WO2009119788A1 - Particule de polymère, particule conductrice, matériau conducteur anisotrope et structure de connexion - Google Patents

Particule de polymère, particule conductrice, matériau conducteur anisotrope et structure de connexion Download PDF

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Publication number
WO2009119788A1
WO2009119788A1 PCT/JP2009/056226 JP2009056226W WO2009119788A1 WO 2009119788 A1 WO2009119788 A1 WO 2009119788A1 JP 2009056226 W JP2009056226 W JP 2009056226W WO 2009119788 A1 WO2009119788 A1 WO 2009119788A1
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polymer particles
monomer
polymer
particles
metal layer
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PCT/JP2009/056226
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English (en)
Japanese (ja)
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伸也 上野山
博史 山内
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積水化学工業株式会社
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Priority to JP2009514282A priority Critical patent/JP4669905B2/ja
Publication of WO2009119788A1 publication Critical patent/WO2009119788A1/fr

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    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K3/00—Apparatus or processes for manufacturing printed circuits
    • H05K3/30—Assembling printed circuits with electric components, e.g. with resistor
    • H05K3/32—Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits
    • H05K3/321—Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits by conductive adhesives
    • H05K3/323—Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits by conductive adhesives by applying an anisotropic conductive adhesive layer over an array of pads
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/12—Powdering or granulating
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
    • H05K2201/02—Fillers; Particles; Fibers; Reinforcement materials
    • H05K2201/0203—Fillers and particles
    • H05K2201/0206—Materials
    • H05K2201/0221—Insulating particles having an electrically conductive coating

Definitions

  • the present invention relates to polymer particles formed by polymerization of monomers, for example, polymer particles that can be used as conductive particles for connecting electrodes of members to be connected, and the polymer particles.
  • the present invention relates to conductive particles, anisotropic conductive materials, and connection structures.
  • Anisotropic conductive materials such as anisotropic conductive paste, anisotropic conductive ink, anisotropic conductive adhesive, anisotropic conductive film, or anisotropic conductive sheet are widely known.
  • anisotropic conductive materials conductive particles are dispersed in paste, ink, or resin.
  • the anisotropic conductive material is used, for example, to electrically connect electrodes of a substrate such as a glass substrate or a printed substrate.
  • Patent Document 1 discloses conductive particles having base particles and a conductive layer formed on the surface of the base particles. ing. A divinylbenzene-ethylvinylbenzene mixture is used as part of the monomer to form the substrate particles. This conductive particle has a compressive elastic modulus of 2.5 ⁇ 10 9 N / m 2 or less when 10% of the particle diameter is displaced, a compression deformation recovery rate of 30% or more, and a fracture strain of 30% or more. is there. Patent Document 1 describes that when the electrodes of the substrate are electrically connected using the conductive particles, the connection resistance value is lowered and the connection reliability is improved. JP 2003-313304 A
  • the connection resistance value between the electrodes may be increased.
  • the anisotropic conductive material is bonded to the epoxy adhesive, the adhesive force of the anisotropic conductive material is high.
  • the anisotropic conductive material is directly bonded to the polyimide film, the adhesive force of the anisotropic conductive material tends to be low.
  • the compressive deformation recovery rate of the conductive particles is high.
  • the anisotropic conductive material sometimes peeled off. For this reason, the connection resistance value between the electrodes may not be sufficiently lowered.
  • another substrate is placed on the substrate so that the electrodes face each other. Overlapping. Next, the conductive particles are compressed by pressurization to connect the electrodes.
  • indentations generated by applying pressure to the electrode in contact with the conductive particles described in Patent Document 1 when the pressure is applied are not sufficiently formed.
  • voids may occur around the conductive particles. For this reason, the conductive reliability between the electrodes of the two-layer flexible printed board and the glass substrate may be low.
  • An object of the present invention is to improve the conductive reliability when a connection target member is electrically connected by conductive particles having a metal layer formed on the surface or an anisotropic conductive material including the conductive particles. It is to provide polymer particles that can be produced, and conductive particles, anisotropic conductive materials, and connection structures using the polymer particles.
