 2 and a conductive layer 3 containing metal conductive fibers in this order on the base material 1, and further has other layers as necessary. It becomes.
- the average thickness of the cushion layer 2 is 1 ⁇ m to 50 ⁇ m, preferably 5 ⁇ m to 20 ⁇ m.
- the average thickness of the cushion layer 2 is 1 ⁇ m or more, the transfer uniformity and the unevenness followability tend to be excellent, and when it is 50 ⁇ m or less, the curl balance of the conductive member 3 tends to be excellent.
- the shape, structure, size, and the like are not particularly limited and can be appropriately selected depending on the purpose.
- the structure may be a single layer structure, a laminated structure, or the like, and the size may be appropriately selected according to the application.
- the conductive member is flexible and preferably transparent, and the “transparent” includes colorless and transparent, colored transparent, translucent, colored translucent, and the like.
- the cushion layer has a cushion layer.
- an electroconductive layer straddles the unevenness
- the structure include a single layer structure and a laminated structure. The size can be appropriately selected according to the application.
- the cushion layer is a layer that plays a role of improving transferability with the transfer target, and contains at least a polymer, and further contains other components as necessary.
- the polymer contained in the cushion layer is not particularly limited as long as it is a polymer that softens when heated, and can be appropriately selected according to the purpose.
- examples thereof include thermoplastic resins.
- the thermoplastic resin include acrylic resin, styrene-acrylic copolymer, polyvinyl alcohol, polyethylene, ethylene-vinyl acetate copolymer, ethylene-ethyl acrylate copolymer, ethylene-methacrylic acid copolymer, polychlorinated resin.
- Vinyl gelatin such as cellulose nitrate, cellulose triacetate, cellulose diacetate, cellulose acetate butyrate, cellulose acetate propionate; vinylidene chloride, vinyl chloride, styrene, acrylonitrile, vinyl acetate, alkyl (1 to 4 carbon atoms)
- cellulose esters such as cellulose nitrate, cellulose triacetate, cellulose diacetate, cellulose acetate butyrate, cellulose acetate propionate
- vinylidene chloride vinyl chloride, styrene, acrylonitrile, vinyl acetate, alkyl (1 to 4 carbon atoms
- Examples include homopolymers or copolymers containing acrylate, vinyl pyrrolidone, etc., soluble polyesters, polycarbonates, soluble polyamides, and the like. These may be used individually by 1 type and may use 2 or more types together.
- the glass transition temperature of the cushion layer is preferably 40 ° C. to 150 ° C., more preferably 90 ° C. to 120 ° C.
- the glass transition temperature is 40 ° C. or higher, it is suppressed that the handling property is lowered due to being too soft at room temperature.
- the glass transition temperature is 150 ° C. or lower, the cushion layer is not softened by the heat laminating method and the conductive layer is transferred. It is possible to suppress a decrease in performance.
- the glass transition temperature may be adjusted by adding a plasticizer or the like.
- Examples of the other components include organic polymer substances described in paragraph [0001] and thereafter of JP-A-5-72724, various plasticizers for adjusting the adhesive force with the base material, supercooling substances, adhesion Examples include improvers, fillers, antioxidants, surfactants, mold release agents, thermal polymerization inhibitors, viscosity modifiers, and solvents.
- the said cushion layer can be formed by apply
- the coating method is not particularly limited and may be appropriately selected depending on the intended purpose. For example, roll coating method, bar coating method, dip coating method, spin coating method, casting method, die coating method, blade coating method, gravure Examples thereof include a coating method, a curtain coating method, a spray coating method, and a doctor coating method.
- the conductive member according to the present invention is excellent in conductivity and transparency even when exposed to harsh conditions such as high temperature, high humidity conditions or presence of ozone, and has a low surface resistance.
- a touch panel a display electrode
- It is widely applied to electromagnetic shielding, organic EL display electrodes, inorganic EL display electrodes, electronic paper, flexible display electrodes, integrated solar cells, liquid crystal display devices, display devices with touch panel functions, and other various devices.
- application to a touch panel is particularly preferable.
- a conductive layer containing at least (a) a metal conductive fiber having an average minor axis length of 1 nm to 150 nm and (b) a component compound is formed on a substrate.
- suitable production methods include the following two methods (1) and (2).
- the following method (1) can include the following two production methods. In any of the following methods (1-1), (1-2) and (2), the metal conductive fiber as the component (a), the component compound (b) and the matrix as the component (c) are used. A conductive layer is formed.
- a conductive layer is formed using the conductive composition containing (a) a metal conductive fiber having an average minor axis length of 1 nm to 150 nm and (b) a component compound.
- a conductive composition containing (a) a metal conductive fiber having an average minor axis length of 1 nm or more and 150 nm or less, (b) a component compound, and (c) a matrix is provided on the substrate, A conductive layer containing the component (a), the component (b) and the component (c) is formed.
- the component compound (b) is added to the conductive layer containing the metal conductive fiber, and even when added to the layer in contact with the conductive layer, the effect can be exhibited. is there. Therefore, as the method for adding the component compound (b) to the conductive layer, the following three methods can be mentioned.
- the component compound (b) is added to the conductive composition.
- a layer containing metal conductive fibers is formed on the substrate in advance, and this layer is immersed in a solution containing the component compound (b).
- the component compound (b) is added in advance to another layer other than the conductive layer, and introduced and diffused from the separate layer to the conductive layer when the conductive layer is applied and dried.
- the method (1) or (2) is more preferable, and the method (1) is more preferable.
- FIGS. 5 to 8 are diagrams for explaining an example of the method for producing a conductive member of the present invention.
- the conductive layer contains the component (a), the component (b), and the component (c).
- FIG. 6 On the base material, a conductive composition containing (a) component: metal conductive fiber 40 and (b) component compound 50 is applied (FIG. 6 (A)). c) Component: A liquid containing a polymerizable compound 60 capable of forming a matrix is applied (FIG. 6B). This method is effective when the component compound (b) is difficult to dissolve in the liquid containing the polymerizable compound 60 capable of forming the component (c): matrix.
- FIG. 7 Component (a): metal conductive fiber 40 is applied on a base material (FIG. 7 (A)), where (b) component compound 50 and (c) component: matrix are added. A liquid containing a polymerizable compound 60 that can be formed is applied (FIG. 7B). This method is excellent in that the contact resistance between the metal conductive fibers can be lowered.
- FIG. 8 A first layer is formed on a base material by applying a liquid containing (a) component: metal conductive fiber 40 and (c) component: polymerizable compound 60 capable of forming a matrix.
- a second layer containing (b) the component compound 50 is formed on the second layer (FIG. 8 (B)).
- the component compound 50 is diffused (FIG. 8C).
- the separate layer is a layer in contact with the first layer on the surface side far from the substrate 10, but may be a layer in contact with the first layer on the surface side close to the substrate 10.
- the conductive member according to the present invention is applied to, for example, a surface capacitive touch panel, a projection capacitive touch panel, a resistive touch panel, and the like.
- the touch panel includes a so-called touch sensor and a touch pad.
- the layer structure of the touch panel sensor electrode part in the touch panel is a bonding method in which two transparent electrodes are bonded, a method in which transparent electrodes are provided on both surfaces of a single substrate, a single-sided jumper or a through-hole method, or a single-area layer method. It is preferable that it is either.
- the surface capacitive touch panel is described in, for example, JP-T-2007-533044.
- the conductive member according to the present invention is also useful as a transparent electrode in an integrated solar cell (hereinafter sometimes referred to as a solar cell device).
- a solar cell device There is no restriction
- 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 or the like, amorphous silicon, a microcrystalline silicon thin film layer, a thin film containing Ge (germanium), and further, a tandem structure of these two or more layers Used as a photoelectric conversion layer.
- plasma CVD or the like is used for film formation.
- the conductive member according to the present invention can be applied to all the solar cell devices.
- the conductive member may be included in any part of the solar cell device, but it is preferable that the conductive layer is disposed 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.
- the configuration surrounded by [] corresponds to the conductive member according to the present invention.
- TEM transmission electron microscope
- a silver nanowire dispersion liquid (1) was prepared as follows. 1.30 g of stearyltrimethylammonium bromide powder, 33.1 g of sodium bromide powder, 1,000 g of glucose powder and 115.0 g of nitric acid (1N) were dissolved in 12.7 kg of distilled water at 80 ° C. While maintaining this liquid at 80 ° C. and stirring at 500 rpm, 100 g of the additive liquid A was sequentially added at an addition rate of 250 ml / min, additive liquid B at 500 ml / min, and additive liquid C at 500 ml / min. After the addition, the stirring speed was 200 rpm, and the heating and stirring was continued at 80 ° C. for 100 minutes, followed by cooling to 25 ° C. Subsequently, the stirring speed was changed to 500 rpm, and the additive liquid D was added at 500 ml / min. The obtained liquid was used as the charged liquid 101.
- the charged solution 101 was added at once so that the mixing ratio was 1: 1.
- the obtained mixed solution was stirred for 3 minutes to obtain a charged solution 102.
- ultrafiltration was performed as follows. After the feed liquid 102 is concentrated four times, the addition and concentration of a mixed solution of distilled water and 1-propanol (volume ratio of 1: 1) is repeated until the conductivity of the filtrate finally becomes 50 ⁇ S / cm or less. It was.
- the obtained filtrate was concentrated to obtain a silver nanowire dispersion liquid (1) having a metal content of 0.48%.
- the average minor axis length, the average major axis length, the coefficient of variation of the minor axis length of the silver nanowire, and the average aspect ratio were measured as described above.
- the average minor axis length was 20.1 nm
- the average major axis length was 10.5 ⁇ m
- the coefficient of variation was 19.0%.
- the average aspect ratio was 522.
- the ratio of silver nanowires having an average aspect ratio of 50 or more was 82.5%.
- silver nanowire dispersion liquid (1) the silver nanowire dispersion liquid obtained by the said method is shown.
- Preparation Example 2 Preparation of silver nanowire dispersion (2)-
- a silver nanowire dispersion liquid (2) having a metal content of 0.47% was obtained in the same manner as Preparation Example 1 except that 125.0 g of distilled water was used instead of the additive solution A.
- the average minor axis length, the average major axis length, the coefficient of variation of the minor axis length of the silver nanowire, and the average aspect ratio were measured as described above.
- the average minor axis length was 47.0 nm
- the average major axis length was 13.0 ⁇ m
- the coefficient of variation was 22.9%.
- the average aspect ratio was 277.
- silver nanowire dispersion liquid (2) the silver nanowire dispersion liquid obtained by the said method is shown.
- a silver nitrate solution 301 was prepared by dissolving 60 g of silver nitrate powder in 370 g of propylene glycol. 72.0 g of polyvinylpyrrolidone (molecular weight 55,000) was added to 4.45 kg of propylene glycol, and the temperature was raised to 90 ° C. while venting nitrogen gas through the gas phase portion of the container. This solution was used as a reaction solution 301. While maintaining the nitrogen gas flow, 2.55 g of silver nitrate solution 301 was added to the reaction solution 301 that was vigorously stirred, and the mixture was heated and stirred for 1 minute. Furthermore, a solution in which 11.8 g of tetrabutylammonium chloride was dissolved in 100 g of propylene glycol was added to this solution to obtain a reaction solution 302.
- ultrafiltration was performed as follows. Addition and concentration of a mixed solution of distilled water and 1-propanol (volume ratio of 1: 1) to the charged solution 301 were repeated until the filtrate finally had a conductivity of 50 ⁇ S / cm or less. The obtained filtrate was concentrated to obtain a silver nanowire dispersion liquid (3) having a metal content of 0.45%. About the silver nanowire of the obtained silver nanowire dispersion liquid (3), the average minor axis length, the average major axis length, the coefficient of variation of the minor axis length of the silver nanowire, and the average aspect ratio were measured as described above.
- the average minor axis length was 26.8 nm
- the average major axis length was 14.0 ⁇ m
- the variation coefficient was 17.9%.
- the average aspect ratio was 522.
- Preparation Example 4 Pretreatment of glass substrate- A non-alkali glass substrate having a thickness of 0.7 ⁇ m is immersed in a 1% aqueous solution of sodium hydroxide and irradiated with ultrasonic waves for 30 minutes with an ultrasonic cleaner, then washed with ion-exchanged water for 60 seconds, and then at 200 ° C. for 60 minutes. Heat treatment was performed.
- a silane coupling liquid (0.3% aqueous solution of N- ⁇ (aminoethyl) ⁇ -aminopropyltrimethoxysilane, trade name: KBM603, manufactured by Shin-Etsu Chemical Co., Ltd.) was sprayed for 20 seconds with a shower, A glass substrate was obtained by shower washing with pure water.
- the “glass substrate” refers to the alkali-free glass substrate obtained by the pretreatment.
- a bonding solution 1 was prepared with the following composition.
- Adhesive solution 1 ⁇ Takelac WS-4000 5.0 parts (polyurethane for coating, solid content concentration 30%, manufactured by Mitsui Chemicals, Inc.) ⁇ Surfactant 0.3 part (Narrow Acty HN-100, manufactured by Sanyo Chemical Industries) ⁇ Surfactant 0.3 part (Sandet BL, solid content concentration 43%, Sanyo Chemical Industries, Ltd.) ⁇ 94.4 parts of water
- One surface of the 125 ⁇ m-thick PET film 10 was subjected to corona discharge treatment, and the adhesive solution 1 was applied to the surface subjected to the corona discharge treatment and dried at 120 ° C. for 2 minutes to obtain a thickness of 0.
- a first adhesive layer 31 having a thickness of 11 ⁇ m was formed.
- An adhesive solution 2 was prepared with the following composition.
- Adhesive solution 2 was prepared by the following method. While stirring the aqueous acetic acid solution vigorously, 3-glycidoxypropyltrimethoxysilane (KBM-403) was added dropwise to the aqueous acetic acid solution over 3 minutes. Next, 2- (3,4-epoxycyclohexyl) ethyltrimethoxysilane (KBM-303) was added to the resulting aqueous acetic acid solution over 3 minutes while vigorously stirring. Next, tetramethoxysilane was added to the acetic acid aqueous solution containing KBM-403 and KBM-303 with vigorous stirring over 5 minutes, and then the stirring was continued for 2 hours. Next, colloidal silica, a curing agent, and a surfactant were sequentially added thereto to prepare an adhesive solution 2.
- KBM-403 3-glycidoxypropyltrimethoxysilane
- KBM-303 2- (3,4-epoxycyclohexyl) eth
- the adhesive solution 2 is applied to the surface by a bar coating method, dried by heating at 170 ° C. for 1 minute, and having a thickness of 0.
- a second adhesive layer 32 of 5 ⁇ m was formed to obtain a PET substrate 101 having the configuration shown in FIG.
- Example 1 and Comparative Example 1 Preparation of conductive member 1-1) A solution containing an alkoxysilane compound having the following composition (hereinafter also referred to as a sol-gel solution) was stirred at 60 ° C. for 1 hour to confirm that the solution became uniform.
- a sol-gel solution an alkoxysilane compound having the following composition
- the obtained sol-gel solution (3.44 parts) and the silver nanowire dispersion (1) (16.56 parts) obtained in Preparation Example 1 were mixed, and the compound 1-1 described herein was silver.
- An aqueous solution of compound 1-1 was added and mixed so as to contain 0.3 mmol per 1 g of nanowires. Further, it was diluted with distilled water and 1-propanol to prepare a conductive layer coating solution 1-1 having a silver concentration of 0.25% and a 1-propanol concentration of 30%.
