WO2013094636A1 - Particules conductrices, matériau conducteur et structure de connexion - Google Patents

Particules conductrices, matériau conducteur et structure de connexion Download PDF

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Publication number
WO2013094636A1
WO2013094636A1 PCT/JP2012/082910 JP2012082910W WO2013094636A1 WO 2013094636 A1 WO2013094636 A1 WO 2013094636A1 JP 2012082910 W JP2012082910 W JP 2012082910W WO 2013094636 A1 WO2013094636 A1 WO 2013094636A1
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WIPO (PCT)
Prior art keywords
conductive layer
particles
conductive
particle
core
Prior art date
Application number
PCT/JP2012/082910
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English (en)
Japanese (ja)
Inventor
敬三 西岡
Original Assignee
積水化学工業株式会社
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 積水化学工業株式会社 filed Critical 積水化学工業株式会社
Priority to CN201810695985.2A priority Critical patent/CN108806824B/zh
Priority to JP2012558095A priority patent/JP6049461B2/ja
Priority to CN201280040642.3A priority patent/CN103748636A/zh
Priority to KR1020137029906A priority patent/KR101942602B1/ko
Publication of WO2013094636A1 publication Critical patent/WO2013094636A1/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20—Conductive material dispersed in non-conductive organic material
    • H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/18—Non-metallic particles coated with metal
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/52—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating using reducing agents for coating with metallic material not provided for in a single one of groups C23C18/32 - C23C18/50
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
    • H01B5/16—Non-insulated conductors or conductive bodies characterised by their form comprising conductive material in insulating or poorly conductive material, e.g. conductive rubber
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
    • H01R11/00—Individual connecting elements providing two or more spaced connecting locations for conductive members which are, or may be, thereby interconnected, e.g. end pieces for wires or cables supported by the wire or cable and having means for facilitating electrical connection to some other wire, terminal, or conductive member, blocks of binding posts
    • H01R11/01—Individual connecting elements providing two or more spaced connecting locations for conductive members which are, or may be, thereby interconnected, e.g. end pieces for wires or cables supported by the wire or cable and having means for facilitating electrical connection to some other wire, terminal, or conductive member, blocks of binding posts characterised by the form or arrangement of the conductive interconnection between the connecting locations
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601—Process or apparatus
    • C23C18/1633—Process of electroless plating
    • C23C18/1655—Process features
    • C23C18/1662—Use of incorporated material in the solution or dispersion, e.g. particles, whiskers, wires
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/31—Coating with metals
    • C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron

Definitions

  • the present invention relates to conductive particles in which a conductive layer is disposed on the surface of base particles, and more particularly to conductive particles that can be used for electrical connection between electrodes, for example.
  • the present invention also relates to a conductive material and a connection structure using the conductive particles.
  • Anisotropic conductive materials such as anisotropic conductive paste and anisotropic conductive film are widely known.
  • anisotropic conductive material conductive particles are dispersed in a binder resin.
  • the anisotropic conductive material is used for connection between an IC chip and a flexible printed circuit board, connection between an IC chip and a circuit board having an ITO electrode, and the like. For example, after disposing an anisotropic conductive material between the electrode of the IC chip and the electrode of the circuit board, these electrodes can be electrically connected by heating and pressing.
  • Patent Document 1 discloses a conductive material in which a nickel conductive layer or a nickel alloy conductive layer is formed on the surface of spherical base particles having an average particle diameter of 1 to 20 ⁇ m by an electroless plating method. Sex particles are disclosed. The conductive particles have minute protrusions of 0.05 to 4 ⁇ m on the outermost layer of the conductive layer. The conductive layer and the protrusion are substantially continuously connected.
  • Patent Document 2 a plastic core, a polymer electrolyte layer covering the plastic core, metal particles adsorbed on the plastic core through the polymer electrolyte layer, and the metal particles are covered.
  • surroundings of the said plastic core is disclosed.
  • Patent Document 3 discloses conductive particles in which a multilayer conductive layer of a metal plating film layer containing nickel and phosphorus and a gold layer is formed on the surface of a base material particle.
  • a core substance is disposed on the surface of the base particle, and the core substance is covered with a conductive layer.
  • the conductive layer is raised by the core material, and protrusions are formed on the surface of the conductive layer.
  • Patent Documents 1 to 3 described above disclose conductive particles having protrusions on the outer surface of the conductive layer.
  • an oxide film is formed on the surfaces of the electrodes connected by the conductive particles and the conductive layer of the conductive particles.
  • the protrusion of the conductive layer is formed so as to contact the conductive layer and the electrode by eliminating the oxide film on the surface of the electrode and the conductive particle when the electrodes are pressure-bonded via the conductive particle. .
  • the oxide film on the surfaces of the electrodes and the conductive particles cannot be sufficiently eliminated, and the connection resistance is high. May be.
  • An object of the present invention is to provide conductive particles capable of reducing the connection resistance between electrodes when a connection structure is obtained by connecting electrodes, and a conductive material and connection structure using the conductive particles. Is to provide.
  • the method includes a base particle, a conductive layer covering the base particle, and a plurality of core substances embedded in the conductive layer, wherein the conductive layer is outside.
  • a plurality of protrusions on the surface, the core substance is disposed inside the protrusions of the conductive layer, the conductive layer is disposed between the base material particles and the core substance, and the base Conductive particles are provided in which the surface of the material particles and the surface of the core substance are separated from each other, and the average distance between the surface of the base material particles and the surface of the core substance exceeds 5 nm.
  • an average distance between the surface of the base material particle and the surface of the core substance is more than 5 nm and 800 nm or less.
  • the total number of the core materials is 100%, and the distance between the surface of the base material particles and the surface of the core material is more than 5 nm.
  • the ratio is more than 80% and not more than 100%.
  • the metal element contained most in the core material and the metal element contained most in the conductive layer are the same.
  • the conductive layer covers the first conductive layer covering the base particle, the first conductive layer, and the core substance.
  • the core material is disposed on the surface of the first conductive layer and embedded in the second conductive layer, and the second conductive layer.
  • Has a plurality of protrusions on the outer surface the core substance is disposed inside the protrusions of the second conductive layer, and the first substance is interposed between the base particle and the core substance.
  • a conductive layer is disposed.
  • the metal element contained most in the core material and the metal element contained most in the second conductive layer are the same.
  • the conductive layer is a single conductive layer.
  • the core substance is a metal particle.
  • an insulating material attached to the surface of the conductive layer is further provided.
  • the conductive material according to the present invention includes the above-described conductive particles and a binder resin.
  • connection structure includes a first connection target member, a second connection target member, and a connection portion connecting the first and second connection target members, and the connection
  • the part is formed of the above-described conductive particles, or is formed of a conductive material containing the conductive particles and a binder resin.
  • the conductive particle according to the present invention includes a base particle, a conductive layer covering the base particle, and a plurality of core substances embedded in the conductive layer. Protrusions on the outer surface, the core substance is disposed inside the protrusions of the conductive layer, the conductive layer is disposed between the substrate particles and the core substance, and the base The surface of the material particles and the surface of the core substance are separated from each other, and the average distance between the surface of the base material particles and the surface of the core substance exceeds 5 nm. When used for connection between electrodes, the connection resistance between the electrodes can be lowered.
  • FIG. 1 is a cross-sectional view showing conductive particles according to the first embodiment of the present invention.
  • FIG. 2 is a cross-sectional view showing conductive particles according to the second embodiment of the present invention.
  • FIG. 3 is a cross-sectional view showing conductive particles according to the third embodiment of the present invention.
  • FIG. 4 is a front cross-sectional view schematically showing a connection structure using conductive particles according to the first embodiment of the present invention.
  • the conductive particles according to the present invention include base particles, a conductive layer covering the base particles, and a plurality of core substances embedded in the conductive layer.
  • the conductive layer has a plurality of protrusions on the outer surface.
  • the core substance is disposed inside the protrusion of the conductive layer.
  • the conductive layer is disposed between the base particle and the core substance.
  • a partial region of the conductive layer is disposed between the base particle and the core substance.