  • the limited object of the present invention is to electrically connect the electrodes of a flexible printed circuit board such as a two-layer flexible printed circuit board and a glass substrate using conductive particles having a metal layer formed on the surface.
  • another limited object of the present invention is that when conductive members having a low-melting point metal layer formed on the surface thereof are used to electrically connect connection target members, an impact is applied by dropping or the like.
  • Another object of the present invention is to provide polymer particles in which cracks are unlikely to occur in the low melting point metal layer, and conductive particles, anisotropic conductive materials and connection structures using the polymer particles.
  • polymer particles obtained by polymerizing a monomer which is an alicyclic compound having at least two ring structures.
  • the at least two ring structures are a bicyclo ring structure or a tricyclo ring structure.
  • the monomer is an acrylic monomer.
  • the compression recovery rate is 50% or less, and the compression elastic modulus when compressed by 10% is in the range of 980 to 4,900 N / mm 2. .
  • the compression recovery rate is in the range of 10 to 50%.
  • the polymer particles according to the present invention are preferably polymer particles obtained by polymerizing a monofunctional monomer, which is an alicyclic compound having at least two ring structures, and a polyfunctional monomer, and at least 2
  • a polymer particle obtained by polymerizing a monomer component containing 20 to 90% by weight of a monofunctional monomer which is an alicyclic compound having one ring structure and 10 to 80% by weight of a polyfunctional monomer is more preferable. preferable.
  • the polymer particles according to the present invention are also preferably polymer particles obtained by polymerizing a polyfunctional monomer that is an alicyclic compound having at least two ring structures.
  • polymer particles obtained by polymerizing a monomer component containing 20% by weight or more of a polyfunctional monomer which is an alicyclic compound having at least two ring structures are preferable.
  • the polymer particles according to the present invention polymerize a monofunctional monomer that is an alicyclic compound having at least two ring structures and a polyfunctional monomer that is an alicyclic compound having at least two ring structures. It is also preferred that the polymer particles obtained by
  • the conductive particles according to the present invention include polymer particles configured according to the present invention and a metal layer covering the surface of the polymer particles.
  • the compression recovery rate is 45% or less.
  • the outer surface of the metal layer is a metal layer containing nickel, a metal layer containing palladium, or a metal layer containing a low melting point metal.
  • the anisotropic conductive material according to the present invention includes conductive particles and a binder resin.
  • connection structure which concerns on this invention has connected the 1st connection object member, the 2nd connection object member, and the 1st, 2nd connection object member, and the electroconductive particle comprised according to this invention With.
  • connection structure includes a first connection target member, a second connection target member, and a connection part connecting the first and second connection target members, and the connection part. Is formed of an anisotropic conductive material constructed according to the present invention.
  • polymer particles are obtained by polymerizing a monomer that is an alicyclic compound having at least two ring structures. Therefore, the conductivity of a metal layer formed on the surface of the polymer particles is obtained.
  • the connection target member is electrically connected with the particles or the anisotropic conductive material containing the conductive particles, the conductive reliability can be increased.
  • the connection resistance value between the electrodes becomes low. Furthermore, the impression which the electroconductive particle contacted becomes easy to be formed in electrodes, such as an electrode of a printed circuit board or a glass substrate. For this reason, the conduction
  • connection target member is electrically connected using conductive particles having a low melting point metal layer formed on the surface of the polymer particles according to the present invention
  • the melting point is low even if an impact such as dropping is applied. Cracks are unlikely to occur in the metal layer.
  • FIG. 1 is a front sectional view schematically showing a connection structure using conductive particles according to an embodiment of the present invention.
  • FIG. 2 is an enlarged front sectional view showing a contact portion between the conductive particle and the electrode of the connection structure shown in FIG.
  • FIG. 3 is a partially cutaway front cross-sectional view schematically showing a state in which a void is generated in a connection structure using conventional conductive particles.
  • the polymer particles according to the present invention can be obtained by polymerizing a monomer that is an alicyclic compound having at least two ring structures.