- the surface of the second adhesive layer 32 of the PET substrate 101 is subjected to corona discharge treatment, and the silver amount is 0.012 g / m 2 and the total solid content coating amount is 0.096 g / m 2 on the surface by a bar coating method. Then, the conductive layer coating solution 1-1 was applied so that the conductive layer 20 was dried at 140 ° C. for 1 minute to advance the sol-gel reaction, whereby the conductive layer 20 was formed. Thus, a conductive member 1-1 having the structure shown in the sectional view of FIG. 1 was obtained.
- a conductive member as a comparative example was prepared in the same manner as the production method of the conductive member 1-1 except that the compound 1-1 was not added at the preparation of the conductive layer coating solution. 1-2 was produced.
- the conductive member 1-1 is the same as that shown in Table 1, except that the type and amount of component compound (b) to be added (in mmol per 1 g of silver nanowires) are changed as shown in Table 1.
- Conductive members 1-3 to 1-18 of the present invention were produced in the same manner as the production method 1-1.
- conductive members 1-35 to 1-39 Preparation of conductive members 1-35 to 1-39
- the compound A-1 to A- described above can be used as a compound that can be adsorbed to a metal according to the present invention or a compound that can be coordinated to a metal ion.
- Conductive members 1-35 to 1-39, which are comparative examples, were prepared in the same manner as the conductive member 1-1 except that 4 was added (the types and amounts added are listed in Table 1).
- the fine line resistance of the conductive member patterned into a stripe pattern or a fine line pattern was measured using a tester (custom, CDM-5000E).
- a tester custom, CDM-5000E
- five resistance values of the conductive line were measured for each conductive member, and the average value was obtained.
- the resistance of 100 lines having a line width of 300 ⁇ m and a length of 30 mm was measured, and an average value was calculated.
- the total light transmittance (%) of each conductive member was measured using a haze guard plus manufactured by Gardner.
- the total light transmittance measurement of the conductive part and the non-conductive part after patterning was performed according to the following procedure. Since it is difficult to measure the conductive part and non-conductive part of an actual fine pattern with a haze meter, an evaluation pattern (10 mm ⁇ ) is placed in the same sample as the actual fine pattern, and the total light transmittance of the conductive part was measured. The measurement was performed for the CIE visibility function y under the C light source at a measurement angle of 0 °, and the average value was obtained by measuring the central part of five randomly selected conductive regions of a 10 cm ⁇ 10 cm sample. I did. A: Transmissivity of 90% or more, good level B: Transmissivity of 85% or more and less than 90%, somewhat problematic level
- Optical properties (haze) The haze value of the portion corresponding to the conductive region of the conductive member was measured using a haze guard plus manufactured by Gardner. The measurement was carried out by measuring the central part of five randomly selected conductive regions of a 10 cm ⁇ 10 cm sample to obtain an average value.
- the haze value measurement of the electroconductive part and non-conductive part after patterning was performed in the following procedure. Since it is difficult to measure the conductive part and non-conductive part of an actual fine pattern with a haze meter, an evaluation pattern (10 mm ⁇ ) is placed in the same sample as the actual fine pattern, and the haze value of the conductive part is measured. did.
- Each conductive member was subjected to forced heating treatment in an oven at 180 ° C. for 4 hours using a dry oven OFW-600 manufactured by AS ONE.
- RDT surface resistance value
- RDT / R0 rate of change of the surface resistance value relative to the surface resistance value (R0) before the heat treatment.
- the heat resistance of each conductive member was evaluated and the following ranking was performed.
- the same ranking was performed by the change rate of the above-mentioned thin wire
- Rank 5 Change rate of surface resistance value less than 10%
- Highly preferred level Rank 4 Change rate of surface resistance value 10% or more, less than 20%
- Preferred level Rank 3 Change rate of surface resistance value 20% or more, less than 35%
- Allowable level Rank 2 Rate of change of surface resistance value 35% or more, less than 50%
- Slightly problematic level Rank 1 Change rate of surface resistance value 50% or more Problem level
- Each electroconductive member was subjected to forced moist heat treatment by leaving it in an environment of 85 ° C. and 85% RH for 240 hours using a small environmental tester SH-241 manufactured by Espec Co., Ltd.
- SH-241 manufactured by Espec Co., Ltd.
- the heat-and-moisture resistance of the structural members was evaluated and the following ranking was performed.
- the same ranking was performed by the change rate of the above-mentioned thin wire
- Rank 5 Change rate of surface resistance value less than 10%
- Highly preferred level Rank 4 Change rate of surface resistance value 10% or more, less than 20%
- Preferred level Rank 3 Change rate of surface resistance value 20% or more, less than 35%
- Allowable level Rank 2 Rate of change of surface resistance value 35% or more, less than 50%
- Slightly problematic level Rank 1 Change rate of surface resistance value 50% or more Problem level
- Each conductive member is exposed to an ozone amount of 15 ppm at 25 ° C. for 4 hours, and the surface resistance value (ROT) of each conductive member before and after the treatment is measured by the method described above.
- ROT surface resistance value
- Rank 5 Change rate of surface resistance value 100% or more and less than 150%
- Highly preferred level Rank 4 Change rate of surface resistance value 150% or more and less than 200%
- Preferred level Rank 3 Change rate of surface resistance value 200% or more , Less than 350% Allowable level Rank 2: Change rate of surface resistance value 350% or more, less than 500%
- Slightly problematic level Rank 1 Change rate of surface resistance value 500% or more Problem level
- Table 1 shows the following.
- the conductive members 1-1, 1-3 to 1-34 containing the component compound (b) according to the present invention have little change in resistivity during high temperature storage, good ozone resistance, and excellent weather resistance. Excellent.
- the conductive members 1-19 to 1-25, 33 and 34 which are further used in combination with compounds represented by the general formulas (3) to (11), Compared with the case where only the component compound (b) according to the invention is added, the overall performance of the conductive member is excellent in terms of optical properties, heat resistance, moist heat resistance and ozone resistance.
- the conductive members 1-26 to 1-34 containing a compound that can be adsorbed to the metal according to the present invention or a compound that can be coordinated to a metal ion are: Compared with the case where only the component compound (b) according to the present invention is added, the overall performance of the conductive member is excellent in terms of optical properties, heat resistance, moist heat resistance and ozone resistance.
- the compounds represented by the general formulas (3) to (11), and the compounds adsorbable to the metal according to the present invention, or metal ions are coordinated.
- the conductive members 1-33 to 1-34 containing the possible compounds are more advantageous in terms of optical properties, heat resistance, moist heat resistance and ozone resistance than when only the component compound (b) according to the present invention is added.
- the overall performance of the conductive member is particularly excellent.
- the conductive members 1-2 and 1-35 to 1-33 of Comparative Examples to which the compound according to the present invention is not added are insufficient in terms of heat resistance, moist heat resistance or ozone resistance.
- Example 2 and Comparative Example 2 Evaluation of short axis length dependency-
- the method for preparing the silver nanowire dispersion liquid described in Preparation Example 1 except that the initial temperature 20 ° C. of the first-stage mixed liquid was changed to 24 ° C.
- a silver nanowire dispersion was prepared, and the obtained silver nanowire dispersion was designated as Ag-2.
- the preparation method of the silver nanowire dispersion liquid of the preparation example 1 it was the same as the preparation method of the silver nanowire dispersion liquid of the preparation example 1 except having changed the initial temperature 20 degreeC of the liquid mixture of the 1st step into 28 degreeC.
- a silver nanowire dispersion liquid was prepared, and the obtained silver nanowire dispersion liquid was designated as Ag-3.
- the average minor axis length, the average major axis length, and the coefficient of variation of the silver nanowire minor axis length were measured as described above.
- the silver nanowires contained in Ag-2 had an average minor axis length of 27.6 nm, an average major axis length of 31.8 ⁇ m, and a minor axis length variation coefficient of 25.2%.
- the silver nanowires contained in Ag-3 had an average minor axis length of 33.6 nm, an average major axis length of 28.8 ⁇ m, and a minor axis length variation coefficient of 27.5%.
- the conductive member 1- 1 was used except that Ag-2 was used instead of the silver nanowire dispersion liquid (1).
- Conductive members 2-1 to 2-3 were produced in the same manner as the production methods 1, 1-2, and 1-8.
- the conductive member 2 was prepared in the same manner as the conductive members 1-1, 1-2, and 1-8 except that Ag-3 was used instead of the silver nanowire dispersion liquid (1).
- -4 to 2-6 were produced.
- the silver nanowire dispersion liquid (2) of Preparation Example 2 was used instead of the silver nanowire dispersion liquid (1).
- Conductive members 2-7 to 2-9 were produced in the same manner as in the production methods of the conductive members 1-1, 1-2, and 1-8 except that the silver nanowire dispersion liquid (
- the conductive member 2 was prepared in the same manner as the conductive members 1-1, 1-2, and 1-8 except that the silver nanowire dispersion liquid (3) of Preparation Example 3 was used instead of 1).
- ⁇ 10 to 2-12 were produced.
- the obtained conductive members 2-1 to 2-12 were evaluated in the same manner as in Example 1, and the obtained evaluation results are shown in Table 2. For reference, the evaluation results of the conductive members 1-1, 1-2, and 1-8 obtained in Example 1 are also shown in Table 2.
- the effect of the present invention is also effective for thicker silver nanowires that have increased the average minor axis length of the silver nanowires. It can be seen that as the average minor axis length of the silver nanowires increases, the heat resistance, moist heat resistance and ozone resistance of the conductive member not containing the compound of the present invention improve, but are insufficient. On the other hand, as the average minor axis length of the silver nanowire increases, the haze value increases, and it can be seen that the smaller average minor axis length shows more preferable optical characteristics as the transparent conductive film.
- the effect of this invention expresses preferably also in the electroconductive member using the silver nanowire dispersion liquid (3) prepared in the non-aqueous solvent. That is, in order to realize more preferable optical characteristics as the transparent conductive film, it is effective to use silver nanowires having a short average minor axis length (that is, thin), and the heat resistance, moist heat resistance, and It can be seen that the present invention is particularly effective as a means for improving ozone resistance.
- Example 3 and Comparative Example 3 -Evaluation of conductive material after patterning-
- the conductive member 1-1 obtained in Example 1 was patterned by the following method.
- a positive resist (photosoluble composition) having the following composition was applied to the conductive member 1-1 using a wire bar coater so that the dry film thickness was 2 ⁇ m.
- the nanowire was dissolved to form a silver nanowire stripe pattern. Furthermore, the mask resist was completely dissolved by performing post-exposure and peeling development processing described later.
- Exposure was performed with a high-pressure mercury lamp i-line (365 nm) under conditions of an intensity of 150 mJ / cm 2 (illuminance 20 mW / cm 2 ).
- Exposure was performed with a high-pressure mercury lamp i-line (365 nm) under the condition of an intensity of 300 mJ / cm 2 (illuminance 20 mW / cm 2 ).
- Paddle development was performed for 90 seconds with a 0.4 mass% TMAH aqueous solution (23 ° C.) to remove the exposed portion. Subsequently, it was washed with pure water (23 ° C.) for 90 seconds, and after washing with water, the sample was dried at room temperature.
- the obtained patterned conductive member was designated as a conductive member 1-1P.
- (Positive resist composition) -Acrylic binder (A-1) 11.0 parts by mass as solid content-Photosensitizer (TAS-200 manufactured by Toyo Gosei Co., Ltd.) 6.2 parts by mass-EHPA-3150 (manufactured by Daicel Chemical Industries, Ltd.) 5 .2 parts by mass-Adhesion promoter (KBM-403 manufactured by Shin-Etsu Chemical Co., Ltd.) 0.1 parts by mass-Solvent PGMEA 45.0 parts by mass-Solvent MFG 32.5 parts by mass
- the weather resistance (heat resistance and ozone resistance) of each conductive member was evaluated by the following method.
- the resistance value was measured by the method described in [Resistance value of conductive member after patterning].
- the conductivity rank was ranked based on the surface resistance value, and the weather resistance was ranked based on the thin wire resistance value.
- the evaluation results are shown in Table 3.
- Example 4 and Comparative Example 4 In the method for producing the conductive members 1-1 to 1-43 of Example 1, the method for producing the conductive members 1-1 to 1-43, except that the PET substrate 101 was replaced with the glass substrate produced in Preparation Example 2. In the same manner, conductive members 4-1 to 4-43 were produced. As a result of evaluating these conductive members in the same manner as in Example 1, the conductivity of the present invention having the component compound (b) as compared with the conductive member 4-2 not having the component compound (b). All of the members 4-1, 4-3 to 4-34 exhibited good weather resistance (heat resistance and ozone resistance).
- Example 5 and Comparative Example 5 The conductive member 1-2 of the comparative example was immersed in an aqueous solution of the compound 1-1, 1-10, 1-11 or 2-2 for 5 minutes, washed with running water, and blown and dried. Conductive members 5-2P to 5-5P containing component compounds in the conductive layer were produced. In addition, in the method for producing the conductive member 5-2P, the conductive member 5-2P except that the aqueous solution of the compound 1-1 was replaced with the aqueous solution of the compound 1-1 or 1-10 and the compound 7-15. Conductive members 5-6P and 5-7P were produced in the same manner as the production method.
- the method for producing the conductive member 5-2P except that the aqueous solution of the compound 1-1 was replaced with the aqueous solution of the compound 2-2 and the compound 7-23. Similarly, conductive member 5-8P was produced.
- component compound (b) in the conductive layers of these conductive members 5-2P to 5-8P was subjected to solvent extraction after pulverizing each conductive member with a freezer mill, and using high performance liquid chromatography. It was measured by analysis. Evaluation similar to Example 1 was performed with respect to these conductive members. The results are shown in Table 4. In Table 4, the conductive member 1-2 of the comparative example is defined as the conductive member 5-1P, and the evaluation results are also shown.
- Example 6 and Comparative Example 6 For the conductive members 1-1, 1-2, and 1-8, a soluble protective layer having an average thickness of 0.8 ⁇ m was formed by applying a composition for a soluble protective layer having the following composition onto the conductive layer and drying it. Formed. Further, patterning was performed in the same manner as in Example 3 to prepare conductive members 6-1P to 6-9P. These conductive members were evaluated in the same manner as in Example 1. The results are shown in Table 5.
- this invention is effective also in the electroconductive member which has a soluble protective layer
- component compound of this invention is contained by any one of an electroconductive layer or a soluble protective layer. It can be seen that the effects of the present invention are exhibited. Even if the component compound (b) is contained in the soluble protective layer, the effect of the present invention is manifested. Therefore, the component compound (b) of the present invention is transferred from the soluble protective layer to the photosensitive layer and exhibits the effect. It is presumed that it is performing. Moreover, it turns out that it is more preferable that the effect of this invention is applied, after adding beforehand to an electroconductive layer coating liquid, or adding to both an electroconductive layer and a soluble protective layer.
- Example 7 Preparation of conductive member patterned by providing a photoresist layer
- resist composition (1) Preparation of resist composition (1)- Each component was added and stirred so that it might become the following composition, and the resist composition (1) was prepared.
- composition of resist composition (1) Composition of resist composition (1)
- the resist composition (1) obtained above was applied onto the conductive layer by a bar coating method so as to have a dry film thickness of 5 ⁇ m. It dried for 5 minutes in 150 degreeC oven.
- the substrate was irradiated with a high-pressure mercury lamp i-line (365 nm) at an intensity of 400 mJ / cm 2 (illuminance 50 mW / cm 2 ) from above the exposure mask and exposed in a nitrogen atmosphere.