  • the surface of the base particle and the surface of the core substance are separated from each other.
  • the average distance between the surface of the substrate particle and the surface of the core substance is more than 5 nm.
  • An oxide film is often formed on the surface of the electrode connected by the conductive particles. Furthermore, an oxide film is often formed on the outer surface of the conductive layer.
  • the oxide film is eliminated by the protrusions by placing the conductive particles between the electrodes and then pressing them. For this reason, an electrode and electroconductive particle can be made to contact and the connection resistance between electrodes can be made low.
  • the conductive layer is disposed between the base particle and the core substance, and the surface of the base particle and the surface of the core substance are spaced apart from each other.
  • the core material is difficult to push the base material particle when the conductive particles are compressed between the electrodes. A part of the region is difficult to sink into the base particle.
  • the base particles are relatively soft resin particles
  • the core substance is difficult to push the base particles, and a part of the core substance is difficult to sink into the base particles.
  • the protrusions of the conductive layer are strongly pressed against the electrodes during pressure bonding between the electrodes. As a result, the oxide film is effectively eliminated by the protrusions. For this reason, an electrode and electroconductive particle can be made to contact effectively and the connection resistance between electrodes can be made low effectively.
  • the conductive particles according to the present invention have the above-described configuration, when the conductive particles are compressed to connect the electrodes, it is possible to form an appropriate indentation on the electrodes.
  • the indentation formed on the electrode is a concave portion of the electrode formed by pressing the electrode with conductive particles.
  • a conductive material such as anisotropic conductive material
  • the binder resin between the conductive layer and the electrode is effectively eliminated. it can.
  • the connection resistance between the electrodes can also be lowered by effectively eliminating the binder resin.
  • conductive particles including an insulating material are used, the insulating material between the conductive layer and the electrode can be effectively eliminated by the protrusions, so that the conduction reliability between the electrodes is effectively increased. Can do.
  • the average between the surface of the base particle and the surface of the core substance The distance is preferably 5 nm or more, more preferably 10 nm or more.
  • the upper limit of the average distance between the surface of the substrate particle and the surface of the core substance is not particularly limited, and is appropriately determined in consideration of the thickness of the conductive layer.
  • the average distance between the surface of the base material particle and the surface of the core substance may be 800 nm or less, or 100 nm or less.
  • the average distance between the surface of the base material particle and the surface of the core substance is preferably 30 nm or less, more preferably 20 nm or less.
  • the average distance between the surface of the base material particle and the surface of the core substance may be 9/10 or less, 1/2 or less, or 1/3 or less of the thickness of the conductive layer. There may be.
  • the surface of the base particle in the total number of 100% of the core substance is preferably 50% or more, more preferably more than 80% and 100% or less. In all of the core materials, the distance between the surface of the base particle and the surface of the core material may exceed 5 nm.
  • the average distance between the surface of the base particle and the surface of the core substance is measured after measuring the distance (the shortest distance between the gaps) between the surface of the base particle and each surface of the plurality of core substances. It is calculated by averaging the obtained values.
  • the conductive particles include five core materials A to E embedded in the conductive layer, the distance between the surface of the base material particle and the surface of the core material A, the surface of the base material particle and the core material B
  • the distance between the surface, the distance between the surface of the base material particle and the surface of the core material C, the distance between the surface of the base material particle and the surface of the core material D, the surface of the base material particle and the surface of the core material E Is calculated by averaging the five measured values.
  • the number of core materials is 10 or more, it is preferable to measure the distance between the surface of the base material particles and each surface of all the core materials. The distance from each surface of the core material may be measured, and the average distance may be calculated from the 10 measured values.
  • the distance between the surface of the base material particle and the surface of the core substance was obtained by photographing a plurality of cross-sections of the conductive particles to obtain an image, and creating a stereoscopic image from the obtained image. By using a stereoscopic image, it can be measured accurately.
  • the section can be imaged using a focused ion beam-scanning electron microscope (FIBSEM) or the like. For example, a thin film slice of conductive particles is prepared using a focused ion beam, and the cross section is observed with a scanning electron microscope. A three-dimensional image of the particles can be obtained by repeating the operation several hundred times and analyzing the image.
  • FIBSEM focused ion beam-scanning electron microscope
  • the conductive layer has protrusions on the outer surface. There are a plurality of protrusions. An oxide film is often formed on the surface of the conductive layer and the surface of the electrode connected by the conductive particles. By using conductive particles having protrusions on the outer surface of the conductive layer, the oxide particles are effectively eliminated by the protrusions by placing the conductive particles between the electrodes and pressing them. For this reason, an electrode and the conductive layer of electroconductive particle can be contacted still more reliably, and the connection resistance between electrodes can be made low.
  • the conductive particles are provided with an insulating material on the surface, or when the conductive particles are dispersed in a binder resin and used as a conductive material, the protrusions of the conductive particles cause a gap between the conductive particles and the electrode. Insulating substances or binder resins can be effectively eliminated. For this reason, the conduction
  • the average height of the plurality of protrusions is preferably 0.001 ⁇ m or more, more preferably 0.05 ⁇ m or more, preferably 0.9 ⁇ m or less, more preferably 0.2 ⁇ m or less.
  • the connection resistance between the electrodes can be effectively lowered.
  • FIG. 1 is a cross-sectional view showing conductive particles according to the first embodiment of the present invention.
  • the conductive layer 3 is disposed on the surface of the base particle 2.
  • a single conductive layer 3 is formed.
  • the conductive layer 3 covers the base particle 2.
  • the conductive layer 3 has a plurality of protrusions 3a on the outer surface.
  • the plurality of core substances 4 are arranged on the surface of the base particle 2 and are embedded in the conductive layer 3.
  • the core substance 4 is disposed inside the protrusion 3a.
  • One core material 4 is arranged inside one protrusion 3a.
  • the outer surface of the conductive layer 3 is raised by the plurality of core materials 4, and a plurality of protrusions 3 a are formed.
  • the conductive layer 3 is disposed between the surface of the base particle 2 and the surface of the core substance 4.
  • the surface of the base particle 2 and the surface of the core material 4 are separated from each other.
  • the core substance 4 is not in contact with the base particle 2.
  • the average distance between the surface of the base material particle 2 and the surface of the core substance 4 exceeds 5 nm.
  • the conductive layer 3 part (conductive layer part 3b) of sufficient thickness is arrange
  • the distance between the surface of the base material particle 2 and the surface of the core material 4 is the thickness of the conductive layer portion 3 b disposed between the surface of the base material particle 2 and the surface of the core material 4.
  • the insulating material 5 is disposed on the surface of the conductive layer 3.
  • the insulating material 5 is an insulating particle.
  • the insulating substance 5 is made of an insulating material.
  • the conductive particles do not necessarily include an insulating substance.
  • the conductive particles may include an insulating layer that covers the outer surface of the conductive layer instead of the insulating particles as an insulating substance.
  • FIG. 2 is a cross-sectional view showing conductive particles according to the second embodiment of the present invention.
  • the conductive layer 2 includes a base particle 2, a conductive layer 12, a plurality of core substances 4, and an insulating substance 5.
  • the conductive layer 12 is disposed on the surface of the base particle 2.
  • the conductive layer 12 covers the base particle 2.
  • the conductive layer 12 has a plurality of protrusions 12a on the outer surface.
  • a multilayer conductive layer 12 is formed.
  • the conductive layer 12 includes a first conductive layer 16 and a second conductive layer 17.
  • the first conductive layer 16 is disposed on the surface of the base particle 2.
  • the first conductive layer 16 covers the base particle 2.
  • the first conductive layer 16 is a single layer.
  • the first conductive layer may be a multilayer.
  • the core material 4 is disposed on the first conductive layer 16.
  • the core material 4 is embedded in the conductive layer 12 and the second conductive layer 17.
  • a first conductive layer 16 is disposed between the base particle 2 and the core substance 4.
  • the distance between the surface of the base material particle 2 and the surface of the core material 4 is such that the conductive layer portion 12 b disposed between the surface of the base material particle 2 and the surface of the core material 4 and It is the thickness of the 1st conductive layer 16 (1st conductive layer 16 part).