  • the alicyclic compound having at least two ring structures is preferably a polycyclic compound.
  • the at least two ring structures include a bicyclo ring structure, a tricyclo ring structure, a spiro ring structure, or a dispiro ring structure.
  • the at least two ring structures are preferably a bicyclo ring structure or a tricyclo ring structure.
  • the compression recovery rate of the polymer particles can be lowered.
  • gap arises when an adhesive layer etc. interface peel from the connection object members, such as a board
  • the voids are preferably not generated. However, the gap may be generated to such an extent that the conductive reliability is not affected.
  • the monomer is not particularly limited as long as it is an alicyclic compound having at least two ring structures.
  • the monomer include acrylic monomers, vinyl ether compounds, epoxy compounds, and isocyanate compounds. Among them, an acrylic monomer is preferable because the compression recovery rate of the polymer particles can be lowered.
  • acrylic monomer examples include dimethylol-tricyclodecane di (meth) acrylate, 1,3-adamantanediol di (meth) acrylate, isobornyl (meth) acrylate, dicyclopentenyl (meth) acrylate, dicyclo Examples include pentanyl (meth) acrylate, 2-methyl-2-adamantyl (meth) acrylate, 2-ethyl-2-adamantyl (meth) acrylate, and 3-hydroxy-1-adamantyl (meth) acrylate.
  • (meth) acrylate means a methacrylate or an acrylate.
  • vinyl ether compound examples include tricyclodecane vinyl ether and tricyclodecane monomethyl vinyl ether.
  • the monomer component in addition to the monomer that is an alicyclic compound having at least two ring structures, another monomer other than the monomer may be used.
  • the content of the monomer that is an alicyclic compound having at least two ring structures in 100% by weight of the monomer component is preferably 5% by weight or more, and more preferably 20% by weight or more.
  • the other monomer include styrene and divinylbenzene.
  • Monofunctional acrylic monomers include isobornyl (meth) acrylate, dicyclopentenyl (meth) acrylate, dicyclopentanyl (meth) acrylate, 2-methyl-2-adamantyl (meth) acrylate, 2-ethyl-2-adamantyl ( Meth) acrylate or 3-hydroxy-1-adamantyl (meth) acrylate is preferably used.
  • the content of the bifunctional acrylic monomer is in the range of 20 to 80% by weight per 100% by weight of the monomer component. Is preferred.
  • the bifunctional acrylic monomer dimethylol-tricyclodecane di (meth) acrylate or 1,3-adamantanediol di (meth) acrylate is preferably used.
  • the polymer particles according to the present invention are obtained by polymerizing a monofunctional monomer that is an alicyclic compound having at least two ring structures (hereinafter sometimes abbreviated as monofunctional monomer A) and a polyfunctional monomer.
  • the obtained polymer particles are preferable.
  • the monomer component preferably includes the monofunctional monomer A and a polyfunctional monomer.
  • the polyfunctional monomer include aromatic compounds having at least two vinyl groups or polyfunctional acrylic monomers.
  • the aromatic compound include 1,2-divinylbenzene, 1,3-divinylbenzene, 1,4-divinylbenzene, and the like.
  • “DVB960” manufactured by Nippon Steel Chemical Co., Ltd. is commercially available.
  • the polyfunctional acrylic monomer is preferably a polyfunctional acrylic monomer having a — (R—O) n-unit, such as polytetramethylene glycol di (meth) acrylate, trimethylolpropane tri (meth) acrylate, tetramethylolmethanetri (Meth) acrylate, pentaerythritol tri (meth) acrylate, pentaerythritol tetra (meth) acrylate, triethylene glycol di (meth) acrylate, dipentaerythritol hexa (meth) acrylate and the like.
  • R is an alkylene group having 1 to 9 carbon atoms
  • n is an integer of 1 or more.
  • the 10% K value is relatively high and the 10% K value is controlled within a suitable range as compared with the case where only the monofunctional monomer A is polymerized.