- the exposed substrate was subjected to shower development for 60 seconds with a 1% sodium hydroxide aqueous solution at 35 ° C.
- the shower pressure was 0.08 MPa, and the time until the stripe pattern appeared was 30 seconds.
- conductive members 7-1R, 7-2R, and 7-3R with resist patterns.
- Example 8 -Fabrication of touch panel- Using the conductive member 1-1 of 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 ( (December 2004), “FPD International 2009 Forum T-11 Lecture Textbook”, “Cypress Semiconductor Corporation Application Note AN2292”, etc.
- the manufactured touch panel it is excellent in visibility by improving light transmittance, and it is suitable for character input or screen operation with at least one of bare hands, hands wearing gloves, pointing tool by improving conductivity It was found that a touch panel with excellent responsiveness can be manufactured.
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Abstract
Description
しかしながら、これらの金属導電性繊維を用いた導電性部材は、高温条件、高湿度条件またはオゾン存在下といった過酷な条件に長時間暴露された場合には、金属の酸化や形態変化に起因すると推定される抵抗率の上昇が起こる場合があり、用途によっては耐候性の改良が求められる場合があった。
本発明の導電性組成物は、少なくとも、(a)平均短軸長が1nm以上150nm以下の金属導電性繊維、並びに(b)下記一般式(1)で表される化合物および下記一般式(2)で表される化合物から選ばれる少なくとも1つの化合物、を含有する。
上記一般式(8)において、V8は、水素原子または置換基を表し、R81およびR82は、それぞれ独立に、水素原子または置換基を表す。一般式(9)において、V9は、水素原子または置換基を表し、R91、R92、R93およびR94は、それぞれ独立に、水素原子または窒素原子に置換可能な基を表す。一般式(10)において、V10は、水素原子または置換基を表し、R101、R102、R103およびR104は、それぞれ独立に、水素原子または窒素原子に置換可能な基を表す。一般式(11)において、R111は、水素原子または窒素原子に置換可能な基を表し、V111、V112、V113およびV114は、それぞれ独立に、水素原子または置換基を表し、V111およびV112、並びにV113およびV114は互いに連結して、ビシクロ環、トリシクロ環を形成してもよい。
以下、本発明の代表的な実施形態に基づいて記載されるが、本発明の主旨を超えない限りにおいて、本発明は記載された実施形態に限定されるものではない。
なお、本明細書において、「~」を用いて表される数値範囲は、「~」の前後に記載される数値を下限値および上限値として含む範囲を意味する。
本明細書中、アクリル酸、メタクリル酸のいずれか或いは双方を示すため「(メタ)アクリル酸」と、アクリレート、メタクリレートのいずれか或いは双方を示すため「(メタ)アクリレート」と、それぞれ表記することがある。
また、含有量は特に断りのない限り、質量換算で示し、特に断りのない限り、質量%は、組成物の総量に対する割合を表し、「固形分」とは、組成物中の溶剤を除く成分を表す。
本発明の導電性組成物は、少なくとも、(a)平均短軸長(以下、「平均短軸長さ」、「平均直径」ともいう。)が1nm以上150nm以下の金属導電性繊維(以下、「(a)金属導電性繊維」と称する場合がある)、並びに(b)下記一般式(1)で表される化合物および下記一般式(2)で表される化合物から選ばれる少なくとも1つの化合物(以下、「(b)成分化合物」と称する場合がある)、を含有する。
したがって、(b)成分化合物を金属導電性繊維の近傍に存在させるべく、導電性層中または導電性層に接する層に含有させることにより、過酸化物を低減させ、金属導電性繊維の酸化を抑制し、結果として導電性の低下を抑制しているものと推定される。
以下、本発明の導電性組成物の成分について詳細に説明する。
本発明の導電性組成物は、平均短軸長が1nm以上150nm以下の金属導電性繊維を含有する。金属導電性繊維の平均短軸長さは、1nm~150nmであり、耐久性および光学特性の観点から1nm~70nmが好ましく、1nm~50nmがより好ましく、1nm~40nmが更に好ましく、10nm~40nmが特に好ましい。
なお、金属導電性繊維の短軸方向断面が円形でない場合の平均短軸長さは、短軸方向の測定で最も長い箇所の長さを平均短軸長さとする。また。金属導電性繊維が曲がっている場合、それを弧とする円を考慮し、その半径、および曲率から算出される値を平均長軸長さとする。
アスペクト比の測定方法としては、特に制限はなく、目的に応じて適宜選択することができ、例えば、電子顕微鏡等により測定する方法などが挙げられる。
前記金属導電性繊維のアスペクト比を電子顕微鏡で測定する場合、前記金属導電性繊維のアスペクト比が50以上であるか否かは、電子顕微鏡の1視野で確認できればよい。また、前記金属導電性繊維の平均長軸長さと平均短軸長さとを各々別に測定することによって、前記金属導電性繊維全体のアスペクト比を見積もることができる。
なお、前記金属導電性繊維がチューブ状の場合には、前記アスペクト比を算出するための直径としては、該チューブの外径を用いる。
透明導電膜を形成しやすいという観点からは、金属導電性繊維として、金属ナノワイヤーを用いることが好ましい。本発明における金属ナノワイヤーは、平均短軸長さが1nm~150nmであって、平均長軸長さが1μm~100μmのものが好ましい。
前記変動係数を40%以下とすることにより、耐久性の優れた導電性を確保することが容易となる。
金属ナノワイヤーの平均短軸長さ(直径)の変動係数は、例えば透過型電子顕微鏡(TEM)像から300本の金属ナノワイヤーの平均短軸長さ(直径)を計測し、その標準偏差と平均値を計算することにより、求めることができる。
金属ナノワイヤーの断面形状は、基材上に金属ナノワイヤー水分散液を塗布し、断面を透過型電子顕微鏡(TEM)で観察することにより検知することができる。
前記金属としては、長周期表(IUPAC1991)の第4周期、第5周期、および第6周期からなる群から選ばれる少なくとも1種の金属が好ましく、第2~14族から選ばれる少なくとも1種の金属がより好ましく、第2族、第8族、第9族、第10族、第11族、第12族、第13族、および第14族から選ばれる少なくとも1種の金属が更に好ましく、主成分として含むことが特に好ましい。
また、金属ナノワイヤーの製造方法としては、特開2009-215594号公報、特開2009-242880号公報、特開2009-299162号公報、特開2010-84173号公報、特開2010-86714号公報などに記載の方法を用いることができる。
アルコール類としては、例えば、メタノール、エタノール、プロパノール、2-プロパノール、ブタノール、エチレングリコールなどが挙げられる。
エーテル類としては、例えば、ジオキサン、テトラヒドロフランなどが挙げられる。
ケトン類としては、例えば、アセトンなどが挙げられる。
なお、必要に応じて、粒子形成過程で温度を変更してもよい。当該粒子形成過程の途中で温度を変更することは、核形成の制御や再核発生の抑制、選択成長の促進による単分散性向上に効果があることがある。
還元剤としては、特に制限はなく、金属イオンを還元できるものの中から適宜選択することができる。例えば、水素化ホウ素金属塩、水素化アルミニウム塩、アルカノールアミン、脂肪族アミン、複素環式アミン、芳香族アミン、アラルキルアミン、アルコール、有機酸類、還元糖類、糖アルコール類、亜硫酸塩、ヒドラジン化合物、デキストリン、ハイドロキノン、ヒドロキシアミン、エチレングリコール、グルタチオンなどが挙げられる。
これらの中でも、還元糖類、その誘導体としての糖アルコール類、エチレングリコールが更に好ましく、還元糖類、その誘導体としての糖アルコール類、エチレングリコールが特に好ましい。前記還元剤によっては、機能として分散剤や溶媒としても機能する化合物があり、同様に好ましく用いることができる。
金属ナノワイヤーの形成に用いる還元剤は、金属ナノワイヤー形成後に、限外濾過、透析、ゲル濾過、デカンテーション、遠心分離などの手法により、残量が銀に対して0.1質量%未満まで除去することが好ましい。
分散剤とハロゲン化合物の添加のタイミングは、還元剤の添加前でも添加後でもよく、金属イオンあるいはハロゲン化金属微粒子の添加前でも添加後でもよいが、単分散性のよりよい金属ナノワイヤーを得るためには、ハロゲン化合物の添加を2段階以上に分けることが好ましい。
分散剤としては、例えばアミノ基含有化合物、メルカプト基含有化合物、スルフィド含有化合物、アミノ酸またはその誘導体、ペプチド化合物、多糖類、多糖類由来の天然高分子、合成高分子、またはこれらに由来するゲル等の高分子類、などが挙げられる。
分散剤として使用可能な化合物の構造については、例えば「顔料の事典」(伊藤征司郎編、株式会社朝倉書院発行、2000年)の記載を参照できる。使用する分散剤の種類によって得られる金属ナノワイヤーの形状を制御することができる。
ハロゲン化合物の代替としてハロゲン化銀微粒子を使用してもよく、ハロゲン化合物とハロゲン化銀微粒子を共に使用してもよい。
分散剤としての機能を有するハロゲン化合物としては、オニウム(好ましくは、アンモニウムまたはホスホニウム)のハロゲン化物イオン塩を好ましく挙げることができる。
例えば、ヘキサデシルトリメチルアンモニウムブロミド(HTAB)、ヘキサデシルトリメチルアンモニウムクロリド(HTAC)、ドデシルトリメチルアンモニウムブロミド、ドデシルトリメチルアンモニウムクロリド、ステアリルトリメチルアンモニウムブロミド、ステアリルトリメチルアンモニウムクロリド、デシルトリメチルアンモニウムブロミド、デシルトリメチルアンモニウムクロリド、ジメチルジステアリルアンモニウムブロミド、ジメチルジステアリルアンモニウムクロリド、ジラウリルジメチルアンモニウムブロミド、ジラウリルジメチルアンモニウムクロリド、ジメチルジパルミチルアンモニウムブロミド、ジメチルジパルミチルアンモニウムクロリド、などが挙げられる。
なお、これらの化合物は、金属ナノワイヤー形成後に、限外濾過、透析、ゲル濾過、デカンテーション、遠心分離などの手法により必要により除去してもよい。
金属ナノワイヤーを水性分散させたときの20℃における粘度は、0.5mPa・s~100mPa・sが好ましく、1mPa・s~50mPa・sがより好ましい。
金属ナノワイヤー以外の好ましい金属導電性繊維としては、中空繊維である金属ナノチューブが挙げられる。金属ナノチューブの材料としては、特に制限はなく、いかなる金属であってもよく、例えば、前記した金属ナノワイヤーの材料などを使用することができる。
前記金属ナノチューブの形状としては、単層であってもよく、多層であってもよいが、導電性および熱伝導性に優れる点で単層が好ましい。
本発明の導電性組成物は、下記一般式(1)で表される化合物および下記一般式(2)で表される化合物から選ばれる少なくとも1つの化合物、を含有する。
アルコキシカルボニルアミノ基(好ましくは炭素数2~30の置換もしくは無置換アルコキシカルボニルアミノ基、例えば、メトキシカルボニルアミノ、エトキシカルボニルアミノ、t-ブトキシカルボニルアミノ、n-オクタデシルオキシカルボニルアミノ、N-メチルーメトキシカルボニルアミノ)、アリールオキシカルボニルアミノ基(好ましくは、炭素数7~30の置換もしくは無置換のアリールオキシカルボニルアミノ基、例えば、フェノキシカルボニルアミノ、p-クロロフェノキシカルボニルアミノ、m-n-オクチルオキシフェノキシカルボニルアミノ)、スルファモイルアミノ基(好ましくは、炭素数0~30の置換もしくは無置換のスルファモイルアミノ基、例えば、スルファモイルアミノ、N,N-ジメチルアミノスルホニルアミノ、N-n-オクチルアミノスルホニルアミノ)、アルキルおよびアリールスルホニルアミノ基(好ましくは炭素数1~30の置換もしくは無置換のアルキルスルホニルアミノ、炭素数6~30の置換もしくは無置換のアリールスルホニルアミノ、例えば、メチルスルホニルアミノ、ブチルスルホニルアミノ、フェニルスルホニルアミノ、2,3,5-トリクロロフェニルスルホニルアミノ、p-メチルフェニルスルホニルアミノ)、
更に好ましくは、フェニル、2-メチルフェニル、4-メチルフェニル、2-エチルフェニル、4-エチルフェニル、2,4-ジメチルフェニル、2,6-ジメチルフェニル、2,4,6-トリメチルフェニル、1-ナフチル、2-ナフチル、2-クロロフェニル、4-クロロフェニル、2-メトキシフェニル、3-メトキシフェニル、4-メトキシフェニル、2-ベンジルフェニル、4-ベンジルフェニルなどを挙げることができ、特に好ましくは、フェニルなどを挙げることができる。
更に好ましくは、フェニル、2,4-ジ-t-ブチルフェノキシ、2,4,6-トリ-t-ブチルフェノキシなどを挙げることができる。
R1およびR2で表されるアリールオキシ基は、さらに置換基を有していてもよい。置換基の例としては、前述のR1、R2およびR3で表されるアルキル基の置換基を挙げることができる。
なお、(b)成分化合物として、一般式(1)で表される化合物と、一般式(2)で表される化合物とを併用してもよい。併用することにより、耐熱性および耐オゾン性の両方の性能を向上させることができる。
本発明の導電性組成物は、上記(b)成分化合物に加えて、さらに下記一般式(3)~(11)で表される化合物を含むことが好ましい。
一般式(4)において、V4は、水素原子または置換基を表す。
一般式(5)において、V5は、水素原子または置換基を表し、R51およびR52は、それぞれ独立に、水素原子または窒素原子に置換可能な基を表す。
一般式(6)において、V6は、水素原子または置換基を表し、R61およびR62は、それぞれ独立に、水素原子または窒素原子に置換可能な基を表す。
上記一般式(7)において、V7は、水素原子または置換基を表し、R71およびR72は、それぞれ独立に、水素原子または置換基を表す。
上記一般式(8)において、V8は、水素原子または置換基を表し、R81およびR82は、それぞれ独立に、水素原子または置換基を表す。
一般式(9)において、V9は、水素原子または置換基を表し、R91、R92、R93およびR94は、それぞれ独立に、水素原子または窒素原子に置換可能な基を表す。
一般式(10)において、V10は、水素原子または置換基を表し、R101、R102、R103およびR104は、それぞれ独立に、水素原子または窒素原子に置換可能な基を表す。