  • the second conductive layer 17 is formed separately from the first conductive layer 16.
  • the second conductive layer 17 is formed on the surface of the first conductive layer 16 after the first conductive layer 16 is formed.
  • the second conductive layer 17 is disposed on the surface of the first conductive layer 16.
  • the second conductive layer 17 covers the core material 4 and the first conductive layer 16.
  • the second conductive layer 17 has a plurality of protrusions 17a on the outer surface.
  • the plurality of core materials 4 are embedded in the second conductive layer 17.
  • the core substance 4 is disposed inside the protrusion 17a.
  • the outer surface of the second conductive layer 17 is raised by the plurality of core materials 4 to form protrusions 17a.
  • FIG. 3 is a cross-sectional view showing conductive particles according to the third embodiment of the present invention.
  • the 3 includes a base particle 2, a conductive layer 22, a plurality of core materials 4, and an insulating material 5.
  • the conductive layer 22 is disposed on the surface of the base particle 2.
  • the conductive layer 22 covers the base particle 2.
  • the conductive layer 22 has a plurality of protrusions 22a on the outer surface.
  • a multilayer conductive layer 22 is formed.
  • the conductive layer 22 includes a first conductive layer 26, a second conductive layer 27, and a third conductive layer 28.
  • the first conductive layer 26 is disposed on the surface of the base particle 2.
  • the first conductive layer 26 covers the base particle 2.
  • the core material 4 is disposed on the first conductive layer 26.
  • the core material 4 is embedded in the conductive layer 22 and the second conductive layer 27.
  • a first conductive layer 26 is disposed between the base particle 2 and the core substance 4.
  • the average distance between the surface of the base particle 2 and the surface of the core substance 4 exceeds 5 nm.
  • the distance between the surface of the base material particle 2 and the surface of the core material 4 is such that the conductive layer portion 22 b disposed between the surface of the base material particle 2 and the surface of the core material 4 and This is the thickness of the first conductive layer 26 portion.
  • the second conductive layer 27 is disposed on the surface of the first conductive layer 26.
  • the second conductive layer 27 covers the core material 4 and the first conductive layer 26.
  • the second conductive layer 27 has a plurality of protrusions 27a on the outer surface.
  • the core substance 4 is disposed inside the protrusion 27a.
  • the outer surface of the second conductive layer 27 is raised by the plurality of core materials 4, and protrusions 27 a are formed.
  • the third conductive layer 28 is disposed on the surface of the second conductive layer 27.
  • the third conductive layer 28 covers the second conductive layer 27.
  • the third conductive layer 28 has a plurality of protrusions 28a on the outer surface.
  • the core substance 4 is disposed inside the protrusion 28a.
  • the outer surface of the third conductive layer 28 is raised by the plurality of core materials 4 to form protrusions 28a.
  • the metal element contained most in the core material and the metal element contained most in the conductive layer are the same.
  • the connection resistance in the connection structure is further improved.
  • the metal element contained most in the core substance and the metal element contained most in the conductive layer are the core substance, the conductive layer, or the core substance and the conductive layer. There may be a concentration gradient.
  • the metal element contained most in the core substance and the metal element contained most in the conductive layer may be alloyed with other metals.
  • the metal contained in the core material and the metal contained in the conductive layer may be alloyed at the interface.
  • the metal element contained most in the core material and the metal element contained most in the first conductive layer are the same.
  • the connection resistance in the connection structure is further improved.
  • the metal element contained most in the core material and the metal element contained most in the first conductive layer are the core material, the first conductive layer, or the core material and the above-described core material. There may be a concentration gradient in the first conductive layer.
  • the metal element contained most in the first conductive layer may be alloyed with another metal.
  • the metal contained in the core material and the metal contained in the first conductive layer may be alloyed at the interface.
  • the metal element contained most in the core material and the metal element contained most in the second conductive layer are the same.
  • the connection resistance in the connection structure is further improved.
  • the metal element contained most in the core material and the metal element contained most in the second conductive layer are the core material, the second conductive layer, or the core material and the above-described core material. There may be a concentration gradient in the second conductive layer.
  • the metal element contained most in the second conductive layer may be alloyed with another metal.
  • the metal contained in the core material and the metal contained in the second conductive layer may be alloyed at the interface.
  • the Mohs hardness of the core material is the same as the Mohs hardness of the conductive layer portion disposed between the base material particles and the core material, or the Mohs hardness of the core material is equal to the base material particles and the core material. It is preferable that it is larger than the Mohs hardness of the conductive layer part arrange
  • the Mohs hardness of the core material is preferably the same as the Mohs hardness of the first conductive layer, or the Mohs hardness of the core material is preferably larger than the Mohs hardness of the first conductive layer. In such a case, the core material is difficult to push the base material particles, and a part of the core material is difficult to sink into the base material particles.
  • the connection resistance between the electrodes can be further reduced.
  • the Mohs hardness of the core substance is determined by the conductive layer portion disposed between the base material particles and the core substance or the Mohs of the first conductive layer. It is preferable that it is larger than the hardness.
  • the connection resistance is further increased.
  • the absolute value of the difference between the Mohs hardness of the core material and the Mohs hardness of the conductive layer portion or the first conductive layer disposed between the base particle and the core material is: Preferably it is 0.1 or more, More preferably, it is 0.5 or more.
  • the Mohs hardness of the core substance is preferably smaller than the Mohs hardness of the conductive layer portion disposed between the base material particles and the core substance.
  • the Mohs hardness of the core material is preferably smaller than the Mohs hardness of the first conductive layer.
  • the conductive layer portion and the first conductive layer have some cushioning properties.
  • the impact resistance is further enhanced.
  • the absolute value of the difference between the Mohs hardness of the core material and the Mohs hardness of the conductive layer portion or the first conductive layer disposed between the base particle and the core material is preferably 0.1 or more, more preferably 0.5 or more.
  • Examples of the substrate particles include resin particles, inorganic particles excluding metals, organic-inorganic hybrid particles, and metal particles.
  • the substrate particles are preferably substrate particles excluding metal particles, and more preferably resin particles, inorganic particles excluding metal, or organic-inorganic hybrid particles.
  • the base material particles are preferably resin particles formed of a resin.
  • the substrate particles are resin particles, the effect of reducing the connection resistance obtained by the configuration of the conductive layer and the core substance of the present invention is considerably increased.
  • the said electroconductive particle is compressed by crimping
  • the substrate particles are resin particles, the conductive particles are easily deformed during the pressure bonding, and the contact area between the conductive particles and the electrode is increased. For this reason, the conduction
  • the resin for forming the resin particles include polyolefin resins such as polyethylene, polypropylene, polystyrene, polyvinyl chloride, polyvinylidene chloride, polypropylene, polyisobutylene, and polybutadiene; acrylic resins such as polymethyl methacrylate and polymethyl acrylate.
  • polyolefin resins such as polyethylene, polypropylene, polystyrene, polyvinyl chloride, polyvinylidene chloride, polypropylene, polyisobutylene, and polybutadiene
  • acrylic resins such as polymethyl methacrylate and polymethyl acrylate.
  • Resin for forming the resin particles can be designed and synthesized, and the hardness of the base particles can be easily controlled within a suitable range, which is suitable for conductive materials and having physical properties at the time of compression.
  • the monomer having an ethylenically unsaturated group includes a non-crosslinkable monomer and a crosslinkable monomer. And so on.