  • the compression recovery rate can be increased. That is, by using a polyfunctional monomer as a crosslinking agent together with the monofunctional monomer A, the 10% K value and the compression recovery rate can be controlled.
  • the monomer component preferably contains 20 to 90% by weight of the monofunctional monomer A and 10 to 80% by weight of the polyfunctional monomer. In this case, polymer particles having a 10% K value and a favorable compression recovery rate can be easily obtained.
  • the monomer component preferably includes 20 to 80% by weight of the monofunctional monomer A and 20 to 80% by weight of the polyfunctional monomer A, and further includes 40 to 60% by weight of the monofunctional monomer A and 40 to 60% by weight of the polyfunctional monomer. % Is more preferable.
  • the polymer particle according to the present invention is a polymer particle obtained from a polyfunctional monomer that is an alicyclic compound having at least two ring structures (hereinafter sometimes abbreviated as polyfunctional monomer B).
  • polyfunctional monomer B an alicyclic compound having at least two ring structures
  • the monomer component preferably contains the polyfunctional monomer B. Even if only the polyfunctional monomer B is polymerized, the 10% K value can be made relatively high, the 10% K value can be controlled within a suitable range, and the compression recovery rate can be made relatively high. However, other monomers may be used together with the polyfunctional monomer B.
  • the monomer component preferably contains 20% by weight or more of the polyfunctional monomer B.
  • the 10% K value can be increased and the 10% K value can be controlled within a suitable range without the polymer particles becoming too flexible.
  • the polyfunctional monomer B and an acrylic monomer such as polytetramethylene glycol di (meth) acrylate having two functional groups are used in combination, the 10% K value can be controlled within a suitable range.
  • the polyfunctional monomer B and a vinyl monomer such as divinylbenzene having an aromatic ring and at least two functional groups are used in combination, the 10% K value and the compression recovery rate can be increased.
  • the more preferable lower limit of the content of the polyfunctional monomer B in 100% by weight of the monomer component is 20% by weight, the preferable upper limit is 80% by weight, and the more preferable upper limit is 60% by weight.
  • the content of the polyfunctional monomer B in 100% by weight of the monomer component may be 100% by weight.
  • the other monomer used in combination with the polyfunctional monomer B may be a monofunctional monomer A that is an alicyclic compound having at least two ring structures.
  • the polymerization method is not particularly limited. Specific examples of the polymerization method include conventionally known polymerization methods such as a suspension polymerization method, an emulsion polymerization method, a seed polymerization method, and a dispersion polymerization method.
  • the above suspension polymerization method and emulsion polymerization method are suitable for the purpose of producing fine particles having a variety of particle sizes.
  • the suspension polymerization method and the emulsion polymerization method it is preferable to classify polymer particles obtained by polymerization and select polymer particles having a desired particle size or particle size distribution.
  • the seed polymerization method is suitable for the purpose of producing a large amount of polymer particles having specific particle sizes.
  • the seed polymerization method is a method in which seed particles such as styrene polymer particles are swollen with a monomer that is an alicyclic compound having at least two ring structures and polymerized. Therefore, when the polymer particles of the present invention are produced using a seed polymerization method, the polymer particles of the present invention may contain a component constituting the seed particles. For example, when styrene polymer particles are used as seed particles, the resulting polymer particles may contain a styrene polymer.
  • the solvent used for the polymerization is not particularly limited.
  • the solvent is appropriately selected according to the monomer component.
  • Examples of the solvent include water, alcohol, cellosolve, ketone, and acetate. Other solvents other than these solvents may be used.
  • Specific examples of the alcohol include methanol, ethanol, and propanol.
  • Specific examples of the cellosolve include methyl cellosolve and ethyl cellosolve.
  • Specific examples of the ketone include acetone, methyl ethyl ketone, methyl butyl ketone, and 2-butanone.
  • Specific examples of the acetate include ethyl acetate and butyl acetate.
  • Specific examples of the other solvent include acetonitrile, N, N-dimethylformamide, dimethyl sulfoxide and the like. As for these solvents, only 1 type may be used and 2 or more types may be used together.