一般式(11)において、R111は、水素原子または窒素原子に置換可能な基を表し、V111、V112、V113およびV114は、それぞれ独立に、水素原子または置換基を表し、V111およびV112、並びにV113およびV114は互いに連結して、ビシクロ環、トリシクロ環を形成してもよい。
前記一般式(3)~(11)で表される化合物は、導電性層中または導電性層と接する層中で発生したラジカル種を失活させる機能を有しているものと考えられる。
したがって、ラジカル種を失活させ得る一般式(3)~(11)で表される化合物と、ラジカル種により生成する過酸化物を失活させ得る(b)成分化合物とを併用することは、導電性の低下を抑える観点から好適である。
以下に、一般式(3)で表される化合物の具体例を示す。但し、本発明はこれらに限定されるものではない。
以下に、一般式(4)で表される化合物の具体例を示す。但し、本発明はこれらに限定されるものではない。
一般式(5)におけるV5で表される基の結合形態は、一般式(5)に含まれる環状構造の置換可能な任意の位置に、1~4個の範囲で任意の個数が結合していることを表す。V5が置換基を表すとき、好ましい基としては、前述の一般式(1)においてR1、R2およびR3で表されるアルキル基で説明した置換基を挙げることができる。一般式(5)に複数のV5で表される基が存在している場合、それぞれの基は同一であっても、異なっていてもよく、互いに結合して環を形成していてもよい。
一般式(6)におけるV6で表される基の結合形態は、一般式(6)に含まれる環状構造の置換可能な任意の位置に、1~4個の範囲で任意の個数が結合していることを表す。V6が置換基を表すとき、好ましい基としては、前述の一般式(1)においてR1、R2およびR3で表されるアルキル基で説明した置換基を挙げることができる。一般式(6)に複数のV6で表される基が存在している場合、それぞれの基は同一であっても、異なっていてもよく、互いに結合して環を形成していてもよい。
一般式(7)におけるV7で表される基の結合形態は、一般式(7)に含まれる環状構造の置換可能な任意の位置に、1~4個の範囲で任意の個数が結合していることを表す。V7が置換基を表すとき、好ましい基としては、前述の一般式(1)においてR1、R2およびR3で表されるアルキル基で説明した置換基を挙げることができる。一般式(7)に複数のV7で表される基が存在している場合、それぞれの基は同一であっても、異なっていてもよく、互いに結合して環を形成していてもよい。
R71またはR72が置換基を表す場合、これらの基は、さらに置換基を有していてもよい。置換基の例としては、前述の一般式(1)のR1、R2およびR3で表されるアルキル基で説明した置換基を挙げることができる。
一般式(8)におけるV8で表される基の結合形態は、一般式(8)に含まれる環状構造の置換可能な任意の位置に、1~4個の範囲で任意の個数が結合していることを表す。V8が置換基を表すとき、好ましい基としては、前述の一般式(1)においてR1、R2およびR3で表されるアルキル基で説明した置換基を挙げることができる。一般式(8)に複数のV8で表される基が存在している場合、それぞれの基は同一であっても、異なっていてもよく、互いに結合して環を形成していてもよい。
R81およびR82で表される置換基としては、前述のR1、R2およびR3で表されるアルキル基で説明した置換基を挙げることができ、好ましくは、アルキル基、アルケニル基、アルキニル基、または、アリール基であり、それぞれの好ましい例としては、前述のR1、R2およびR3で説明した例を挙げることができる。
R81またはR82が置換基を表す場合、これらの基は、さらに置換基を有していてもよい。置換基の例としては、前述の一般式(1)のR1、R2およびR3で表されるアルキル基で説明した置換基を挙げることができる。
一般式(9)におけるV9で表される基の結合形態は、一般式(9)に含まれる環状構造の置換可能な任意の位置に、1~4個の範囲で任意の個数が結合していることを表す。V9が置換基を表すとき、好ましい基としては、前述の一般式(1)においてR1、R2およびR3で表されるアルキル基で説明した置換基を挙げることができる。一般式(9)に複数のV9で表される基が存在している場合、それぞれの基は同一であっても、異なっていてもよく、互いに結合して環を形成していてもよい。
一般式(10)におけるV10で表される基の結合形態は、一般式(10)に含まれる環状構造の置換可能な任意の位置に、1~4個の範囲で任意の個数が結合していることを表す。V10が置換基を表すとき、好ましい基としては、前述の一般式(1)においてR1、R2およびR3で表されるアルキル基で説明した置換基を挙げることができる。一般式(10)に複数のV10で表される基が存在している場合、それぞれの基は同一であっても、異なっていてもよく、互いに結合して環を形成していてもよい。
V111、V112、V113およびV114が置換基を表すとき、好ましい基としては、前述の一般式(1)においてR1、R2およびR3で表されるアルキル基で説明した置換基を挙げることができる。V111、V112、V113およびV114は、それぞれの基は同一であっても、異なっていてもよく、互いに結合して環を形成していてもよい。
また、オゾン存在下での導電性の観点からは、一般式(1)で表される化合物又は(2)で表される化合物と、一般式(3)~(11)の少なくとも1種で表される化合物を組み合わせることが好ましく、一般式(1)で表される化合物と、一般式(3)~(11)の少なくとも1種で表される化合物を組み合わせることがより好ましい。
本発明の導電性組成物は、さらにマトリックスを形成し得る重合性化合物を含んでいてもよい。ここで、「マトリックス」とは、金属導電性繊維を含んで層を形成する物質の総称であり、金属導電性繊維の分散を安定に維持させる機能を有する。マトリックスは、非感光性のものであっても、感光性のものであってもよい。導電性層がマトリックスを含むことにより、導電性層における金属導電性繊維の分散が安定に維持される上、基材表面に導電性層を接着層を介することなく形成した場合においても基材と導電性層との強固な接着が確保されるため、より好ましい。
非感光性マトリックスについて説明する。好適な非感光性マトリックスとしては、有機高分子または、無機高分子を含むものが挙げられる。
上記ゾルゲル硬化物は、キズおよび磨耗に対して高い耐性を有するものが容易に製造できるという点から好ましい。
M(ORp)aRq 4-a (12)
アルキル基を示す場合の炭素数は好ましくは1~18、より好ましくは1~8であり、さらにより好ましくは1~4である。また、アリール基を示す場合は、フェニル基が好ましい。
アルキル基またはアリール基は置換基を更に有していてもよく、導入可能な置換基としては、前述の一般式(1)におけるR1、R2およびR3で表されるアルキル基で例示した置換基を挙げることができる。この化合物は分子量1000以下であることが好ましい。
以下に、一般式(12)で示される化合物の具体例を挙げるが、本発明はこれに限定されるものではない。
MがSiでaが2の場合、すなわち、ジアルコキシシランとしては、例えば、ジメチルジメトキシシラン、ジエチルジメトキシシラン、プロピルメチルジメトキシシラン、ジメチルジエトキシシラン、ジエチルジエトキシシラン、ジプロピルジエトキシシラン、γ-クロロプロピルメチルジエトキシシラン、アセトキシメチルメチルジエトキシシラン、アセトキシメチルメチルジメトキシシラン、フェニルメチルジメトキシシラン、フェニルエチルジエトキシシラン、フェニルメチルジプロポキシシラン、ビニルメチルジメトキシシラン、ビニルメチルジエトキシシラン、ビニルメチルジブトキシシラン、イソプロペニルメチルジメトキシシラン、イソプロペニルメチルジエトキシシラン、イソプロペニルメチルジブトキシシラン、などを挙げることができる。これらのうち特に好ましいものとしては、入手容易な観点と親水性層との密着性の観点から、ジメチルジメトキシシラン、ジエチルジメトキシシラン、ジメチルジエトキシシラン、ジエチルジエトキシシラン等を挙げることができる。
MがTiでaが2の場合、すなわち、ジアルコキシチタネートとしては、例えば、ジメチルジメトキシチタネート、ジエチルジメトキシチタネート、プロピルメチルジメトキシチタネート、ジメチルジエトキシチタネート、ジエチルジエトキシチタネート、ジプロピルジエトキシチタネート、フェニルエチルジエトキシチタネート、フェニルメチルジプロポキシチタネート、ジメチルジプロポキシチタネート等を挙げることができる。
MがTiでaが3の場合、すなわち、トリアルコキシチタネートとしては、例えば、メチルトリメトキシチタネート、エチルトリメトキシチタネート、プロピルトリメトキシチタネート、メチルトリエトキシチタネート、エチルトリエトキシチタネート、プロピルトリエトキシチタネート、クロロメチルトリエトキシチタネート、フェニルトリメトキシチタネート、フェニルトリエトキシチタネート、フェニルトリプロポキシチタネート等を挙げることができる。
MがTiでaが2の場合、すなわち、テトラアルコキシチタネートとしては、例えば、テトラメトキシチタネート、テトラエトキシチタネート、テトラプロポキシチタネート、テトライソプロポキシチタネート、テトラブトキシチタネート等を挙げることができる。
MがZrの場合、すなわち、ジルコニウムのアルコキシドとしては、例えば、前記チタンを含むものとして例示した化合物に対応するジルコネートを挙げることができる。
MがAlの場合、即ち、アルミニウムのアルコキシドとしては、例えば、トリメトキシアルミネート、トリエトキシアルミネート、トリプロポキシアルミネート、テトラエトキシアルミネート等を挙げることができる。
上記特定アルコキシドは、一種類の化合物を単独で用いても、二種類以上の化合物を組み合わせて使用してもよい。
本発明の導電性組成物が前記特定アルコキシドを含む場合には、ゾルゲル反応を促進させるため、酸性触媒または塩基性触媒を添加することが好ましい。以下、この触媒について、説明する。
触媒としては、アルコキシド化合物の加水分解および重縮合の反応を促進させるものであれば、任意のものを使用することができる。
このような触媒としては、酸、あるいは塩基性化合物が含まれ、そのまま用いるか、または、水またはアルコールなどの溶媒に溶解させた状態のもの(以下、これらを包括してそれぞれ酸性触媒、塩基性触媒とも称する)が使用される。
酸、あるいは塩基性化合物を溶媒に溶解させる際の濃度については特に限定はなく、用いる酸、或いは塩基性化合物の特性、触媒の所望の含有量などに応じて適宜選択すればよい。ここで、触媒を構成する酸或いは塩基性化合物の濃度が高い場合は、加水分解、重縮合速度が速くなる傾向がある。但し、濃度の高過ぎる塩基性触媒を用いると、沈殿物が生成して導電性層に欠陥となって現れる場合があるので、塩基性触媒を用いる場合、その濃度は水溶液での濃度換算で1N以下であることが好ましい。
構成金属元素の中では、Mg、Ca、St、Baなどの第2族元素;Al、Gaなどの第13族元素;Ti、Zrなどの第4族元素;およびV、Nb、Taなどの第5族元素;が好ましく、それぞれ触媒効果の優れた錯体を形成する。その中でもZr、AlおよびTiから得られる錯体が優れており、好ましい。
金属錯体のシリカゾルゲル反応での挙動については、J.Sol-Gel.Sci.and Tec.16.209(1999)に詳細な記載がある。反応メカニズムとしては以下のスキームを推定している。すなわち、塗布液中では、金属錯体は、配位構造を取って安定であり、塗布後の加熱乾燥過程に始まる脱水縮合反応では、酸触媒に似た機構で架橋を促進させるものと考えられる。いずれにしても、この金属錯体を用いたことにより塗布液の経時安定性、並びに導電性層の皮膜面質および高耐久性に優れるものを得られる。
上記の金属錯体触媒は、市販品として容易に入手でき、また公知の合成方法、例えば各金属塩化物とアルコールとの反応によっても得られる。
上記のゾルゲル塗布液には、基材上に均一な塗布液膜の形成性を確保するために、所望により、溶剤を含有させてもよい。
このような溶剤としては、例えば、水、ケトン系溶剤(例えば、アセトン、メチルエチルケトン、ジエチルケトンなど)、アルコール系溶剤(例えば、メタノール、エタノール、2-プロパノール、1-プロパノール、1-ブタノール、tert-ブタノールなど)、塩素系溶剤(例えば、クロロホルム、ジクロロメタンなど)、芳香族系溶剤(例えば、ベンゼン、トルエンなど)、エステル系溶剤(例えば、酢酸エチル、酢酸ブチル、酢酸イソプロピルなど)、エーテル系溶剤(例えば、ジエチルエーテル、テトラヒドロフラン、ジオキサンなど)、グリコールエーテル系溶剤(例えば、エチレングリコールモノメチルエーテル、エチレングリコールジメチルエーテルなど)等が挙げられる。
次に、感光性マトリックスについて説明する。
感光性マトリックスの好ましい例としては、リソグラフィック・プロセスに好適なフォトレジスト組成物が挙げられる。マトリックスとしてフォトレジスト組成物を含む場合には、導電性領域と非導電性領域とをパターン状に有する導電性層を、リソグラフィック・プロセスにより形成することが可能となる点で好ましい。このようなフォトレジスト組成物のうち、特に好ましいものとして、透明性および柔軟性に優れ、かつ基材との接着性に優れた導電性層が得られるという点から、光重合性組成物が挙げられる。以下、この光重合性組成物について説明する。
光重合性組成物は、(I)付加重合性不飽和化合物と、(II)光が照射されるとラジカルを発生する光重合開始剤とを基本成分として含み、更に所望により(III)バインダー、(IV)その他、上記成分(I)~(III)以外の添加剤を含むものである。
以下、これらの成分について、説明する。
成分(I)の付加重合性不飽和化合物(以下、「重合性化合物」ともいう。)は、ラジカルの存在下で付加重合反応を生じて高分子化される化合物であり、通常、分子末端に少なくとも一つの、より好ましくは二つ以上の、更に好ましくは四つ以上のエチレン性不飽和結合を有する化合物が使用される。これらは、例えば、モノマー、プレポリマー、即ち2量体、3量体およびオリゴマー、またはそれらの混合物などの化学的形態をもつ。このような重合性化合物としては、種々のものが知られており、それらは成分(I)として使用することができる。
成分(II)の光重合開始剤は、光が照射されるとラジカルを発生する化合物である。このような光重合開始剤には、光照射により、最終的には酸となる酸ラジカルを発生する化合物およびその他のラジカルを発生する化合物などが挙げられる。以下、前者を「光酸発生剤」と呼び、後者を「光ラジカル発生剤」と呼ぶ。
光酸発生剤としては、光カチオン重合の光開始剤、光ラジカル重合の光開始剤、色素類の光消色剤、光変色剤、あるいはマイクロレジスト等に使用されている活性光線または放射線の照射により酸ラジカルを発生する公知の化合物およびそれらの混合物を適宜に選択して使用することができる。
また、活性光線または放射線の照射により酸ラジカルを発生する基、あるいは化合物を樹脂の主鎖または側鎖に導入した化合物、例えば、米国特許第3,849,137号明細書、独国特許第3914407号明細書、特開昭63-26653号、特開昭55-164824号、特開昭62-69263号、特開昭63-146038号、特開昭63-163452号、特開昭62-153853号、特開昭63-146029号の各公報等に記載の化合物を用いることができる。
更に、米国特許第3,779,778号、欧州特許第126,712号等の各明細書に記載の化合物も、酸ラジカル発生剤として使用することができる。