  • non-crosslinkable monomer examples include styrene monomers such as styrene and ⁇ -methylstyrene; carboxyl group-containing monomers such as (meth) acrylic acid, maleic acid, and maleic anhydride; (Meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, butyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, lauryl (meth) acrylate, cetyl (meth) acrylate, stearyl (meth) acrylate, cyclohexyl ( Alkyl (meth) acrylates such as meth) acrylate and isobornyl (meth) acrylate; acids such as 2-hydroxyethyl (meth) acrylate, glycerol (meth) acrylate, polyoxyethylene (meth) acrylate and glycidyl (meth) acrylate Atom
  • crosslinkable monomer examples include tetramethylolmethane tetra (meth) acrylate, tetramethylolmethane tri (meth) acrylate, tetramethylolmethane di (meth) acrylate, trimethylolpropane tri (meth) acrylate, and dipenta Erythritol hexa (meth) acrylate, dipentaerythritol penta (meth) acrylate, glycerol tri (meth) acrylate, glycerol di (meth) acrylate, (poly) ethylene glycol di (meth) acrylate, (poly) propylene glycol di (meth) Polyfunctional (meth) acrylates such as acrylate, (poly) tetramethylene di (meth) acrylate, 1,4-butanediol di (meth) acrylate; triallyl (iso) cyanurate, tri Lil
  • the resin particles can be obtained by polymerizing the polymerizable monomer having an ethylenically unsaturated group by a known method. Examples of this method include a method of suspension polymerization in the presence of a radical polymerization initiator, and a method of polymerizing by swelling a monomer together with a radical polymerization initiator using non-crosslinked seed particles.
  • the substrate particles are inorganic particles or organic-inorganic hybrid particles excluding metal particles
  • examples of the inorganic material for forming the substrate particles include silica and carbon black. Although it does not specifically limit as the particle
  • grains obtained by performing are mentioned.
  • examples of the organic / inorganic hybrid particles include organic / inorganic hybrid particles formed of a crosslinked alkoxysilyl polymer and an acrylic resin.
  • the substrate particles are metal particles
  • examples of the metal for forming the metal particles include silver, copper, nickel, silicon, gold, and titanium.
  • the substrate particles are preferably not metal particles.
  • the particle diameter of the substrate particles is preferably 0.1 ⁇ m or more, more preferably 0.5 ⁇ m or more, still more preferably 1 ⁇ m or more, still more preferably 1.5 ⁇ m or more, particularly preferably 2 ⁇ m or more, preferably 1000 ⁇ m or less, More preferably, it is 500 ⁇ m or less, still more preferably 300 ⁇ m or less, still more preferably 50 ⁇ m or less, still more preferably 30 ⁇ m or less, particularly preferably 5 ⁇ m or less, and most preferably 3 ⁇ m or less.
  • the particle diameter of the substrate particles When the particle diameter of the substrate particles is equal to or greater than the above lower limit, the contact area between the conductive particles and the electrodes is increased, so that the conduction reliability between the electrodes is further increased, and the electrodes are connected via the conductive particles. The connection resistance between them becomes even lower. Further, when forming the conductive layer on the surface of the base particle by electroless plating, it becomes difficult to aggregate and the aggregated conductive particles are hardly formed. When the particle diameter is not more than the above upper limit, the conductive particles are easily compressed, the connection resistance between the electrodes is further reduced, and the distance between the electrodes is further reduced.
  • the particle diameter of the base particle indicates a diameter when the base particle is a true sphere, and indicates a maximum diameter when the base particle is not a true sphere.
  • the particle diameter of the substrate particles is particularly preferably 0.1 ⁇ m or more and 5 ⁇ m or less.
  • the particle diameter of the substrate particles is in the range of 0.1 to 5 ⁇ m, even when the distance between the electrodes is small and the thickness of the conductive layer is increased, small conductive particles can be obtained.
  • the particle diameter of the substrate particles is preferably 0.5 ⁇ m or more. More preferably, it is 2 ⁇ m or more, preferably 3 ⁇ m or less.
  • the metal for forming the conductive layer is not particularly limited. Furthermore, when the conductive particles are metal particles that are conductive layers as a whole, the metal for forming the metal particles is not particularly limited. Examples of the metal include gold, silver, copper, palladium, platinum, zinc, iron, tin, lead, aluminum, cobalt, indium, nickel, chromium, titanium, antimony, bismuth, thallium, germanium, cadmium, silicon, and tungsten. , Molybdenum, and alloys thereof. Examples of the metal include tin-doped indium oxide (ITO) and solder.
  • ITO tin-doped indium oxide
  • the metal element constituting the conductive layer preferably contains nickel.
  • the conductive layer preferably contains at least one selected from the group consisting of nickel, tungsten, molybdenum, palladium, phosphorus and boron, and more preferably contains nickel and phosphorus or boron.
  • the material forming the conductive layer may be an alloy containing phosphorus, boron, or the like. In the conductive layer, nickel and tungsten or molybdenum may be alloyed.
  • the total content of phosphorus and boron is preferably 4% by weight or less in 100% by weight of the conductive layer.
  • the total content of phosphorus and boron is not more than the above upper limit, the content of metals such as nickel is relatively increased, so that the connection resistance between the electrodes is further reduced.
  • the total content of phosphorus and boron is preferably 0.1% by weight or more, more preferably 0.5% by weight or more.
  • the metal element contained most in the core material, the conductive layer, and the second conductive layer is preferably an alloy containing tin, nickel, palladium, copper, or gold, and more preferably nickel or palladium. .
  • the conductive layer may be formed of a single layer. Furthermore, like the conductive particles 11 and 21, the conductive layer may be formed of a plurality of layers. That is, the conductive layer may be a single layer or may have a stacked structure of two or more layers.
  • the outermost layer is preferably a gold layer, a nickel layer, a palladium layer, a copper layer, or an alloy layer containing tin and silver, and the gold layer or the palladium layer Is more preferable, and a gold layer is particularly preferable.
  • the outermost layer is these preferred conductive layers, the connection resistance between the electrodes is further reduced.
  • the outermost layer is a gold layer, the corrosion resistance is further enhanced.
  • the method for forming the conductive layer on the surface of the substrate particles is not particularly limited.
  • a method for forming the conductive layer for example, a method by electroless plating, a method by electroplating, a method by physical vapor deposition, and a method of coating the surface of base particles with metal powder or a paste containing metal powder and a binder Etc.
  • the method by electroless plating is preferable.
  • the method by physical vapor deposition include methods such as vacuum vapor deposition, ion plating, and ion sputtering.
  • the average particle diameter of the conductive particles is preferably 0.11 ⁇ m or more, more preferably 0.5 ⁇ m or more, further preferably 0.51 ⁇ m or more, particularly preferably 1 ⁇ m or more, preferably 100 ⁇ m or less, more preferably 20 ⁇ m or less, More preferably, it is 5.6 micrometers or less, Most preferably, it is 3.6 micrometers or less. It is.
  • the average particle diameter of the conductive particles is not less than the above lower limit and not more than the above upper limit, the contact area between the conductive particles and the electrode becomes sufficiently large when the electrodes are connected using the conductive particles, and the conductive Aggregated conductive particles are less likely to be formed when the layer is formed. Further, the distance between the electrodes connected via the conductive particles does not become too large, and the conductive layer is difficult to peel from the surface of the base material particles.
  • the “average particle size” of the conductive particles indicates a number average particle size.
  • the average particle diameter of the conductive particles can be obtained by observing 50 arbitrary conductive particles with an electron microscope or an optical microscope and calculating an average value.
  • the thickness of the conductive layer is preferably 0.005 ⁇ m or more, more preferably 0.01 ⁇ m or more, preferably 1 ⁇ m or less, more preferably 0.3 ⁇ m or less.
  • the thickness of the conductive layer is not less than the above lower limit and not more than the above upper limit, sufficient conductivity is obtained, and the conductive particles do not become too hard, and the conductive particles are sufficiently deformed when connecting the electrodes. .
  • the thickness of the outermost conductive layer is preferably 0.001 ⁇ m or more, more preferably 0.01 ⁇ m or more, preferably 0.5 ⁇ m or less, more preferably 0. .1 ⁇ m or less.
  • the coating with the outermost conductive layer can be made uniform, corrosion resistance can be sufficiently enhanced, and the connection resistance between the electrodes can be increased. It can be made sufficiently low.
  • the thickness of the conductive layer can be measured by observing the cross section of the conductive particles or the conductive particles with insulating particles using, for example, a transmission electron microscope (TEM).
  • TEM transmission electron microscope
  • the number of protrusions on the outer surface of the conductive layer per one of the conductive particles is preferably 3 or more, more preferably 5 or more.