  • the average particle diameter of the polymer particles is preferably in the range of 0.1 to 1,000 ⁇ m.
  • a more preferable lower limit of the average particle diameter of the polymer particles is 1 ⁇ m, a further preferable lower limit is 1.5 ⁇ m, and a particularly preferable lower limit is 2 ⁇ m.
  • a more preferable upper limit of the average particle diameter of the polymer particles is 500 ⁇ m, a further preferable upper limit is 300 ⁇ m, and a particularly preferable upper limit is 30 ⁇ m. If the average particle diameter is too small, the contact area between the conductive particles and the electrode becomes small, and the connection resistance value may increase. Further, when the metal layer is formed on the surface of the polymer particles by electroless plating, the particles easily aggregate and the aggregated conductive particles are easily formed. When the average particle diameter is too large, the conductive particles are not easily compressed, and the connection resistance value between the electrodes may be increased.
  • the above average particle diameter indicates the number average particle diameter.
  • the average particle diameter can be measured using, for example, a Coulter counter (manufactured by Beckman Coulter).
  • the polymer particle CV value (coefficient of variation in particle size distribution) is preferably 10% or less, and more preferably 3% or less. If the CV value exceeds 10%, the interval between the electrodes connected by the conductive particles may vary.
  • CV value (%) ( ⁇ / Dn) ⁇ 100 ⁇ : standard deviation of polymer particle diameter Dn: average particle diameter
  • the compression recovery rate of the polymer particles is preferably 50% or less, and more preferably 40% or less. If the compression recovery rate exceeds 50%, the anisotropic conductive material may peel from the substrate or the like due to the repulsive force of the conductive particles used for connection between the electrodes. As a result, the connection resistance value between the electrodes may increase.
  • the compression recovery rate of the polymer particles is preferably 5% or more, more preferably 10% or more, and even more preferably 20% or more.
  • the compression recovery rate can be measured as follows.
  • a load is applied up to the reversal load value (5.00 mN) in the center direction of the polymer particle using a micro compression tester. Thereafter, the load is gradually reduced to the load value for origin (0.40 mN). The load-compression displacement during this period is measured, and the compression recovery rate can be obtained from the following equation.
  • the load speed is 0.33 mN / sec.
  • the micro compression tester for example, “Fischer Scope H-100” manufactured by Fischer is used.
  • Compression recovery rate (%) [(L 1 ⁇ L 2 ) / L 1 ] ⁇ 100
  • L 1 Compressive displacement from the load value for the origin when the load is applied to the reverse load value
  • L 2 Compressive displacement from the reverse load value when the load is released to the load value for the origin
  • the compression modulus (10% K value) when the diameter of the polymer particles is displaced by 10% is preferably in the range of 196 to 6,860 N / mm 2 .
  • a more preferable lower limit of the 10% K value is 980 N / mm 2
  • a more preferable upper limit is 4,900 N / mm 2 .
  • the compression modulus (20% K value) when the diameter of the polymer particles is displaced by 20% is preferably in the range of 196 to 6,860 N / mm 2 .
  • a more preferable lower limit of the 20% K value is 600 N / mm 2
  • a further preferable lower limit is 980 N / mm 2
  • a more preferable upper limit is 4,900 N / mm 2
  • a further preferable upper limit is 3,900 N / mm 2. It is.
  • the compression modulus (30% K value) when the diameter of the polymer particles is displaced by 30% is preferably in the range of 196 to 6,860 N / mm 2 .
  • a more preferable lower limit of the 30% K value is 600 N / mm 2
  • a further preferable lower limit is 980 N / mm 2
  • a more preferable upper limit is 4,900 N / mm 2 .
  • the compression modulus (10% K value, 20% K value, and 30% K value) is too low, the polymer particles may be destroyed when compressed. If the compression modulus (10% K value, 20% K value, and 30% K value) is too high, the connection resistance value between the electrodes may increase.
  • the compression elastic modulus (10% K value, 20% K value, and 30% K value) can be measured as follows.