光ラジカル発生剤は、光を直接吸収し、または光増感されて分解反応若しくは水素引き抜き反応を起こし、ラジカルを発生する機能を有する化合物である。光ラジカル発生剤としては、波長200nm~500nmの領域に吸収を有するものであることが好ましい。
このような光ラジカル発生剤としては、多数の化合物が知られており、例えば特開2008-268884号公報に記載されているようなカルボニル化合物、ケタール化合物、ベンゾイン化合物、アクリジン化合物、有機過酸化化合物、アゾ化合物、クマリン化合物、アジド化合物、メタロセン化合物、ヘキサアリールビイミダゾール化合物、有機ホウ酸化合物、ジスルホン酸化合物、オキシムエステル化合物、アシルホスフィン(オキシド)化合物、が挙げられる。これらは目的に応じて適宜選択することができる。これらの中でも、ベンゾフェノン化合物、アセトフェノン化合物、ヘキサアリールビイミダゾール化合物、オキシムエステル化合物、およびアシルホスフィン(オキシド)化合物が露光感度の観点から特に好ましい。
バインダーとしては、線状有機高分子重合体であって、分子(好ましくは、アクリル系共重合体、スチレン系共重合体を主鎖とする分子)中に少なくとも1つのアルカリ可溶性を促進する基(例えばカルボキシル基、リン酸基、スルホン酸基など)を有するアルカリ可溶性樹脂の中から適宜選択することができる。
これらの中でも、有機溶剤に可溶でアルカリ水溶液に可溶なものが好ましく、また、解離性基を有し、塩基の作用により解離性基が解離した時にアルカリ可溶となるものが特に好ましい。ここで、解離性基とは、塩基の存在下で解離することが可能な官能基を表す。
前記側鎖にカルボン酸を有するポリマーとしては、例えば特開昭59-44615号、特公昭54-34327号、特公昭58-12577号、特公昭54-25957号、特開昭59-53836号、特開昭59-71048号の各公報に記載されているような、メタクリル酸共重合体、アクリル酸共重合体、イタコン酸共重合体、クロトン酸共重合体、マレイン酸共重合体、部分エステル化マレイン酸共重合体等、並びに側鎖にカルボン酸を有する酸性セルロース誘導体、水酸基を有するポリマーに酸無水物を付加させたもの等であり、更に側鎖に(メタ)アクリロイル基を有する高分子重合体も好ましいものとして挙げられる。
更に、側鎖に(メタ)アクリロイル基を有する高分子重合体や(メタ)アクリル酸/グリシジル(メタ)アクリレート/他のモノマーからなる多元共重合体も有用なものとして挙げられる。該ポリマーは任意の量で混合して用いることができる。
前記アルキル(メタ)アクリレートまたはアリール(メタ)アクリレートとしては、例えばメチル(メタ)アクリレート、エチル(メタ)アクリレート、プロピル(メタ)アクリレート、ブチル(メタ)アクリレート、イソブチル(メタ)アクリレート、ペンチル(メタ)アクリレート、ヘキシル(メタ)アクリレート、オクチル(メタ)アクリレート、フェニル(メタ)アクリレート、ベンジル(メタ)アクリレート、トリル(メタ)アクリレート、ナフチル(メタ)アクリレート、シクロヘキシル(メタ)アクリレート、ジシクロペンタニル(メタ)アクリレート、ジシクロペンテニル(メタ)アクリレート、ジシクロペンテニルオキシエチル(メタ)アクリレート、などが挙げられる。これらは、1種単独で使用してもよいし、2種以上を併用してもよい。
ここで、前記重量平均分子量は、ゲル・パーミエイション・クロマトグラフィー法により測定し、標準ポリスチレン検量線を用いて求めることができる。
光重合性組成物は、上記成分(I)~(III)以外のその他の添加剤を添加してもよい。その他の添加剤としては、例えば、増感剤、連鎖移動剤、架橋剤、分散剤、溶媒、界面活性剤、酸化防止剤、硫化防止剤、金属腐食防止剤、粘度調整剤、防腐剤等の各種の添加剤などが挙げられる。
連鎖移動剤は、光重合性組成物の露光感度向上のために使用されるものである。このような連鎖移動剤としては、例えば、N,N-ジメチルアミノ安息香酸エチルエステルなどのN,N-ジアルキルアミノ安息香酸アルキルエステル、2-メルカプトベンゾチアゾール、2-メルカプトベンゾオキサゾール、2-メルカプトベンゾイミダゾール、N-フェニルメルカプトベンゾイミダゾール、1,3,5-トリス(3-メルカブトブチルオキシエチル)-1,3,5-トリアジン-2,4,6(1H,3H,5H)-トリオンなどの複素環を有するメルカプト化合物、ペンタエリスリトールテトラキス(3-メルカプトプロピオネート)、ペンタエリスリトールテトラキス(3-メルカプトブチレート)、1,4-ビス(3-メルカプトブチリルオキシ)ブタンなどの脂肪族多官能メルカプト化合物などが挙げられる。これらは、1種単独で使用してもよいし、2種以上を併用してもよい。
架橋剤は、フリーラジカル又は酸及び熱により化学結合を形成し、導電性層を硬化させる化合物で、例えばメチロール基、アルコキシメチル基、アシロキシメチル基から選ばれる少なくとも1つの基で置換されたメラミン系化合物、グアナミン系化合物、グリコールウリル系化合物、ウレア系化合物、フェノール系化合物もしくはフェノールのエーテル化合物、エポキシ系化合物、オキセタン系化合物、チオエポキシ系化合物、イソシアネート系化合物、又はアジド系化合物、メタクリロイル基又はアクリロイル基などを含むエチレン性不飽和基を有する化合物、などが挙げられる。これらの中でも、膜物性、耐熱性、溶剤耐性の点でエポキシ系化合物、オキセタン系化合物、エチレン性不飽和基を有する化合物が特に好ましい。
なお、架橋剤としてエチレン性不飽和二重結合基を有する化合物を用いる場合、当該架橋剤も、また、前記(I)重合性化合物に包含され、その含有量は、本発明における(I)重合性化合物の含有量に含まれることを考慮すべきである。
架橋剤の含有量は、前述の金属導電性繊維を含む光重合性組成物の固形分の総質量を基準として、1質量部~250質量部が好ましく、3質量部~200質量部がより好ましい。
分散剤は、光重合性組成物中における前述の金属導電性繊維が凝集することを防止しつつ分散させるために用いられる。分散剤としては、前記金属導電性繊維を分散させることができれば特に制限はなく、目的に応じて適宜選択することができる。例えば、顔料分散剤として市販されている分散剤を利用でき、特に金属導電性繊維に吸着する性質を持つ高分子分散剤が好ましい。このような高分子分散剤としては、例えばポリビニルピロリドン、BYKシリーズ(ビックケミー社製)、ソルスパースシリーズ(日本ルーブリゾール社製など)、アジスパーシリーズ(味の素株式会社製)などが挙げられる。
分散剤の含有量としては、成分(III)のバインダー100質量部に対し、0.1質量部~50質量部が好ましく、0.5質量部~40質量部がより好ましく、1質量部~30質量部が特に好ましい。分散剤の含有量を0.1質量部以上とすることで、分散液中での金属導電性繊維の凝集が効果的に抑制され、50質量部以下とすることで、塗布工程において安定な液膜が形成され、塗布ムラの発生が抑制されるため好ましい。
溶媒は、前述の金属導電性繊維を含む光重合性組成物を基材表面に膜状に形成するための塗布液とするために使用される成分であり、目的に応じて適宜選択することができ、例えば、プロピレングリコールモノメチルエーテル(PGME)、プロピレングリコールモノメチルエーテルアセテート(PGMEA)、メタノール、エタノール、1-プロパノール、2-プロパノール、ブタノール、1-メトキシ-2-プロパノール、3-メトキシブタノール、アセトン、メチルエチルケトン、メチルイソブチルケトン、シクロヘキサノン、酢酸メチル、酢酸エチル、酢酸プロピル、酢酸イソプロピル、酢酸ブチル、3-エトキシプロピオン酸エチル、3-メトキシプロピオン酸メチル、乳酸エチル、γ-ブチロラクトン、炭酸プロピレン、N-メチル-2-ピロリジノン、N-エチル-2-ピロリジノンなどが挙げられる。これらは、1種単独で使用してもよいし、2種以上を併用してもよい。
このような溶媒を含む塗布液の固形分濃度は、0.1質量%~20質量%の範囲で含有させることが好ましい。
本発明の導電性組成物には、上記成分(a)~(c)以外に、更に、金属に吸着可能な化合物、または金属イオンに配位可能な化合物を含有してもよい。このような金属に吸着可能な化合物、または金属イオンに配位可能な化合物としては、特に制限はなく、目的に応じて適宜選択することができる。例えばアゾール化合物(ベンゾトリアゾール、4-メチルベンゾトリアゾール、5-メチルベンゾトリアゾール、4-エチルベンゾトリアゾール、5,6-ジメチルベンゾベンゾトリアゾール、トリルトリアゾール、ベンジルトリアゾール、5,6-ジメチルベンゾイミダゾール、チアジアゾール、テトラゾールなど)、トリアジン化合物、アンモニウム化合物、ホスホニウム化合物、メルカプト化合物(2-メルカプトベンゾオキサゾール、2-メルカプトベンゾチアゾール、2-メルカプトテトラゾール、2-メルカプトピリミジン、2-メルカプトベンゾイミダゾール、ジチオチアジアゾール、アルキルジチオチアジアゾール、および、アルキルチオールなど)、スルフィド化合物、ジスルフィド化合物などが好適である。
金属に吸着可能な化合物、または金属イオンに配位可能な化合物の添加方法は任意の方法から選択できるが、例えば、導電性組成物中に、化合物単独、あるいは適切な溶媒で溶解または分散した溶液として添加してもよく、作製後の導電性層を金属に吸着可能な化合物、または金属イオンに配位可能な化合物の溶液に浸漬してもよい。
金属に吸着可能な化合物、または金属イオンに配位可能な化合物の好ましい添加量は、金属導電性繊維の質量あたり、好ましくは0.1%以上100%以下であり、更に好ましくは1%以上50%以下であり、特に好ましくは2%以上25%以下である。0.1%以上100%以下とすることにより、金属導電性繊維の腐蝕または錆びの発生を効果的に防止しつつ、高い導電性が維持される。
上記の塗布液における金属導電性繊維の濃度は、0.001質量%以上50質量%以下の範囲から、所望とする導電性層の厚さに応じて適宜選択される。
本発明の導電性部材は、基材上に、少なくとも、(a)平均短軸長さが1nm以上150nm以下の金属導電性繊維、(b)成分化合物、を含有する導電性層を有する。
導電性層は、基材上に直接設けられても、基材上に設けた、下塗り層、中間層、クッション層など、単数または複数の他の層の上に設けられていてもよい。また、導電性層上には、表面保護層(可溶性保護層など)、ハードコート層、酸素遮断層、帯電防止層などの他の層を更に設けてもよい。特に、導電性層が前記(c)マトリックスを含まない導電性組成物によって形成される場合、基材上に予め接着層を設けておき、この接着層上に、上記導電性組成物で構成される導電性層を設けた態様が好ましい。
上記基材としては、導電性層を担うことができるものである限り、形状、構造、大きさ等については特に制限はなく、目的に応じて適宜選択することができ、例えば、前記形状としては、板状、膜状、および、シート状などが挙げられる。構造としては、単層構造、積層構造などが挙げられる。基材は、透明であっても、不透明であってもよい。
基材の材料としては特に制限はなく、目的に応じて適宜選択することができる。例えば、透明ガラス基板、合成樹脂製シート(フィルム)、金属基板、セラミック板、半導体基板に使用されるシリコンウエハーなどを挙げることができる。
合成樹脂製シートとしては、例えば、ポリエチレンテレフタレート(PET)シート、ポリカーボネートシート、トリアセチルセルロース(TAC)シート、ポリエーテルスルホンシート、ポリエステルシート、アクリル樹脂シート、塩化ビニル樹脂シート、芳香族ポリアミド樹脂シート、ポリアミドイミドシート、ポリイミドシートなどが挙げられる。
金属基板としては、例えば、アルミニウム板、銅板、ニッケル板、ステンレス板などが挙げられる。
本発明に用いられるプラズマ処理としては、真空グロー放電、大気圧グロー放電等によるものがあり、その他の方法としてフレームプラズマ処理等の方法があげられる。これらは、例えば特開平6-123062号公報、特開平11-293011号公報、同11-5857号公報等に記載された方法を用いることができる。
コロナ放電処理は、従来公知のいずれの方法、例えば特公昭48-5043号公報、同47-51905号公報、特開昭47-28067号公報、同49-83767号公報、同51-41770号公報、同51-131576号公報等に開示された方法により達成することができる。処理機としては市販の各種コロナ処理機が適用でき、例えばSOFTAL(ソフタル)社のマルチナイフ電極を有するコロナ処理機は多数本の電極で構成され、電極の間に空気を送ることによりフィルムの加熱防止やフィルム表面に出てくる低分子の除去等が行えるので有用である。また、片面に導電性層を付与した基材の、導電性層を付与していない面に対しては、電極と導電性層の間のスパークを避けるために、放電電極としては誘電体被覆電極(セラミック電極、クォーツ電極など)を、対向電極としてはステンレスなどの金属ロールを用いてコロナ処理を行うことが望ましい。
なお、本発明では、前記基材として本発明の目的を妨げない程度に着色したものを用いることもできる。
本発明に係る導電性層は、少なくとも(a)平均短軸長さが1nm以上150nm以下の金属導電性繊維、および(b)成分化合物、を含有する。
なお、前述の通り、前記(a)金属導電性繊維と(b)成分化合物とは、それぞれが別の層に添加されていてもよく、その場合には、(a)金属導電性繊維と(b)成分化合物とを含む本発明の導電性組成物を用いなくともよい。
金属導電性繊維の平均短軸長さおよび平均長軸長さの測定方法は既述の通りである。
本発明の導電性部材は、導電性層上に少なくとも水溶性ポリマーを含む可溶性保護層を有することも好ましい。前記可溶性保護層は、水溶性ポリマーを含有し、更に必要に応じてその他の成分を含有してなる。本発明の可用性保護層は、本発明に係る(b)成分化合物を含んでいてもよい。
前記水溶性ポリマーとしては、特に制限はなく、目的に応じて適宜選択することができ、例えばゼラチン、ゼラチン誘導体、ガゼイン、寒天、でんぷん、ポリビニルアルコール、ポリアクリル酸共重合体、カルボキシアルキルセルロース、水溶性セルロースエーテル等のセルロース誘導体、ポリビニルピロリドン、デキストラン、ポリアルキレングリコールなどが挙げられる。これらは、1種単独で使用してもよいし、2種以上を併用してもよい。これらの中でも、ポリビニルピロリドン、ポリビニルアルコール、及び水溶性セルロース誘導体が特に好ましい。
前記水溶性セルロース誘導体としては、例えばカルボキシメチルセルロース、ヒドロキシエチルセルロース、ヒドロキシプロピルメチルセルロースなどが挙げられる。
前記ポリアルキレングリコールとしては、例えば、ポリエチレングリコール、エチレングリコール/プロピレングリコール共重合体、などが挙げられ、重量平均分子量が、5,000~100,000のポリアルキレングリコールが好ましい。
ここで、前記可溶性保護層の平均厚みは、例えば走査型電子顕微鏡(SEM)による保護層断面の観察により測定することができる。
前記塗布法としては、特に制限はなく、目的に応じて適宜選択することができ、例えばロールコート法、バーコート法、ディップコーティング法、スピンコーティング法、キャスティング法、ダイコート法、ブレードコート法、バーコート法、グラビアコート法、カーテンコート法、スプレーコート法、ドクターコート法、などが挙げられる。
前記印刷法としては、例えば凸版(活版)印刷法、孔版(スクリーン)印刷法、平版(オフセット)印刷法、凹版(グラビア)印刷法、などが挙げられる。
前記可溶性保護層の除去は、導電性層のパターン形成時に行ってもよいし、ユーザー側においてパターン形成と共に行ってもよい。