  • the upper limit of the number of protrusions is not particularly limited. The upper limit of the number of protrusions can be appropriately selected in consideration of the average particle diameter of conductive particles and the like.
  • the conductive layer Since the core substance is embedded in the conductive layer, the conductive layer has a plurality of protrusions on the outer surface.
  • a first conductive layer is formed on the surface of the base particle, a core substance is disposed on the first conductive layer, and then a second conductive layer is formed.
  • Examples thereof include a method and a method of adding a core substance in the middle of forming a conductive layer on the surface of the base particle.
  • the material constituting the core material there may be mentioned a conductive material and a non-conductive material.
  • the conductive material include conductive non-metals such as metals, metal oxides, and graphite, and conductive polymers.
  • the conductive polymer include polyacetylene.
  • the non-conductive substance include silica, alumina, barium titanate, zirconia, and the like. Among them, metal is preferable because conductivity can be increased and connection resistance can be effectively reduced.
  • the core substance is preferably metal particles.
  • the metal examples include gold, silver, copper, platinum, zinc, iron, lead, tin, aluminum, cobalt, indium, nickel, chromium, titanium, antimony, bismuth, germanium and cadmium, and tin-lead.
  • examples thereof include alloys composed of two or more metals such as alloys, tin-copper alloys, tin-silver alloys, tin-lead-silver alloys, and tungsten carbide. Of these, nickel, copper, silver or gold is preferable.
  • the metal constituting the core material may be the same as or different from the metal constituting the conductive layer.
  • the metal constituting the core material preferably includes a metal constituting the conductive layer. It is preferable that the metal which comprises the said core substance contains nickel. It is preferable that the metal which comprises the said core substance contains nickel.
  • the shape of the core substance is not particularly limited.
  • the shape of the core substance is preferably a lump.
  • Examples of the core substance include a particulate lump, an agglomerate in which a plurality of fine particles are aggregated, and an irregular lump.
  • the average diameter (average particle diameter) of the core substance is preferably 0.001 ⁇ m or more, more preferably 0.05 ⁇ m or more, preferably 0.9 ⁇ m or less, more preferably 0.2 ⁇ m or less.
  • the connection resistance between the electrodes can be effectively reduced.
  • the “average diameter (average particle diameter)” of the core substance indicates a number average diameter (number average particle diameter).
  • the average diameter of the core material is obtained by observing 50 arbitrary core materials with an electron microscope or an optical microscope and calculating an average value.
  • Inorganic particles may be disposed on the surface of the core substance. It is preferable that there are a plurality of inorganic particles arranged on the surface of the core substance. Inorganic particles may be attached to the surface of the core substance. You may use the composite particle provided with such an inorganic particle and a core substance.
  • the size (average diameter) of the inorganic particles is preferably smaller than the size (average diameter) of the core substance, and the inorganic particles are preferably inorganic fine particles.
  • Examples of the material of the inorganic particles arranged on the surface of the core substance include barium titanate (Mohs hardness 4.5), silica (silicon dioxide, Mohs hardness 6-7), zirconia (Mohs hardness 8-9), Examples include alumina (Mohs hardness 9), tungsten carbide (Mohs hardness 9), diamond (Mohs hardness 10), and the like.
  • the inorganic particles are preferably silica, zirconia, alumina, tungsten carbide or diamond, and are also preferably silica, zirconia, alumina or diamond.
  • the Mohs hardness of the inorganic particles is preferably 5 or more, more preferably 6 or more.
  • the Mohs hardness of the inorganic particles is preferably larger than the Mohs hardness of the conductive layer.
  • the Mohs hardness of the inorganic particles is preferably larger than the Mohs hardness of the second conductive layer.
  • the absolute value of the difference between the Mohs hardness of the inorganic particles and the Mohs hardness of the conductive layer, and the absolute value of the difference between the Mohs hardness of the inorganic particles and the Mohs hardness of the second conductive layer are preferably 0.1. Above, more preferably 0.2 or more, still more preferably 0.5 or more, particularly preferably 1 or more. Further, when the conductive layer is formed of a plurality of layers, the effect of reducing the connection resistance is more effectively exhibited when the inorganic particles are harder than all the metals constituting the plurality of layers.
  • the average particle size of the inorganic particles is preferably 0.0001 ⁇ m or more, more preferably 0.005 ⁇ m or more, preferably 0.5 ⁇ m or less, more preferably 0.1 ⁇ m or less.
  • the connection resistance between the electrodes can be effectively reduced.
  • the “average particle size” of the inorganic particles indicates the number average particle size.
  • the average particle diameter of the inorganic particles is obtained by observing 50 arbitrary inorganic particles with an electron microscope or an optical microscope and calculating an average value.
  • the average diameter of the composite particles is preferably 0.0012 ⁇ m or more, more preferably 0.0502 ⁇ m or more, preferably Is 1.9 ⁇ m or less, more preferably 1.2 ⁇ m or less.
  • the average diameter of the composite particles is not less than the above lower limit and not more than the above upper limit, the connection resistance between the electrodes can be effectively reduced.
  • the “average diameter (average particle diameter)” of the composite particles indicates a number average diameter (number average particle diameter).
  • the average diameter of the composite particles is determined by observing 50 arbitrary composite particles with an electron microscope or an optical microscope and calculating an average value.
  • the conductive particles according to the present invention preferably include an insulating material disposed on the surface of the conductive layer.
  • an insulating material disposed on the surface of the conductive layer.
  • an insulating material is present between the plurality of electrodes, so that it is possible to prevent a short circuit between electrodes adjacent in the lateral direction instead of between the upper and lower electrodes.
  • the insulating substance between the conductive layer of the conductive particles and the electrodes can be easily excluded. Since the conductive particles have a plurality of protrusions on the outer surface of the conductive layer, the insulating material between the conductive layer of the conductive particles and the electrode can be easily excluded.
  • the insulating material is an insulating particle because the insulating material can be more easily removed when the electrodes are crimped.
  • thermoplastic resin examples include vinyl polymers and vinyl copolymers.
  • thermosetting resin an epoxy resin, a phenol resin, a melamine resin, etc.
  • water-soluble resin examples include polyvinyl alcohol, polyacrylic acid, polyacrylamide, polyvinyl pyrrolidone, polyethylene oxide, and methyl cellulose. Of these, water-soluble resins are preferable, and polyvinyl alcohol is more preferable.
  • Examples of a method for disposing an insulating material on the surface of the conductive layer include a chemical method and a physical or mechanical method.
  • Examples of the chemical method include an interfacial polymerization method, a suspension polymerization method in the presence of particles, and an emulsion polymerization method.
  • Examples of the physical or mechanical method include spray drying, hybridization, electrostatic adhesion, spraying, dipping, and vacuum deposition. In particular, since the insulating substance is difficult to be detached, a method of disposing the insulating substance on the surface of the conductive layer through a chemical bond is preferable.
  • the average diameter (average particle diameter) of the insulating material can be appropriately selected depending on the particle diameter of the conductive particles and the use of the conductive particles.
  • the average diameter (average particle diameter) of the insulating material is preferably 0.005 ⁇ m or more, more preferably 0.01 ⁇ m or more, preferably 1 ⁇ m or less, more preferably 0.5 ⁇ m or less.
  • the average diameter of the insulating material is not less than the above lower limit, the conductive layers of the plurality of conductive particles are difficult to contact when the conductive particles are dispersed in the binder resin.
  • the average diameter of the insulating particles is not more than the above upper limit, it is not necessary to make the pressure too high in order to eliminate the insulating material between the electrodes and the conductive particles when the electrodes are connected. There is no need for heating.
  • the “average diameter (average particle diameter)” of the insulating material indicates a number average diameter (number average particle diameter).
  • the average diameter of the insulating material is obtained using a particle size distribution measuring device or the like.
  • the conductive material according to the present invention includes the conductive particles described above and a binder resin.
  • the conductive particles are preferably dispersed in a binder resin and used as a conductive material.
  • the conductive material is preferably an anisotropic conductive material.
  • the binder resin is not particularly limited.