  • the compression elastic modulus can be obtained by the following formula.
  • the micro compression tester for example, “Fischer Scope H-100” manufactured by Fischer is used.
  • K value (N / mm 2 ) (3/2 1/2 ) ⁇ F ⁇ S ⁇ 3 / 2 ⁇ R ⁇ 1/2
  • F Load value (N) when the polymer particles are 10%, 20% or 30% compressively deformed
  • S Compression displacement (mm) when the polymer particles are 10%, 20% or 30% compressively deformed
  • R radius of polymer particles (mm)
  • the above-mentioned compression elastic modulus universally and quantitatively represents the hardness of the polymer particles.
  • the hardness of the polymer particles can be expressed quantitatively and uniquely.
  • the electroconductive particle which concerns on this invention has the said polymer particle and the metal layer which has coat
  • the metal constituting the metal layer is not particularly limited.
  • metals include gold, silver, copper, platinum, zinc, iron, lead, tin, aluminum, cobalt, indium, nickel, chromium, titanium, antimony, bismuth, germanium, cadmium, palladium, tin-lead alloy, tin -Copper alloy, tin-silver alloy or tin-lead-silver alloy.
  • the metal which comprises the said metal layer is nickel, copper, palladium, or gold
  • the method for forming the metal layer on the surface of the polymer particles is not particularly limited.
  • Examples of the method for forming the metal layer include methods such as electroless plating, electroplating, and sputtering.
  • the method of forming the said metal layer on the surface of a polymer particle is a method of forming by electroless plating.
  • the outer surface of the metal layer of the conductive particles is preferably a gold layer, a nickel layer, or a palladium layer, and is preferably a nickel layer or a palladium layer. Furthermore, the metal layer is preferably formed of a nickel layer and a palladium layer laminated on the surface of the nickel layer. By forming these preferable metal layers, the connection resistance value between the electrodes connected by the conductive particles is lowered. Further, when the outer surface of the metal layer is a nickel layer or a palladium layer, the metal oxide covering the electrode surface can be easily removed when the conductive particles are brought into contact with the electrode. For this reason, the outer surface of the metal layer and the metal on the electrode surface easily come into contact with each other, and the connection resistance value is lowered.
  • the outer surface of the metal layer is preferably a metal layer containing nickel, a metal layer containing palladium, or a metal layer containing a low melting point metal.
  • the metal oxide covering the electrode surface can be easily removed, and the outer surface of the metal layer and the electrode surface Since the contact with the metal becomes easy, the connection resistance value is lowered.
  • the outer surface of the metal layer is a metal layer containing a low-melting-point metal, the metal layer containing the low-melting-point metal and the electrode are brought into surface contact instead of point contact by reflow, so that the connection resistance value is lowered.
  • the connection target members using conductive particles with a low melting point metal layer formed on the surface of the polymer particles the low melting point metal layer cracks even if an impact such as dropping is applied. Is less likely to occur.
  • the metal layer may be a single layer or may have a laminated structure of two or more layers.
  • the inner layer / outer layer may be a nickel layer / gold layer, a nickel layer / palladium layer, or a copper layer / low melting point metal layer.
  • a low melting point metal layer that is, a metal layer containing a low melting point metal, a metal layer containing tin, a metal layer containing tin and silver, a metal layer containing tin and copper, a metal layer containing tin, silver and copper, or Examples thereof include a metal layer containing tin, silver and nickel.
  • the low melting point metal refers to a metal having a melting point of 300 ° C. or lower. Moreover, it is preferable that 50 weight% or more of tin is contained in 100 weight% of the metal contained in the metal layer containing the low melting point metal, more preferably 70 weight% or more, and 90 weight% or more. Is more preferable.
  • the outer surface of the metal layer covering the surface of the polymer particles is a low melting point metal layer, stress applied to the conductive particles can be relieved, so that the electrodes can be easily connected.
  • connection target member When the connection target member is electrically connected to the outer surface of the metal layer of the conductive particle using the polymer particle according to the present invention by the conductive particle having the low melting point metal layer formed, Even if an impact is applied, cracks are unlikely to occur in the low melting point metal layer. For this reason, electrical conductivity reliability can be improved.