前記水としては、特に制限はなく、目的に応じて適宜選択することができ、例えばイオン交換水、限外濾過水、逆浸透水、蒸留水等の純水、又は超純水などが挙げられる。
前記アルカリ溶液に含まれるアルカリとしては、特に制限はなく、目的に応じて適宜選択することができ、例えばテトラメチルアンモニウムヒドロキシド、テトラエチルアンモニウムヒドロキシド、2-ヒドロキシエチルトリメチルアンモニウムハイドロオキサイド、炭酸ナトリウム、炭酸水素ナトリウム、炭酸カリウム、炭酸水素カリウム、水酸化ナトリウム、水酸化カリウムなどが挙げられる。
前記水及びアルカリ溶液の浸漬時間は、特に制限はなく、目的に応じて適宜選択することができるが、10秒間~5分間であることが好ましい。
上記表面抵抗は、本発明に係る導電性部材における導電性層の基材側とは反対側の表面を四探針法)により測定された値である。四探針法による表面抵抗の測定方法は、例えばJIS K 7194:1994(導電性プラスチックの4探針法による抵抗率試験方法)などに準拠して測定することができ、市販の表面抵抗率計を用いて、簡便に測定することができる。表面抵抗を制御するには、導電性層に含まれる金属導電性繊維の種類および含有比率の少なくとも一つを調整すればよい。より具体的には、例えば、前記マトリックスと金属導電性繊維の含有比率を調製することにより、所望の範囲の表面抵抗を有する導電性層を形成することができる。
本発明に係る導電性部材は、ヘイズが10%以下であることが好ましく、5%以下であることが更に好ましく、2%以下であることが特に好ましい。
本発明の導電性部材の好ましい態様として、下記の3つの態様を挙げることができる。
第一の態様に係る導電性部材は、例えば、太陽電池の透明電極、電磁波シールド材、帯電防止材などに好ましく使用することができる。
第二の好ましい態様に係る導電性部材は、例えばタッチパネルや配線材料を作製する場合に使用される。この場合、所望の形状を有する導電性領域と非導電性領域が形成され、例えば、既存のITO透明導電膜で施されている電極形状が挙げられる。具体的には、国際公開第2005/114369号パンフレット、国際公開第2004/061808号パンフレット、特開2010-33478号公報、特開2010-44453号公報に開示されているストライプ形状のパターン、ダイヤモンドパターンと呼ばれているものなどが挙げられる。
第三の態様においては、導電性層の全領域が導電性(非パターン化導電性層)であっても、導電性領域と非導電性領域を有するパターン化導電性層であってもよい。非パターン化導電性層である場合の好ましい用途は、前述の本発明の第一の好ましい態様と同一であり、パターン化導電性層である場合の好ましい用途および形状は、前述の本発明の第二の好ましい態様と同一である。
本発明の第一の好ましい態様、および、第二の好ましい態様は、基材上に金属導電性繊維を含む導電性層を設けた導電性部材であり、前述の基材および、導電性層から、その目的に応じて任意の組合せを選択することができる。本発明においては、導電性層のマトリックスとして、前述のゾルゲル硬化物を使用することが好ましい。
(1)予め非パターン化導電性層を形成しておき、この非パターン化導電性層の所望の領域に含まれる金属導電性繊維に炭酸ガスレーザー、YAGレーザー等の高エネルギーのレーザー光線を照射して、金属導電性繊維の一部を断線または消失させて当該所望の領域を非導電性領域とするパターニング方法。この方法は、例えば、特開2010-4496号公報に記載されている。
また、(2)、(3)、(4)および(5)に記載の露光に用いる光源は、フォトレジスト組成物の感光波長域との関連で選定されるが、一般的にはg線、h線、i線、j線等の紫外線が好ましく用いられる。また、青色LEDを用いてもよい。
パターン露光の方法にも特に制限はなく、フォトマスクを利用した面露光で行ってもよいし、レーザービーム等による走査露光で行ってもよい。この際、レンズを用いた屈折式露光でも反射鏡を用いた反射式露光でもよく、コンタクト露光、プロキシミティー露光、縮小投影露光、反射投影露光などの露光方式を用いることができる。
前記塗布法としては、特に制限はなく、例えばロールコート法、バーコート法、ディップコーティング法、スピンコーティング法、キャスティング法、ダイコート法、ブレードコート法、バーコート法、グラビアコート法、カーテンコート法、スプレーコート法、ドクターコート法、などが挙げられる。
前記印刷法としては、例えば凸版(活版)印刷法、孔版(スクリーン)印刷法、平版(オフセット)印刷法、凹版(グラビア)印刷法、などが挙げられる。
前記希硝酸の濃度は、1質量%~20質量%であることが好ましい。
前記過酸化水素の濃度は、3質量%~30質量%であることが好ましい。
漂白定着時間は、180秒間以下が好ましく、120秒間以下1秒間以上がより好ましく、90秒間以下5秒間以上が更に好ましい。また、水洗または安定化時間は、180秒間以下が好ましく、120秒間以下1秒間以上がより好ましい。
前記漂白定着液としては、写真用漂白定着液であれば特に制限はなく、目的に応じて適宜選択することができ、例えば、富士フイルム株式会社製CP-48S、CP-49E(カラーペーパー用漂白定着剤)、コダック社製エクタカラーRA漂白定着液、大日本印刷株式会社製漂白定着液D-J2P-02-P2、D-30P2R-01、D-22P2R-01などが挙げられる。これらの中でも、CP-48S、CP-49Eが特に好ましい。
前記インクジェット印刷としては、例えばピエゾ方式およびサーマル方式のいずれも使用可能である。
また光ラジカル発生剤は単独で用いてもよいし、適宜溶剤による希釈やポリマーや増粘剤、無機微粒子を加えて塗布適性やインクジェット吐出適性、スクリーン印刷適性を付与し、または視認性を良くするために顔料や染料を添加して着色してもよい。
前記パターンの大きさとしては、特に制限はなく、目的に応じて適宜選択することができるが、ナノサイズからミリサイズのいずれの大きさであっても構わない。
本発明の第一の好ましい態様、および、第二の好ましい態様については、基材と導電性層との間に少なくとも一層の中間層を有することが好ましい。基材と導電性層との間に中間層を設けることにより、基材と導電性層との密着性、導電性層の全光線透過率、導電性層のヘイズ、および導電性層の膜強度のうちの少なくとも一つの向上を図ることが可能となる。
中間層としては、基材と導電性層との接着力を向上させるための接着剤層、導電性層に含まれる成分との相互作用により機能性を向上させる機能性層などが挙げられ、目的に応じて適宜設けられる。
また、導電性層と接する中間層(即ち、中間層が単層の場合には、当該中間層が、そして中間層が複数の層を含む場合には、そのうちの導電性層と接する中間層)が、当該導電性層に含まれる金属導電性繊維と相互作用可能な官能基を有する化合物を含む機能性層であることが、全光線透過率、ヘイズ、および膜強度に優れた導電性層が得られることから好ましい。このような中間層を有する場合においては、導電性層が金属導電性繊維とマトリックスとを含むものであっても、膜強度に優れた導電性層が得られる。
上記のような官能基を有する化合物としては、例えばウレイドプロピルトリエトキシシラン、ポリアクリルアミド、ポリ(N-メチルアクリルアミド)などのようなアミド基を有する化合物、例えばN-β(アミノエチル)γ-アミノプロピルトリメトキシシラン、3-アミノプロピルトリエトキシシラン、ビス(ヘキサメチレン)トリアミン、ポリ(2-アミノエチルアクリルアミド)などのようなアミノ基を有する化合物、例えば3-メルカプトプロピルトリメトキシシラン、2-メルカプトエチルトリメトキシシランなどのようなメルカプト基を有する化合物、例えばポリ(p-スチレンスルホン酸ナトリウム)、ポリ(アクリルアミド-2-メチルプロパンスルホン酸)などのようなスルホン酸またはその塩の基を有する化合物、例えばポリアクリル酸、ポリメタクリル酸、ポリアクリル酸部分ナトリウム塩などのようなカルボン酸基を有する化合物、例えば例えばポリ(2-ホスホノキシエチルメタクリラート)などのようなリン酸基を有する化合物、例えばポリビニルホスホン酸などのようなホスホン酸基を有する化合物が挙げられる。
これらの官能基を選択することで、導電性層形成用の塗布液を塗布後、金属導電性繊維と中間層に含まれる官能基とが相互作用を生じて、乾燥する際に金属導電性繊維が凝集するのを抑制し、金属導電性繊維が均一に分散された導電性層を形成することができる。
図2において、基材10と導電性層20との間に、前記第一の好ましい実施形態と同様の第1の接着層31および第2の接着層32に加え、導電性層20に隣接して機能性層33を備えて構成される中間層30を有する。本明細書における中間層30は、前記第1の接着層31、第2の接着層32、および、機能性層33から選択される少なくとも1層を含んで構成される層をさす。
上記導電性部材3は、該基材1上に、クッション層2と、金属導電性繊維を含有する導電性層3とをこの順に有してなり、更に必要に応じてその他の層を有してなる。
前記導電性部材は、可撓性を有し、透明であることが好ましく、前記「透明」には、無色透明のほか、有色透明、半透明、有色半透明などが含まれる。
第三の好ましい実施形態では、クッション層を有する。前記クッション層を有することで、導電性層が基材側の凹凸を跨いでも断線せず、凹凸追従性が向上する。前記クッション層の形状、構造、大きさ等については特に制限はなく、目的に応じて適宜選択することができ、例えば、前記形状としては、膜状、シート状などが挙げられる。前記構造としては、単層構造、積層構造などが挙げられる。前記大きさとしては、用途等に応じて適宜選択することができる。
前記クッション層は、被転写体との転写性を向上させる役割を果たす層であり、少なくともポリマーを含有し、更に必要に応じてその他の成分を含有してなる。
前記塗布方法としては、特に制限はなく、目的に応じて適宜選択することができ、例えばロールコート法、バーコート法、ディップコーティング法、スピンコーティング法、キャスティング法、ダイコート法、ブレードコート法、グラビアコート法、カーテンコート法、スプレーコート法、ドクターコート法、などが挙げられる。
本発明の導電性部材の製造方法は、基材上に、少なくとも、(a)平均短軸長さが1nm以上150nm以下の金属導電性繊維、(b)成分化合物、を含有する導電性層を形成できる方法であれば特に制限されない。好適な製造方法として下記(1)および(2)の2つの方法を挙げることができ、さらに下記(1)の方法は下記2つの製造方法を挙げることができる。下記(1-1)、(1-2)および(2)の方法は、いずれも、前記(a)成分である前記金属導電性繊維、(b)成分化合物および(c)成分であるマトリックスを含む導電性層を形成する。
(2)基材上に予め金属導電性繊維を含む層を形成し、この層を(b)成分化合物を含有する溶液に浸漬する。
(3)導電性層以外の別層に(b)成分化合物を予め添加し、導電性層を塗布・乾燥する際に、別層から導電性層に拡散させて導入する。
基材上に、(a)成分:金属導電性繊維40、(b)成分化合物50、および(c)成分:マトリックスを形成し得る重合性化合物60を含む導電性組成物を付与する。
この方法は、工程が簡略化されるという利点を有する。
基材上に、(a)成分:金属導電性繊維40および(b)成分化合物50を含む導電性組成物を付与し(図6(A))、ここに(c)成分:マトリックスを形成し得る重合性化合物60を含む液を付与する(図6(B))。
この方法は、(b)成分化合物が、(c)成分:マトリックスを形成し得る重合性化合物60を含む液に溶解しにくい場合に有効である。
基材上に、(a)成分:金属導電性繊維40を付与し(図7(A))、ここに(b)成分化合物50および(c)成分:マトリックスを形成し得る重合性化合物60を含む液を付与する(図7(B))。
この方法は、金属導電性繊維同士の接触抵抗が低くできるという点で優れる。
基材上に、(a)成分:金属導電性繊維40および(c)成分:マトリックスを形成し得る重合性化合物60を含む液を付与して第一層を形成し(図8(A))、別層として、その上に接して(b)成分化合物50を含有する第二層を形成し(図8(B))、第二層から第一層に(b)成分化合物50を拡散させる(図8(C))。
この方法は、b)成分化合物が金属導電性繊維の分散性や接触抵抗に影響する場合に、これらの影響を回避することができる点で優れる。
なお、図8では、別層は、第一層において基材10から遠い面側で接する層となっているが、第一層において基材10に近い面側で接する層であってもよい。
本発明に係る導電性部材は、例えば、表面型静電容量方式タッチパネル、投射型静電容量方式タッチパネル、抵抗膜式タッチパネルなどに適用される。ここで、タッチパネルとは、いわゆるタッチセンサおよびタッチパッドを含むものとする。
前記タッチパネルにおけるタッチパネルセンサー電極部の層構成が、2枚の透明電極を貼合する貼合方式、1枚の基材の両面に透明電極を具備する方式、片面ジャンパーあるいはスルーホール方式あるいは片面積層方式のいずれかであることが好ましい。
前記表面型静電容量方式タッチパネルについては、例えば特表2007-533044号公報に記載されている。
本発明に係る導電性部材は、集積型太陽電池(以下、太陽電池デバイスと称することもある)における透明電極としても有用である。集積型太陽電池としては、特に制限はなく、太陽電池デバイスとして一般的に用いられるものを使用することができる。例えば、単結晶シリコン系太陽電池デバイス、多結晶シリコン系太陽電池デバイス、シングル接合型、またはタンデム構造型等で構成されるアモルファスシリコン系太陽電池デバイス、ガリウムヒ素(GaAs)やインジウム燐(InP)等のIII-V族化合物半導体太陽電池デバイス、カドミウムテルル(CdTe)等のII-VI族化合物半導体太陽電池デバイス、銅/インジウム/セレン系(いわゆる、CIS系)、銅/インジウム/ガリウム/セレン系(いわゆる、CIGS系)、銅/インジウム/ガリウム/セレン/硫黄系(いわゆる、CIGSS系)等のI-III-VI族化合物半導体太陽電池デバイス、色素増感型太陽電池デバイス、有機太陽電池デバイスなどが挙げられる。
(b)[基材-導電性層]-光電変換層-[導電性層-基材]
(c)基材-電極-光電変換層-[導電性層-基材]
(d)裏面電極-光電変換層-[導電性層-基材]
このような太陽電池の詳細については、例えば特開2010-87105号公報に記載されている。
以下の例において、金属ナノワイヤーの平均直径(平均短軸長さ)および平均長軸長さ、並びに、平均短軸長さの変動係数は、以下のようにして測定した。
透過型電子顕微鏡(TEM;日本電子株式会社製、JEM-2000FX)を用いて拡大観察される金属ナノワイヤーから、ランダムに選択した300本の金属ナノワイヤーの直径(平均短軸長さ)と長軸長を測定し、その平均値から金属ナノワイヤーの平均直径(平均短軸長さ)および平均長軸長さ求めた。
上記電子顕微鏡(TEM)像からランダムに選択した300本の金属ナノワイヤーの平均短軸長さ(直径)を測定し、その300本についての標準偏差と平均値を計算することにより、求めた。
-銀ナノワイヤー分散液(1)の調製-
予め、下記の添加液A、B、C、及び、Dを調製した。
ステアリルトリメチルアンモニウムクロリド120mg、ステアリルトリメチルアンモニウムヒドロキシド10%水溶液12.0g、グルコース4.0gを蒸留水240.0gに溶解させ、反応溶液A-1とした。さらに、硝酸銀粉末140mgを蒸留水4.0gに溶解させ、硝酸銀水溶液A-1とした。反応溶液A-1を25℃に保ち、激しく攪拌しながら、硝酸銀水溶液A-1を添加した。硝酸銀水溶液A-1の添加後から180分間、激しい攪拌をし、添加液Aとした。