  • As the binder resin a known insulating resin is used.
  • binder resin examples include vinyl resins, thermoplastic resins, curable resins, thermoplastic block copolymers, and elastomers.
  • vinyl resins examples include vinyl resins, thermoplastic resins, curable resins, thermoplastic block copolymers, and elastomers.
  • the said binder resin only 1 type may be used and 2 or more types may be used together.
  • Examples of the vinyl resin include vinyl acetate resin, acrylic resin, and styrene resin.
  • examples of the thermoplastic resin include polyolefin resin, ethylene-vinyl acetate copolymer, and polyamide resin.
  • examples of the curable resin include an epoxy resin, a urethane resin, a polyimide resin, and an unsaturated polyester resin.
  • the curable resin may be a room temperature curable resin, a thermosetting resin, a photocurable resin, or a moisture curable resin.
  • the curable resin may be used in combination with a curing agent.
  • thermoplastic block copolymer examples include a styrene-butadiene-styrene block copolymer, a styrene-isoprene-styrene block copolymer, a hydrogenated product of a styrene-butadiene-styrene block copolymer, and a styrene-isoprene. -Hydrogenated products of styrene block copolymers.
  • the elastomer examples include styrene-butadiene copolymer rubber and acrylonitrile-styrene block copolymer rubber.
  • the conductive material includes, for example, a filler, an extender, a softener, a plasticizer, a polymerization catalyst, a curing catalyst, a colorant, an antioxidant, a heat stabilizer, and a light stabilizer.
  • a filler for example, a filler, an extender, a softener, a plasticizer, a polymerization catalyst, a curing catalyst, a colorant, an antioxidant, a heat stabilizer, and a light stabilizer.
  • Various additives such as an agent, an ultraviolet absorber, a lubricant, an antistatic agent and a flame retardant may be contained.
  • the method for dispersing the conductive particles in the binder resin is not particularly limited, and a conventionally known dispersion method can be used.
  • Examples of a method for dispersing the conductive particles in the binder resin include a method in which the conductive particles are added to the binder resin and then kneaded and dispersed with a planetary mixer or the like. The conductive particles are dispersed in water. Alternatively, after uniformly dispersing in an organic solvent using a homogenizer or the like, it is added to the binder resin and kneaded with a planetary mixer or the like, and the binder resin is diluted with water or an organic solvent. Then, the method of adding the said electroconductive particle, kneading with a planetary mixer etc. and disperse
  • distributing is mentioned.
  • the conductive material according to the present invention can be used as a conductive paste and a conductive film.
  • the conductive material according to the present invention is a conductive film
  • a film that does not include conductive particles may be laminated on a conductive film that includes conductive particles.
  • the conductive paste is preferably an anisotropic conductive paste.
  • the conductive film is preferably an anisotropic conductive film.
  • the content of the binder resin is preferably 10% by weight or more, more preferably 30% by weight or more, still more preferably 50% by weight or more, particularly preferably 70% by weight or more, preferably 99.% or more. It is 99 weight% or less, More preferably, it is 99.9 weight% or less.
  • the content of the binder resin is not less than the above lower limit and not more than the above upper limit, the conductive particles are efficiently arranged between the electrodes, and the connection reliability of the connection target member connected by the conductive material is further increased.
  • the content of the conductive particles is preferably 0.01% by weight or more, more preferably 0.1% by weight or more, preferably 40% by weight or less, more preferably 20% by weight or less, More preferably, it is 10 weight% or less.
  • the content of the conductive particles is not less than the above lower limit and not more than the above upper limit, the conduction reliability between the electrodes is further enhanced.
  • connection structure can be obtained by connecting the connection target members using the conductive particles of the present invention or using a conductive material containing the conductive particles and a binder resin.
  • connection structure includes a first connection target member, a second connection target member, and a connection portion connecting the first and second connection target members, and the connection portion is a conductive member of the present invention.
  • the connection structure is preferably formed of conductive particles or formed of a conductive material (such as an anisotropic conductive material) containing the conductive particles and a binder resin.
  • the connection portion itself is conductive particles. That is, the first and second connection target members are connected by the conductive particles.
  • FIG. 4 is a front cross-sectional view schematically showing a connection structure using conductive particles according to the first embodiment of the present invention.
  • connection portion 54 includes a first connection target member 52, a second connection target member 53, and a connection portion 54 that connects the first and second connection target members 52 and 53.
  • the connection portion 54 is formed by curing a conductive material including the conductive particles 1.
  • the conductive particles 1 are schematically shown for convenience of illustration.
  • the first connection target member 52 has a plurality of electrodes 52b on the upper surface 52a (front surface).
  • the second connection target member 53 has a plurality of electrodes 53b on the lower surface 53a (front surface).
  • the electrode 52 b and the electrode 53 b are electrically connected by one or a plurality of conductive particles 1. Therefore, the first and second connection target members 52 and 53 are electrically connected by the conductive particles 1.
  • connection structure is not particularly limited.
  • the conductive material is disposed between the first connection target member and the second connection target member to obtain a laminate, and then the laminate is heated and pressurized. Methods and the like.
  • the pressurizing pressure is about 9.8 ⁇ 10 4 to 4.9 ⁇ 10 6 Pa.
  • the heating temperature is about 120 to 220 ° C.
  • connection target member examples include electronic components such as semiconductor chips, capacitors, and diodes, and electronic components such as circuit boards such as printed boards, flexible printed boards, and glass boards.
  • the connection target member is preferably an electronic component.
  • the conductive particles are preferably used for electrical connection of electrodes in an electronic component.
  • the electrode provided on the connection target member examples include metal electrodes such as a gold electrode, a nickel electrode, a tin electrode, an aluminum electrode, a copper electrode, a molybdenum electrode, and a tungsten electrode.
  • the electrode is preferably a gold electrode, a nickel electrode, a tin electrode, or a copper electrode.
  • the connection target member is a glass substrate, the electrode is preferably an aluminum electrode, a copper electrode, a molybdenum electrode, or a tungsten electrode.
  • the electrode formed only with aluminum may be sufficient and the electrode by which the aluminum layer was laminated
  • the material for the metal oxide layer include indium oxide doped with a trivalent metal element and zinc oxide doped with a trivalent metal element. Examples of the trivalent metal element include Sn, Al, and Ga.
  • Example 1 Palladium adhesion process Divinylbenzene resin particles (“Micropearl SP-205” manufactured by Sekisui Chemical Co., Ltd.) having a particle diameter of 5.0 ⁇ m were prepared. The resin particles were etched and washed with water. Next, resin particles were added to 100 mL of a palladium-catalyzed solution containing 8% by weight of a palladium catalyst and stirred. Then, it filtered and wash
  • a suspension was obtained by adding the resin particles to which palladium obtained in 1000 mL of pure water was adhered and dispersing with an ultrasonic disperser. While stirring the obtained suspension at 60 ° C., the nickel plating solution was gradually added dropwise to the suspension to perform electroless nickel plating. Thereafter, the suspension is filtered to remove the particles, washed with water, and dried to obtain a first conductive layer (nickel-molybdenum-phosphorus layer (Ni-Mo-P layer)) The resin particles were coated at a thickness of 5.2 nm) to obtain particles on which the first conductive layer was formed.
  • Nickel containing 0.25 mol / L nickel sulfate, 0.25 mol / L sodium hypophosphite, 0.15 mol / L sodium citrate and 0.01 mol / L sodium molybdate to form a nickel-phosphorus conductive layer A plating solution (pH 8.0) was prepared.
  • the above nickel plating solution is gradually dropped into the suspension, electroless nickel plating is performed, and a second conductive layer (nickel-molybdenum-phosphorus) having a thickness of 90 nm is obtained.
  • a layer Ni—Mo—P layer was formed, and then the suspension was filtered to take out the particles, washed with water, and dried to obtain conductive particles. , Having a protrusion on the outer surface of the second conductive layer, and a core substance disposed on the inner side of the protrusion of the second conductive layer, and the first conductive layer between the resin particles and the core substance. Layers were placed.