  • the thickness of the metal layer is preferably in the range of 5 to 70,000 nm.
  • a more preferable lower limit of the thickness of the metal layer is 10 nm, a further preferable lower limit is 20 nm, a more preferable upper limit is 40,000 nm, a more preferable upper limit is 500 nm, and a further preferable upper limit is 200 nm. If the thickness of the metal layer is too thin, sufficient conductivity may not be obtained. If the thickness of the metal layer is too thick, the difference in coefficient of thermal expansion between the polymer particles and the metal layer becomes large, and the metal layer may be easily peeled off from the polymer particles. When the said metal layer has a laminated structure, the thickness of the said metal layer shows the sum total of the thickness of each metal layer.
  • the compression recovery rate of the conductive particles is preferably 50% or less, preferably 45% or less, and more preferably 40% or less. If the compression recovery rate exceeds 50%, the anisotropic conductive material may peel from the substrate or the like due to the repulsive force of the conductive particles used for connection between the electrodes. As a result, the connection resistance value between the electrodes may increase. When the compression recovery rate of the conductive particles is 45% or less, the connection resistance value between the electrodes can be further reduced.
  • the compression recovery rate of the conductive particles is preferably 5% or more, more preferably 10% or more, and even more preferably 20% or more.
  • the anisotropic conductive material according to the present invention includes the conductive particles and a binder resin.
  • the binder resin is not particularly limited.
  • the binder resin for example, an insulating resin is used.
  • the binder resin include vinyl resins, thermoplastic resins, curable resins, thermoplastic block copolymers, and elastomers.
  • the said binder resin only 1 type may be used and may be used together.
  • the vinyl resin include vinyl acetate resin, acrylic resin, and styrene resin.
  • the thermoplastic resin include polyolefin resin, ethylene-vinyl acetate copolymer or polyamide resin.
  • the curable resin include an epoxy resin, a urethane resin, a polyimide resin, or 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, or a styrene- Examples include hydrogenated products of isoprene-styrene block copolymers.
  • elastomer examples include styrene-butadiene copolymer rubber or acrylonitrile-styrene block copolymer rubber.
  • Anisotropic conductive materials include, for example, fillers, extenders, softeners, plasticizers, polymerization catalysts, curing catalysts, colorants, antioxidants, thermal stabilizers, light stabilizers, in addition to conductive particles and binder resins.
  • Various additives such as an agent, an ultraviolet absorber, a lubricant, an antistatic agent or a flame retardant may be contained.
  • the method for dispersing the conductive particles in the binder resin may be any conventionally known dispersion method and is not particularly limited.
  • a method for dispersing the conductive particles in the binder resin for example, after adding the conductive particles in the binder resin, kneading and dispersing with a planetary mixer or the like, the conductive particles in water or an organic solvent. After uniformly dispersing using a homogenizer, etc., add into the binder resin, knead and disperse with a planetary mixer, etc., or after diluting the binder resin with water or an organic solvent, add conductive particles And a method of kneading and dispersing with a planetary mixer or the like.
  • the anisotropic conductive material of the present invention can be used as an anisotropic conductive paste, anisotropic conductive ink, anisotropic conductive adhesive, anisotropic conductive film, or anisotropic conductive sheet.
  • anisotropic conductive material containing the conductive particles of the present invention is used as a film-like adhesive such as an anisotropic conductive film or an anisotropic conductive sheet
  • the film-like shape containing the conductive particles is used.
  • a film-like adhesive that does not contain conductive particles may be laminated on the adhesive.
  • connection structure can be obtained by connecting the connection target member using the conductive particles of the present invention or an anisotropic 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 that electrically connects the first and second connection target members.
  • the connection structure is preferably formed of the conductive particles of the invention or 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.
  • connection target member examples include electronic components such as semiconductor chips, capacitors, and diodes, and circuit boards such as printed boards, flexible printed boards, and glass boards.