硝酸銀粉末42.0gを蒸留水958gに溶解した。
25%アンモニア水75gを蒸留水925gと混合した。
ポリビニルピロリドン(K30)400gを蒸留水1.6kgに溶解した。
―銀ナノワイヤー分散液(2)の調製―
調製例1において、添加液Aの代わりに蒸留水125.0gを使用したこと以外は調製例1と同様にして、金属含有量0.47%の銀ナノワイヤー分散液(2)を得た。
得られた銀ナノワイヤー分散液(2)の銀ナノワイヤーについて、前述のようにして平均短軸長、平均長軸長、銀ナノワイヤーの短軸長の変動係数、平均アスペクト比を測定した。その結果、平均短軸長47.0nm、平均長軸長13.0μm、変動係数が22.9%であった。平均アスペクト比は277であった。以後、「銀ナノワイヤー分散液(2)」と表記する場合は、上記方法で得られた銀ナノワイヤー分散液を示す。
-銀ナノワイヤー分散液(3)の調製-
プロピレングリコール370gに硝酸銀粉末60gを溶解させ、硝酸銀溶液301を調製した。プロピレングリコール4.45kgにポリビニルピロリドン(分子量55,000)72.0gを添加し、窒素ガスを容器の気相部分に通気しながら、90℃に昇温した。この液を反応溶液301とした。窒素ガスの通気を保持したまま、激しく攪拌している反応溶液301へ硝酸銀溶液301を2.55g添加して、加熱攪拌を1分間行った。さらに、この溶液へテトラブチルアンモニウムクロリド11.8gをプロピレングリコール100gに溶解させた溶液を添加し、反応溶液302とした。
得られた銀ナノワイヤー分散液(3)の銀ナノワイヤーについて、前述のようにして平均短軸長、平均長軸長、銀ナノワイヤーの短軸長の変動係数、平均アスペクト比を測定した。その結果、平均短軸長26.8nm、平均長軸長14.0μm、変動係数が17.9%であった。平均アスペクト比は522であった。以後、「銀ナノワイヤー分散液(3)」と表記する場合は、上記方法で得られた銀ナノワイヤー分散液を示す。
-ガラス基板の前処理-
厚み0.7μmの無アルカリガラス基板を、水酸化ナトリウムの1%水溶液に浸漬して超音波洗浄機によって30分超音波照射し、ついでイオン交換水で60秒間水洗した後、200℃で60分間加熱処理を行った。その後、シランカップリング液(N-β(アミノエチル)γ-アミノプロピルトリメトキシシランの0.3%水溶液、商品名:KBM603、信越化学工業(株)製)をシャワーにより20秒間吹き付け、更に、純水にてシャワー洗浄してガラス基板を得た。以後、「ガラス基板」と表記する場合は、上記前処理で得られた無アルカリガラス基板を示す。
-図1に示す構成を有するPET基板101の作製-
下記の配合で接着用溶液1を調製した。
(接着用溶液1)
・タケラックWS-4000 5.0部
(コーティング用ポリウレタン、固形分濃度30%、三井化学(株)製)
・界面活性剤 0.3部
(ナローアクティHN-100、三洋化成工業(株)製)
・界面活性剤 0.3部
(サンデットBL、固形分濃度43%、三洋化成工業(株)製)
・水 94.4部
(接着用溶液2)
・テトラエトキシシラン 5.0部
(KBE-04、信越化学工業(株)製)
・3-グリシドキシプロピルトリメトキシシラン 3.2部
(KBM-403、信越化学工業(株)製)
・2-(3,4-エポキシシクロヘキシル)エチルトリメトキシシラン 1.8部
(KBM-303、信越化学工業(株)製)
・酢酸水溶液(酢酸濃度=0.05%、pH=5.2) 10.0部
・硬化剤 0.8部
(ホウ酸、和光純薬工業(株)製)
・コロイダルシリカ 60.0部
(スノーテックスO、平均粒子径10nm~20nm、固形分濃度20%、pH=2.6、日産化学工業(株)製)
・界面活性剤 0.2部
(ナローアクティHN-100、三洋化成工業(株)製)
・界面活性剤 0.2部
(サンデットBL、固形分濃度43%、三洋化成工業(株)製)
(導電性部材1-1の作製)
下記組成のアルコキシシラン化合物を含有する溶液(以下、ゾルゲル溶液ともいう)を60℃で1時間撹拌して、均一になったことを確認した。
・テトラエトキシシラン(化合物(II)) 5.0部
(KBE-04、信越化学工業(株)製)
・1%酢酸水溶液 10.0部
・蒸留水 4.2部
導電性部材1-1の作製方法において、導電層塗布液調製時に化合物1-1を添加しなかったこと以外は導電性部材1-1の作製方法と同様にして、比較例である導電性部材1-2を作製した。
導電性部材1-1の作製方法において、添加する(b)成分化合物の種類および添加量(銀ナノワイヤー1gに対するmmolで表示)を、表1に記載の通りに代えたこと以外は導電性部材1-1の作製方法と同様にして、本発明の導電性部材1-3~1-18を作製した。
導電性部材1-1の作製方法において、(b)成分化合物に加えて、さらに一般式(3)~(11)で表される化合物を添加(表1に種類と添加量を記載)したこと以外は導電性部材1-1の作製方法と同様にして、本発明の導電性部材1-19~1-25を作製した。
導電性部材1-1の作製方法において、(b)成分化合物に加えて、さらに、本発明に係る金属に吸着可能な化合物、または金属イオンに配位可能な化合物として、下記化合物A-1~A-4を添加(表1に種類と添加量を記載)したこと以外は導電性部材1-1の作製方法と同様にして、本発明の導電性部材1-26~1-32を作製した。
導電性部材1-1の作製方法において、(b)成分化合物に加えて、さらに一般式(3)~(11)で表される化合物、および、本発明に係る金属に吸着可能な化合物、または金属イオンに配位可能な化合物として、上記化合物A-1~A-4を添加(表1に種類と添加量を記載)したこと以外は導電性部材1-1の作製方法と同様にして、本発明の導電性部材1-33~1-34を作製した。
導電性部材1-1の作製方法において、(b)成分化合物に代えて、本発明に係る金属に吸着可能な化合物、または金属イオンに配位可能な化合物として、上記化合物A-1~A-4を添加(表1に種類と添加量を記載)したこと以外は導電性部材1-1の作製方法と同様にして、比較例である導電性部材1-35~1-39を作製した。
導電性部材1-1の作製方法において、(b)成分化合物に代えて、下記比較用化合物C-1~C-4を添加(表1に種類と添加量を記載)したこと以外は導電性部材1-1の作製方法と同様にして、比較例である導電性部材1-40~1-43を作製した。
得られた各導電性部材に対し、以下の評価を行った。なお、光学特性の評価として、全光線透過率およびヘイズ値を下記測定方法にて実施し、耐候性の評価として、耐熱性、耐湿熱性および耐オゾン性を下記測定方法にて実施した。結果を表1に示す。
各導電性部材の表面抵抗値を、三菱化学株式会社製Loresta-GP MCP-T600を用いて測定した。測定は10cm×10cmのサンプルのランダムに選択した5箇所の導電性領域の中央部を測定し平均値を求めた。下記のランク付けを行った。
5:表面抵抗値 165Ω/□未満で、極めて優秀なレベル
4:表面抵抗値 165Ω/□以上、180Ω/□未満で、優秀なレベル
3:表面抵抗値 180Ω/□以上、200Ω/□未満で、許容レベル
2:表面抵抗値 200Ω/□以上、250Ω/□未満で、問題なレベル。
1:表面抵抗値 250Ω/□以上で、極めて問題なレベル。
評価用に5cm四方サイズのパターンを作製し、ランダムに選択した3箇所の導電性領域の中央部を測定し平均値を求めることにより、パターニング後の表面抵抗値として下記のランク付けを行なった。
5:表面抵抗値 165Ω/□未満で、極めて優秀なレベル
4:表面抵抗値 165Ω/□以上、180Ω/□未満で、優秀なレベル
3:表面抵抗値 180Ω/□以上、200Ω/□未満で、許容レベル
2:表面抵抗値 200Ω/□以上、250Ω/□未満で、問題なレベル。
1:表面抵抗値 250Ω/□以上で、極めて問題なレベル。
ストライプパターンまたは細線パターンにパターニングされた導電性部材の細線抵抗を、テスター(カスタム製、CDM-5000E)を用いて測定した。ストライプパターンについてはそれぞれの導電性部材に対し導電性ラインの抵抗値を5本ずつ測定し、平均値として求めた。細線パターンについては、ライン幅300μm長さ30mmのライン100本の抵抗を測定し、平均値を算出した。
各導電性部材の全光線透過率(%)をガードナー社製のヘイズガードプラスを用いて測定した。
なおパターニング後における導電部と非導電部の全光線透過率測定は以下手順で行った。実際の微細パターンの導電部および非導電部をヘイズメーターで測定するのは難しいため、実際の微細パターンと同サンプル中に評価用パターン(10mm□)を入れておき、導電部の全光線透過率を測定した。測定はC光源下のCIE視感度関数yについて、測定角0°で行い、10cm×10cmのサンプルのランダムに選択した5箇所の導電性領域の中央部を測定し平均値を求め、下記のランク付けを行った。
A:透過率90%以上で、良好なレベル
B:透過率85%以上90%未満で、やや問題なレベル
導電性部材の導電性領域に相当する部分のヘイズ値をガードナー社製のヘイズガードプラスを用いて測定した。測定は10cm×10cmのサンプルのランダムに選択した5箇所の導電性領域の中央部を測定し平均値を求めた。
なおパターニング後における導電部と非導電部のヘイズ値測定は以下手順で行った。実際の微細パターンの導電部および非導電部をヘイズメーターで測定するのは難しいため、実際の微細パターンと同サンプル中に評価用パターン(10mm□)を入れておき、導電部のヘイズ値を測定した。
各導電性部材に対し、アズワン(株)製ドライオーブンOFW-600を用いて180℃4時間、オーブンにて強制加熱処理を行った。加熱処理後の各導電性部材の表面抵抗値(RDT)を前述の方法によって測定し、加熱処理前の表面抵抗値(R0)に対する表面抵抗値の変化率(RDT/R0)を求めることにより、各導電性部材の耐熱性を評価し、下記のランク付けを行った。
なお、パターニングされた細線についてランク付けする場合は、前述の細線抵抗値の変化率で同様のランク付けを行った。
ランク5: 表面抵抗値の変化率 10%未満 非常に好ましいレベル
ランク4: 表面抵抗値の変化率 10%以上、20%未満 好ましいレベル
ランク3: 表面抵抗値の変化率 20%以上、35%未満 許容レベル
ランク2: 表面抵抗値の変化率 35%以上、50%未満 やや問題なレベル
ランク1: 表面抵抗値の変化率 50%以上 問題なレベル
各導電性部材に対し、エスペック(株)製小型環境試験機SH-241を用いて85℃85%RHの環境下で240時間放置することにより、強制湿熱処理を行った。強制湿熱処理前後の各導電性部材の表面抵抗値(RWT)を前述の方法によって測定し、強制湿熱処理前の表面抵抗値(R0)に対する変化率(RWT/R0)を求めることにより、各導電性部材の耐湿熱性を評価し、下記のランク付けを行った。
なお、パターニングされた細線についてランク付けする場合は、前述の細線抵抗値の変化率で同様のランク付けを行った。
ランク5: 表面抵抗値の変化率 10%未満 非常に好ましいレベル
ランク4: 表面抵抗値の変化率 10%以上、20%未満 好ましいレベル
ランク3: 表面抵抗値の変化率 20%以上、35%未満 許容レベル
ランク2: 表面抵抗値の変化率 35%以上、50%未満 やや問題なレベル
ランク1: 表面抵抗値の変化率 50%以上 問題なレベル
各導電性部材に対し、オゾン量15ppm、25℃の環境下に4時間暴露し、処理前後の各導電性部材の表面抵抗値(ROT)を前述の方法によって測定し、オゾン暴露前の表面抵抗値(R0)に対する変化率(ROT/R0)を求めることにより、各導電性部材の耐オゾン性を評価し、下記のランク付けを行った。
なお、パターニングされた細線についてランク付けする場合は、前述の細線抵抗値の変化率で同様のランク付けを行った。
ランク5: 表面抵抗値の変化率 100%以上、150%未満 非常に好ましいレベル
ランク4: 表面抵抗値の変化率 150%以上、200%未満 好ましいレベル
ランク3: 表面抵抗値の変化率 200%以上、350%未満 許容レベル
ランク2: 表面抵抗値の変化率 350%以上、500%未満 やや問題なレベル
ランク1: 表面抵抗値の変化率 500%以上 問題なレベル
-短軸長さ依存性の評価-
調製例1に記載の銀ナノワイヤー分散液の調製方法において、一段目の混合液の初期温度20℃を24℃に変更したこと以外は調製例1に記載の銀ナノワイヤー分散液の調製方法と同様にして、銀ナノワイヤー分散液を作製し、得られた銀ナノワイヤー分散液をAg-2とした。
また、調製例1の銀ナノワイヤー分散液の調製方法において、一段目の混合液の初期温度20℃を28℃に変更したこと以外は調製例1の銀ナノワイヤー分散液の調製方法と同様にして、銀ナノワイヤー分散液を作製し、得られた銀ナノワイヤー分散液をAg-3とした。
その結果、Ag-2に含まれる銀ナノワイヤーは、平均短軸長さ27.6nm、平均長軸長さ31.8μm、短軸長さの変動係数が25.2%であった。
また、Ag-3に含まれる銀ナノワイヤーは、平均短軸長さ33.6nm、平均長軸長さ28.8μm、短軸長さの変動係数が27.5%であった。
更に、実施例1の導電性部材1-1、1-2、および、1-8の作製方法において、銀ナノワイヤー分散液(1)に代えて調製例2の銀ナノワイヤー分散液(2)を用いたこと以外は導電性部材1-1、1-2、および、1-8の作製方法と同様にして、導電性部材2-7~2-9を作製し、銀ナノワイヤー分散液(1)に代えて調製例3の銀ナノワイヤー分散液(3)を用いたこと以外は導電性部材1-1、1-2、および、1-8の作製方法と同様にして導電性部材2-10~2-12を作製した。
得られた各導電性部材2-1~2-12に対して、実施例1と同様の評価を行い、得られた評価結果を表2に示した。また参考として、実施例1で得られた導電性部材1-1、1-2、および1-8の評価結果を併せて表2に示した。
すなわち、透明導電膜としてより好ましい光学特性を実現するためには、平均短軸長の短い(すなわち細い)銀ナノワイヤーを用いることが有効であり、その際に顕在化する耐熱性、耐湿熱性および耐オゾン性の改良手段として、本発明は特に有効であることがわかる。
-パターニング後の導電性部材の評価-
実施例1で得た導電性部材1-1に対し、以下の方法でパターニングを行った。まず、導電性部材1-1に、下記組成からなるポジレジスト(光可溶性組成物)を乾燥膜厚が2μmとなるようワイヤーバーコーターを用いて塗設した。90℃120秒間ホットプレート上でプリベイクを行った後、ストライプパターン(ライン/スペース=50μm/50μm)を有する露光マスクを介して、高圧水銀灯を用いて密着露光を施した。露光後の試料に対して後述の現像処理を施し、導電層上にライン/スペース=50μm/50μmからなるマスクレジストを形成した後、後述のエッチング処理工程を施すことによりマスクレジスト残存部以外の銀ナノワイヤーを溶解し、銀ナノワイヤーのストライプパターンを形成した。さらに、後述のポスト露光および剥離現像処理を施すことにより、マスクレジストを完全に溶解した。
(露光)
高圧水銀灯i線(365nm)にて強度150mJ/cm2(照度20mW/cm2)の条件で露光を行った。
0.4質量%のテトラメチルアンモニウムヒドロキシド(TMAH)水溶液(23℃)にてパドル現像を90秒間行い、露光部を除去した。次いで純水(23℃)にて90秒間水洗を行い、水洗後、室温にて試料を乾燥した。
下記エッチングAを用いて23℃90秒間エッチングを行い、さらに純水(23℃)にて90秒間水洗を行った。次いで純水(23℃)にて90秒間水洗を行い、水洗後、室温にて試料を乾燥した。