  • Example 2 Conductive particles were obtained in the same manner as in Example 1 except that the alumina (Al 2 O 3 ) particle slurry (average particle size 100 nm) was changed to a silica particle slurry (average particle size 100 nm).
  • Example 3 Conductive particles were obtained in the same manner as in Example 1 except that the alumina (Al 2 O 3 ) particle slurry (average particle size 100 nm) was changed to a tungsten carbide (WC) particle slurry (average particle size 100 nm).
  • alumina (Al 2 O 3 ) particle slurry average particle size 100 nm
  • WC tungsten carbide
  • Example 4 Conductive particles were obtained in the same manner as in Example 1 except that the thickness of the first conductive layer, which was a nickel-phosphorous layer, was changed to the value shown below.
  • the thickness of the first conductive layer Example 4: 10 ⁇ m
  • Example 5 20 ⁇ m
  • Example 6 100 ⁇ m
  • Example 7 750 ⁇ m
  • Example 8 860 ⁇ m
  • Example 9 (1) Preparation of insulating particles Into a 1000 mL separable flask equipped with a four-neck separable cover, stirring blade, three-way cock, cooling tube and temperature probe, 100 mmol of methyl methacrylate and N, N, N-trimethyl Ion-exchanged water containing a monomer composition containing 1 mmol of —N-2-methacryloyloxyethylammonium chloride and 1 mmol of 2,2′-azobis (2-amidinopropane) dihydrochloride so that the solid content is 5% by weight. Then, the mixture was stirred at 200 rpm and polymerized at 70 ° C. for 24 hours under a nitrogen atmosphere. After completion of the reaction, it was freeze-dried to obtain insulating particles having an ammonium group on the surface, an average particle size of 220 nm, and a CV value of 10%.
  • the insulating particles were dispersed in ion exchange water under ultrasonic irradiation to obtain a 10 wt% aqueous dispersion of insulating particles.
  • Example 2 10 g of the conductive particles obtained in Example 1 were dispersed in 500 mL of ion-exchanged water, 4 g of an aqueous dispersion of insulating particles was added, and the mixture was stirred at room temperature for 6 hours. After filtration through a 3 ⁇ m mesh filter, the particles were further washed with methanol and dried to obtain conductive particles having insulating particles attached thereto.
  • Example 10 Divinylbenzene resin particles having a particle diameter of 5.0 ⁇ m (“Micropearl SP-205” manufactured by Sekisui Chemical Co., Ltd.) and divinylbenzene resin particles having a particle diameter of 5.0 ⁇ m (“Micropearl SP manufactured by Sekisui Chemical Co., Ltd.) are used. Conductive particles were obtained in the same manner as in Example 1 except that the surface of -205 ”) was changed to silica-coated organic-inorganic hybrid particles (particle diameter 5.1 ⁇ m).
  • Example 1 Conductive particles were obtained in the same manner as in Example 1 except that the thickness of the first conductive layer, which was a nickel-phosphorous layer, was changed to 4.5 nm.
  • Divinylbenzene resin particles (“Micropearl SP-205” manufactured by Sekisui Chemical Co., Ltd.) having a particle diameter of 5.0 ⁇ m were prepared. Moreover, an alumina (Al 2 O 3 ) particle slurry (average particle diameter: 100 nm) was prepared. Using resin particles and metal particle slurry, the surface of the resin particles was coated with a core substance to obtain a suspension.
  • Nickel containing 0.25 mol / L nickel sulfate, 0.25 mol / L sodium hypophosphite, 0.15 mol / L sodium citrate and 0.01 mol / L sodium molybdate to form a nickel-phosphorus conductive layer A plating solution (pH 8.0) was prepared.
  • the nickel plating solution was gradually added dropwise to the suspension, and electroless nickel plating was performed to form a conductive layer having a thickness of 100 nm. Thereafter, the suspension was filtered to take out the particles, washed with water, and dried to obtain conductive particles. In the obtained conductive particles, the core substance and the base material particles were in contact.
  • Example 11 (1) Palladium adhesion process The resin particle to which the palladium obtained in Example 1 was adhered was prepared.
  • Nickel plating solution containing 0.23 mol / L nickel sulfate, 0.92 mol / L dimethylamine borane, 0.5 mol / L sodium citrate and 0.01 mol / L sodium tungstate (pH 8. 5) was prepared.
  • a suspension was obtained by adding the resin particles to which palladium obtained in 1000 mL of pure water was adhered and dispersing with an ultrasonic disperser. While stirring the obtained suspension at 60 ° C., the nickel plating solution was gradually added dropwise to the suspension to perform electroless nickel plating. Thereafter, by filtering the suspension, the particles are taken out, washed with water, and dried to cover the resin particles with the first conductive layer (thickness 5.1 nm) which is a nickel-tungsten-boron layer. The particle
  • a nickel plating solution (pH 8.5) containing 0.23 mol / L of nickel sulfate, 0.92 mol / L of dimethylamine borane, 0.5 mol / L of sodium citrate and 0.01 mol / L of sodium tungstate was prepared.
  • the above nickel plating solution was gradually added dropwise to the suspension, and electroless nickel plating was performed to form a second conductive layer having a thickness of 90 nm. Thereafter, the suspension was filtered to take out the particles, washed with water, and dried to obtain conductive particles.
  • the obtained conductive particles had protrusions on the outer surface of the second conductive layer, and the core substance was disposed inside the protrusions of the second conductive layer.
  • the 1st conductive layer was arrange
  • Example 12 Conductive particles were obtained in the same manner as in Example 11 except that the thickness of the first conductive layer, which was a nickel-tungsten-boron layer, was changed to 10 nm.
  • Example 13 Conductive particles were obtained in the same manner as in Example 11 except that the thickness of the first conductive layer, which was a nickel-tungsten-boron layer, was changed to 20 nm.
  • Example 14 A 10% by weight aqueous dispersion of the insulating particles obtained in Example 9 was prepared. 10 g of the conductive particles obtained in Example 11 were dispersed in 500 mL of ion exchange water, 4 g of an aqueous dispersion of insulating particles was added, and the mixture was stirred at room temperature for 6 hours. After filtration through a 3 ⁇ m mesh filter, the particles were further washed with methanol and dried to obtain conductive particles having insulating particles attached thereto.
  • Example 3 Conductive particles were obtained in the same manner as in Example 11 except that the thickness of the first conductive layer, which was a nickel-tungsten-boron layer, was changed to 3 nm.
  • Divinylbenzene resin particles (“Micropearl SP-205” manufactured by Sekisui Chemical Co., Ltd.) having a particle diameter of 5.0 ⁇ m were prepared. Moreover, an alumina (Al 2 O 3 ) particle slurry (average particle diameter: 100 nm) was prepared. Using resin particles and metal particle slurry, the surface of the resin particles was coated with a core substance to obtain a suspension.
  • a nickel plating solution (pH 8.5) containing 0.23 mol / L of nickel sulfate, 0.92 mol / L of dimethylamine borane, 0.5 mol / L of sodium citrate and 0.01 mol / L of sodium tungstate was prepared.
  • the nickel plating solution was gradually added dropwise to the suspension, and electroless nickel plating was performed to form a conductive layer having a thickness of 100 nm. Thereafter, the suspension was filtered to take out the particles, washed with water, and dried to obtain conductive particles. In the obtained conductive particles, the core substance and the base material particles were in contact.
  • Example 15 (1) Palladium adhesion process The resin particle to which the palladium obtained in Example 1 was adhered was prepared.
  • Nickel plating solution containing 0.23 mol / L nickel sulfate, 0.92 mol / L dimethylamine borane, 0.5 mol / L sodium citrate and 0.01 mol / L sodium tungstate (pH 8. 5) was prepared.
  • a suspension was obtained by adding the resin particles to which palladium obtained in 1000 mL of pure water was adhered and dispersing with an ultrasonic disperser. While stirring the obtained suspension at 60 ° C., the nickel plating solution was gradually added dropwise to the suspension to perform electroless nickel plating. Thereafter, the suspension is filtered to remove the particles, washed with water, and dried to coat the resin particles with the first conductive layer having a thickness of 10 nm, which is a nickel-tungsten-boron layer. Particles with a conductive layer formed were obtained.