・エチレンジアミン四酢酸鉄(III)アンモニウム・・・・2.71g
・エチレンジアミン四酢酸二水素二ナトリウム二水和物・・・0.17g
・チオ硫酸アンモニウム(70質量%)・・・3.61g
・亜硫酸ナトリウム・・・0.84g
・氷酢酸・・・0.43g
・水を加えて全量1,000mL
高圧水銀灯i線(365nm)にて強度300mJ/cm2(照度20mW/cm2)の条件で露光を行った。
0.4質量%のTMAH水溶液(23℃)にてパドル現像を90秒間行い、露光部を除去した。次いで純水(23℃)にて90秒間水洗を行い、水洗後、室温にて試料を乾燥した。
・アクリル系バインダー(A-1) 固形分として 11.0質量部
・感光剤(東洋合成工業(株)製TAS-200) 6.2質量部
・EHPA-3150(ダイセル化学工業株式会社製) 5.2質量部
・密着促進剤(信越化学工業(株)製KBM-403) 0.1質量部
・溶剤 PGMEA 45.0質量部
・溶剤 MFG 32.5質量部
MFG:1-メトキシ-2-プロパノール
TAS-200:
共重合体を構成するモノマー成分としてメタクリル酸(MA(A)7.79g、ベンジルメタクリレート(BzM(A)37.21gを使用し、ラジカル重合開始剤としてアゾビスイソブチロニトリル(AIBN)0.5gを使用し、これらを溶剤プロピレングリコールモノメチルエーテルアセテート(PGME(A)55.00g中において重合反応させることにより、下記式で表されるバインダー(A-1)のPGMEA溶液(固形分濃度:45質量%)を得た。なお、重合温度は、温度60℃ないし100℃に調整した。
ゲル・パーミエイション・クロマトグラフィ法(GPC)を用いて測定した結果、ポリスチレン換算による重量平均分子量(Mw)は30,000、分子量分布(Mw/Mn)は2.21であった。
パターニングを施したこれらの導電性部材は、いずれも光学顕微鏡の観察の結果、ライン/スペース=50μm/50μm前後の良好な導電性パターンが形成されていることが確認された。
各試料に対し、実施例1の耐熱性評価と同様にして強制加熱処理(200℃60分間)を施し、強制加熱前後の抵抗値の比を抵抗上昇率として求め、抵抗値の測定を前記〔パターニングを施したあとの導電性部材の抵抗値〕に記載の方法で測定した以外は実施例1と同様にランク付けを行った。
各試料に対し、実施例1の耐オゾン性評価と同様の処理を施し、処理前後の表面抵抗値の変化率を求め、抵抗値の測定を前記〔パターニングを施したあとの導電性部材の抵抗値〕に記載の方法で測定した以外は実施例1と同様にランク付けを行った。
各試料に対し、実施例1の耐湿熱性評価と同様の処理を施し、処理前後の表面抵抗値の変化率を求め、抵抗値の測定を前記〔パターニングを施したあとの導電性部材の抵抗値〕に記載の方法で測定した以外は実施例1と同様にランク付けを行った。
実施例1の導電性部材1-1~1-43の作製方法において、PET基板101を調製例2で作製したガラス基板に代えたこと以外は導電性部材1-1~1-43の作製方法と同様にして導電性部材4-1~4-43を作製した。これらの導電性部材に対し実施例1と同様の評価を行った結果、(b)成分化合物を有さない導電性部材4-2に比べて、(b)成分化合物を有する本発明の導電性部材4-1、4-3~4-34はいずれも良好な耐候性(耐熱性および耐オゾン性)を示した。
比較例の導電性部材1-2を、化合物1-1、1-10、1-11または2-2の水溶液に5分間浸漬した後に流水で洗浄して、送風乾燥することにより、(b)成分化合物を導電性層に含有させた導電性部材5-2P~5-5Pを作製した。
また、上記導電性部材5-2Pの作製方法において、化合物1-1の水溶液を、化合物1-1又は1-10と化合物7-15との水溶液に代えたこと以外は導電性部材5-2Pの作製方法と同様にして、導電性部材5-6Pおよび5-7Pを作製した。
更に、上記導電性部材5-2Pの作製方法において、化合物1-1の水溶液を、化合物2-2と化合物7-23との水溶液に代えたこと以外は導電性部材5-2Pの作製方法と同様にして、導電性部材5-8Pを作製した。
なお、表4には、比較例の導電性部材1-2を導電性部材5-1Pとして、その評価結果も併記した。
導電性部材1-1、1-2、および1-8について、導電性層上に、下記組成の可溶性保護層用組成物を塗布し、乾燥させることで、平均厚み0.8μmの可溶性保護層を形成した。更に、実施例3と同様にしてパターニングを施し、導電性部材6-1P~6-9Pを作成した。これらの導電性部材について、実施例1と同様に評価を行った。結果を表5に示す。
・ポリビニルアルコール(PVA、PVA205(鹸化率=88%);株式会社クラレ製)・・・10g
・イオン交換水・・・90g
・ポリオキシエチレンラウリルエーテル(界面活性剤)・・・0.05g
・本発明の(b)成分化合物・・・表5に記載の種類と量
上記組成を混合し、撹拌して、可溶性保護層用組成物を調製した。
(フォトレジスト層を設けることによりパターニングされた導電性部材の調製)
-レジスト組成物(1)の調製-
下記組成となるように、それぞれの成分を加え、攪拌し、レジスト組成物(1)を調製した。
(レジスト組成物(1)の組成)
・実施例3で合成のバインダー(A-1)・・・3.80質量部(固形分40.0質量%、PGMEA溶液)
・感光性化合物としてのKAYARAD DPHA(日本化薬株式会社製)・・・1.59質量部
・光重合開始剤としてのIRGACURE379(チバ・スペシャルティ・ケミカルズ株式会社製)・・・0.159質量部
・架橋剤としてのEHPE-3150(ダイセル化学株式会社製)・・・0.150質量部
・メガファックF781F(DIC株式会社製)・・・0.002質量部
・PGMEA・・・19.3質量部
導電性部材1-1、1-2、および、1-8について、導電性層上に、上記で得られたレジスト組成物(1)を乾燥膜厚5μmとなるようバーコート法により塗布し、150℃のオーブンで5分間乾燥した。この基板に露光マスク上から、高圧水銀灯i線(365nm)を強度400mJ/cm2(照度50mW/cm2)で照射し、窒素雰囲気下で露光した。
露光後の基板を、35℃1%水酸化ナトリウム水溶液でシャワー現像60秒間を行った。シャワー圧は0.08MPa、ストライプパターンが出現するまでの時間は30秒であった。純水のシャワーでリンスした後、50℃で1分間乾燥し、レジストパターン付導電性部材7-1R、7-2R、および7-3Rを作製した。
また、露光マスクは、ベタ露光/未露光箇所、かつ細線パターン(L/S=300/300μm、電極長さ30mm)が形成可能な露光マスクを用いた。
上記レジストパターン付導電性部材7-1R、7-2R、および7-3Rを、CP-48S-A液と、CP-48S-B液(いずれも、富士フイルム株式会社製、カラーペーパー漂白定着剤)と、純水とを質量比で1:1:6となるように混合し、35℃に調整したエッチング液に2分間浸漬させてエッチング処理を行い、純水のシャワーでリンスした後、エアーナイフでサンプル表面の水を吹き飛ばし、60℃で5分間乾燥した。
エッチング後の基板を、35℃に保温した2.5%テトラメチルアンモニウムヒドロキシド水溶液でシャワー現像を75秒間行った。シャワー圧は3.0MPaであった。純水のシャワーでリンスした後、エアーナイフでサンプル表面の水を吹き飛ばし、60℃で5分間乾燥し、パターニングした導電性部材7-1P、7-2P、および7-3Pを作製した。得られた各導電性部材について、実施例3と同様の方法で表面抵抗、光学特性(全光線透過率、ヘイズ)を評価し、その結果を表6に示した。
-タッチパネルの作製-
実施例1の導電性部材1-1を用いて、『最新タッチパネル技術』(2009年7月6日発行、株式会社テクノタイムズ)、三谷雄二監修、“タッチパネルの技術と開発”、シーエムシー出版(2004年12月発行)、「FPD International 2009 Forum T-11講演テキストブック」、「Cypress Semiconductor Corporation アプリケーションノートAN2292」等に記載の方法により、タッチパネルを作製した。
作製したタッチパネルを使用した場合、光透過率の向上により視認性に優れ、かつ導電性の向上により素手、手袋を嵌めた手、指示具のうち少なくとも一つによる文字等の入力または画面操作に対し応答性に優れるタッチパネルを製作できることが分かった。
10 基材
20 導電性層
30 中間層
40 金属導電性繊維
50 (b)成分化合物
60 マトリックス
Claims (22)
- 少なくとも、
(a)平均短軸長が1nm以上150nm以下の金属導電性繊維、並びに
(b)下記一般式(1)で表される化合物および下記一般式(2)で表される化合物から選ばれる少なくとも1つの化合物、
を含有する導電性組成物。
一般式(2)において、R4およびR5は、各々独立にアルキル基を表す。R4およびR5は、二価以上の有機基または単結合を介して互いに連結してもよい。なお、一般式(2)で表される化合物は、R4およびR5の少なくとも一つから一個の水素原子を取り除いて一価の基となり、この一価の基が二価以上の有機基または単結合を介してR4およびR5の少なくとも一つと連結した、一般式(2)で表される構造が一分子中に複数存在する化合物を含む。〕 - さらに、(c)マトリックスを形成し得る重合性化合物を含む請求項1に記載の導電性組成物。
- 前記(c)マトリックスを形成し得る重合性化合物が、非感光性化合物である請求項2に記載の導電性組成物。
- 前記(c)マトリックスを形成し得る重合性化合物が、ゾルゲル硬化物を形成し得る化合物である請求項3に記載の導電性組成物。
- 前記(a)金属導電性繊維に対する前記(c)マトリックスを形成し得る重合性化合物の含有比率((c)/(a))が、質量比で0.001/1~100/1である請求項1~4のいずれか1項に記載の導電性組成物。
- 前記(b)一般式(1)で表される化合物および一般式(2)で表される化合物から選ばれる少なくとも1つの化合物が、前記(a)金属導電性繊維1g当たり、0.005mmol以上30mmol以下含まれる請求項1~請求項5のいずれか1項に記載の導電性組成物。
- 前記一般式(1)におけるR1およびR2の少なくとも一方が、アルコキシ基またはアリールオキシ基であり、R3がアリール基である請求項1~請求項6のいずれか1項に記載の導電性組成物。
- さらに、下記一般式(3)~(11)で表される化合物を少なくとも1種含む請求項1~請求項7のいずれか1項に記載の導電性組成物。
- 前記金属導電性繊維が、銀を50モル%以上100モル%以下含む請求項1~請求項8のいずれか1項に記載の導電性組成物。
- 前記金属導電性繊維の平均短軸長が1nm以上30nm以下である請求項1~請求項9のいずれか1項に記載の導電性組成物。
- 基材と、前記基材上に設けられた請求項1~請求項10のいずれか1項に記載の導電性組成物から形成される導電性層と、を有する導電性部材。
- さらに、前記導電性層上に少なくとも水溶性ポリマーを含む可溶性保護層を有する請求項11に記載の導電性部材。
- 前記導電性層における表面抵抗が、1Ω/□以上1000Ω/□以下である請求項11または請求項11に記載の導電性部材。
- 前記導電性層が、導電性領域および非導電性領域を含む請求項11~請求項13のいずれか1項に記載の導電性部材。
- 前記基材と前記導電性層との間に、更に少なくとも一層の中間層を有する請求項11~請求項14のいずれか1項に記載の導電性部材。
- 請求項11~請求項15のいずれか1項に記載の導電性部材を含むタッチパネル。
- 請求項11~請求項15のいずれか1項に記載の導電性部材を含む太陽電池。
- 基材上に、
少なくとも、(a)平均短軸長が1nm以上150nm以下の金属導電性繊維、並びに、(b)下記一般式(1)で表される化合物および下記一般式(2)で表される化合物から選ばれる少なくとも1つの化合物、を含有する請求項1に記載の導電性組成物を用いて、導電性層を形成する導電性層の形成工程を含む導電性部材の製造方法。
一般式(2)において、R4およびR5は、各々独立にアルキル基を表す。R4およびR5は、二価以上の有機基または単結合を介して互いに連結してもよい。なお、一般式(2)で表される化合物は、R4およびR5の少なくとも一つから一個の水素原子を取り除いて一価の基となり、この一価の基が二価以上の有機基または単結合を介してR4およびR5の少なくとも一つと連結した、一般式(2)で表される構造が一分子中に複数存在する化合物を含む。〕 - 前記導電性層の形成工程は、基材上に、(a)平均短軸長が1nm以上150nm以下の金属導電性繊維、並びに、前記(b)一般式(1)で表される化合物および一般式(2)で表される化合物から選ばれる少なくとも1つの化合物、を含有する導電性組成物を付与した後に、
(c)マトリックスを付与して、
前記(a)成分、前記(b)成分および前記(c)成分を含む導電性層を形成する、請求項18に記載の導電性部材の製造方法。 - 前記導電性層の形成工程は、基材上に、(a)平均短軸長が1nm以上150nm以下の金属導電性繊維、前記(b)一般式(1)で表される化合物および一般式(2)で表される化合物から選ばれる少なくとも1つの化合物、並びに、(c)マトリックスを含有する導電性組成物を付与して、
前記(a)成分、前記(b)成分および前記(c)成分を含む導電性層を形成する、請求項18に記載の導電性部材の製造方法。 - 基材上に、(a)平均短軸長が1nm以上150nm以下の金属導電性繊維を付与した後、
(b)下記一般式(1)で表される化合物および下記一般式(2)で表される化合物から選ばれる少なくとも1つの化合物、並びに(c)マトリックスを含有する組成物を付与して、
前記(a)成分、(b)成分および(c)成分を含む導電性層を形成する、導電性部材の製造方法。
一般式(2)において、R4およびR5は、各々独立にアルキル基を表す。R4およびR5は、二価以上の有機基または単結合を介して互いに連結してもよい。なお、一般式(2)で表される化合物は、R4およびR5の少なくとも一つから一個の水素原子を取り除いて一価の基となり、この一価の基が二価以上の有機基または単結合を介してR4およびR5の少なくとも一つと連結した、一般式(2)で表される構造が一分子中に複数存在する化合物を含む。〕 - 前記請求項11~請求項15のいずれか1項に記載の、前記基材と前記導電性層とを有する前記導電性部材に、フォトレジスト層を設ける工程と、
前記フォトレジスト層をパターン状に露光し現像して、パターン状のフォトレジスト層を形成する工程と、
前記パターン状のフォトレジスト層を介して、前記導電性層をエッチングする工程と、
を少なくとも有する、パターン化導電性層を有する導電性部材の製造方法。
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KR20140129206A (ko) | 2014-11-06 |
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US20150013763A1 (en) | 2015-01-15 |
CN104205244B (zh) | 2016-04-27 |
CN104205244A (zh) | 2014-12-10 |
US9224518B2 (en) | 2015-12-29 |
KR101662418B1 (ko) | 2016-10-04 |
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