  • a nickel plating solution (pH 7.0) containing 0.23 mol / L of nickel sulfate, 0.92 mol / L of dimethylamine borane and 0.5 mol / L of sodium citrate was prepared.
  • the above nickel plating solution was gradually added dropwise to the suspension, and electroless nickel plating was performed to form a second conductive layer having a thickness of 90 nm. Thereafter, the suspension was filtered to take out the particles, washed with water, and dried to obtain conductive particles.
  • the obtained conductive particles had protrusions on the outer surface of the second conductive layer, and the core substance was disposed inside the protrusions of the second conductive layer.
  • the 1st conductive layer was arrange
  • Example 16 Conductive particles were obtained in the same manner as in Example 15 except that the thickness of the first conductive layer, which was a nickel-tungsten-boron layer, was changed to 5.1 nm.
  • Example 17 Conductive particles were obtained in the same manner as in Example 15 except that the thickness of the first conductive layer, which was a nickel-tungsten-boron layer, was changed to 20 nm.
  • Example 18 Conductive particles were obtained in the same manner as in Example 15 except that the barium titanate (BaTiO 3 ) particle slurry (average particle size 100 nm) was changed to alumina (Al 2 O 3 ) particle slurry (average particle size 100 nm). It was.
  • Example 19 Conductive particles were obtained in the same manner as in Example 16 except that the barium titanate (BaTiO 3 ) particle slurry (average particle size 100 nm) was changed to alumina (Al 2 O 3 ) particle slurry (average particle size 100 nm). It was.
  • Example 20 Conductive particles were obtained in the same manner as in Example 17 except that the barium titanate (BaTiO 3 ) particle slurry (average particle size 100 nm) was changed to alumina (Al 2 O 3 ) particle slurry (average particle size 100 nm). It was.
  • Example 21 Conductive particles were obtained in the same manner as in Example 15 except that sodium tungstate 0.01 mol / L was added to the nickel plating solution for forming the second conductive layer.
  • Example 22 A 10% by weight aqueous dispersion of the insulating particles obtained in Example 9 was prepared. 10 g of the conductive particles obtained in Example 15 were dispersed in 500 mL of ion-exchanged water, 4 g of an aqueous dispersion of insulating particles was added, and the mixture was stirred at room temperature for 6 hours. After filtration through a 3 ⁇ m mesh filter, the particles were further washed with methanol and dried to obtain conductive particles having insulating particles attached thereto.
  • Divinylbenzene resin particles (“Micropearl SP-205” manufactured by Sekisui Chemical Co., Ltd.) having a particle diameter of 5.0 ⁇ m were prepared. Moreover, barium titanate (BaTiO 3 ) particle slurry (average particle diameter: 100 nm) was prepared. Using resin particles and metal particle slurry, the surface of the resin particles was coated with a core substance to obtain a suspension.
  • a nickel plating solution (pH 8.5) containing 0.23 mol / L of nickel sulfate, 0.92 mol / L of dimethylamine borane, 0.5 mol / L of sodium citrate and 0.01 mol / L of sodium tungstate was prepared.
  • the nickel plating solution was gradually added dropwise to the suspension, and electroless nickel plating was performed to form a conductive layer having a thickness of 100 nm. Thereafter, the suspension was filtered to take out the particles, washed with water, and dried to obtain conductive particles. In the obtained conductive particles, the core substance and the base material particles were in contact.
  • Example 6 Conductive particles were obtained in the same manner as in Example 18 except that the thickness of the first conductive layer, which was a nickel-tungsten-boron layer, was changed to 1 nm.
  • Example 23 A 10% by weight aqueous dispersion of the insulating particles obtained in Example 9 was prepared. 10 g of the conductive particles obtained in Example 18 were dispersed in 500 mL of ion-exchanged water, 4 g of an aqueous dispersion of insulating particles was added, and the mixture was stirred at room temperature for 6 hours. After filtration through a 3 ⁇ m mesh filter, the particles were further washed with methanol and dried to obtain conductive particles having insulating particles attached thereto.
  • a thin film slice of conductive particles was prepared using a focused ion beam, and the cross section was observed with a scanning electron microscope. The operation was repeated 200 times, and image analysis was performed to obtain a three-dimensional image of the particles. From the stereoscopic image, the distance between the surface of the base particle and the surface of the core material was determined.
  • connection resistance Fabrication of connection structure 10 parts by weight of bisphenol A type epoxy resin (“Epicoat 1009” manufactured by Mitsubishi Chemical Corporation), 40 parts by weight of acrylic rubber (weight average molecular weight of about 800,000), 200 parts by weight of methyl ethyl ketone, and a microcapsule type curing agent (Asahi Kasei Chemicals) "HX3941HP” manufactured by HX3941) and 2 parts by weight of a silane coupling agent ("SH6040" manufactured by Toray Dow Corning Silicone Co., Ltd.) are mixed, and the conductive particles are added so that the content is 3% by weight.
  • a resin composition was obtained by dispersing.
  • the obtained resin composition was applied to a 50 ⁇ m-thick PET (polyethylene terephthalate) film whose one surface was release-treated, and dried with hot air at 70 ° C. for 5 minutes to produce an anisotropic conductive film.
  • the thickness of the obtained anisotropic conductive film was 12 ⁇ m.
  • the obtained anisotropic conductive film was cut into a size of 5 mm ⁇ 5 mm.
  • a two-layer flexible printed board (width 2 cm, length 1 cm) having the same aluminum electrode was aligned and aligned so that the electrodes overlapped.
  • the laminated body of the glass substrate and the two-layer flexible printed circuit board was thermocompression bonded under pressure bonding conditions of 10 N, 180 ° C., and 20 seconds to obtain a connection structure.
  • a two-layer flexible printed board in which an aluminum electrode is directly formed on a polyimide film was used.
  • connection resistance measurement The connection resistance between the opposing electrodes of the obtained connection structure was measured by the 4-terminal method. Further, the connection resistance was determined according to the following criteria.
  • connection resistance is 2.0 ⁇ or less ⁇ : Connection resistance exceeds 2.0 ⁇ , 3.0 ⁇ or less ⁇ : Connection resistance exceeds 3.0 ⁇ , 5.0 ⁇ or less ⁇ : Connection resistance exceeds 5.0 ⁇
  • connection resistance was dropped from a position of 70 cm in height, and the impact resistance was evaluated by confirming conduction. From the rate of increase in resistance value from the initial resistance value, impact resistance was determined according to the following criteria.
  • ⁇ The average value of the number of impressions per electrode area 0.02 mm 2 is 20 or more.
  • ⁇ The average value of the number of impressions per electrode area 0.02 mm 2 is 5 or more and less than 20.
  • Tables 1 to 3 show the Mohs hardness of the first and second conductive layers and the core material. In Tables 1 to 3 below, “-” indicates no evaluation.

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Dispersion Chemistry (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Conductive Materials (AREA)
  • Non-Insulated Conductors (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Chemically Coating (AREA)
  • Powder Metallurgy (AREA)

Abstract

L'invention concerne des particules conductrices qui sont capables de réduire la résistance de connexion entre des électrodes. Les particules conductrices (1) selon la présente invention comprennent chacune : une particule de base (2) ; une couche conductrice (3) recouvrant la particule de base (2) ; et des noyaux (4) d'une substance intégrée dans la couche conductrice (3). La couche conductrice (3) a des saillies (3a) sur la surface extérieure de celle-ci. Les noyaux (4) d'une substance sont disposés à l'intérieur des saillies (3a) de la couche conductrice (3). Des distances séparent la surface de la particule de base (2) des surfaces des noyaux (4) d'une substance, la distance moyenne entre celles-ci étant supérieure à 5 nm.
PCT/JP2012/082910 2011-12-21 2012-12-19 Particules conductrices, matériau conducteur et structure de connexion WO2013094636A1 (fr)

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US20170310020A1 (en) * 2014-10-29 2017-10-26 Dexerials Corporation Electrically conductive material
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