  • the electrode provided on the connection target member examples include a metal electrode such as a gold electrode, a nickel electrode, a tin electrode, an aluminum electrode, a copper electrode, a molybdenum electrode, or a tungsten electrode.
  • the electrode is preferably a gold electrode, a nickel electrode, a tin electrode, or a copper electrode.
  • the connection object member is a glass substrate, the electrode is preferably an aluminum electrode, a copper electrode, a molybdenum electrode, or a tungsten electrode.
  • the said electrode is an aluminum electrode, the electrode formed only with aluminum may be sufficient and the electrode by which the aluminum layer was laminated
  • the metal oxide examples include indium oxide doped with a trivalent metal element, zinc oxide doped with a trivalent metal element, and the like. Examples of the trivalent metal element include Sn, Al, and Ga.
  • connection target member on which the metal electrode is formed is electrically connected using the conductive particles of the present invention or the anisotropic conductive material containing the conductive particles and a binder resin, the connection resistance value is lowered. .
  • an aluminum electrode or a copper electrode is preferable.
  • FIG. 1 is a front sectional view schematically showing an example of a connection structure using conductive particles according to an embodiment of the present invention.
  • a printed circuit board 4 has a structure in which a printed circuit board 4 is connected to an upper surface of a glass substrate 2 via an anisotropic conductive film 3 including a plurality of conductive particles 5.
  • a plurality of electrodes 2 a are provided on the upper surface of the glass substrate 2.
  • a plurality of electrodes 4 a are provided on the lower surface of the printed circuit board 4.
  • the electrode 2 a and the electrode 4 a are connected by a plurality of conductive particles 5.
  • a two-layer flexible printed circuit board is used as the printed circuit board 4.
  • a connection target member other than the two-layer flexible printed board may be used.
  • FIG. 1 the printed circuit board 4 and the conductive particles 5 are schematically shown.
  • connection between the electrodes 2a and 4a is usually performed by placing the conductive particles 5 on the electrode 2a of the glass substrate 2 and then stacking the printed circuit board 4 on the glass substrate 2 so that the electrodes 2a and 4a face each other. It is performed by combining and pressurizing.
  • the conductive particles 5 are compressed by pressurization.
  • the contact portion between the conductive particles and the electrode of the connection structure shown in FIG. Indentations are likely to be formed at the portions where the conductive particles 5 of 2a and 4a are in contact. For this reason, the connection resistance value between the electrodes 2a and 4a can be made sufficiently low. Further, the gap A is difficult to occur.
  • the following materials were prepared as monomer components for obtaining polymer particles.
  • Example 1 (Preparation of polymer seed particle dispersion) In a separable flask, 2500 g of ion-exchanged water, 250 g of styrene, 50 g of octyl mercaptan, and 0.5 g of sodium chloride were added and stirred under a nitrogen atmosphere. Then, it heated at 70 degreeC, 2.5 g of potassium peroxide was added, and polymer seed particle
  • Dimethylol-tricyclodecane diacrylate 38 g, divinylbenzene 152 g, benzoyl peroxide 2.6 g, lauryl sulfate triethanolamine 10 g, and ethanol 130 g were added to ion-exchanged water 1000 g and stirred to obtain an emulsion. .
  • the resulting emulsion was added to the polymer seed particle dispersion several times and stirred for 12 hours. Thereafter, 500 g of a 5% by weight aqueous solution of polyvinyl alcohol was added and reacted for 9 hours in a nitrogen atmosphere at 85 ° C. to obtain polymer particles.
  • the obtained resin composition was applied to a 50 ⁇ m-thick PET (polyethylene terephthalate) film having one surface peeled 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.
  • the two-layer flexible printed circuit board (width 2cm, length 1cm) provided with the same aluminum electrode was bonded after aligning so that electrodes might overlap.
  • 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.
  • the 2 layer flexible printed circuit board by which the aluminum electrode was directly formed in the polyimide film was used.
  • Examples 2 to 16 and Comparative Examples 1 to 4 In the same manner as in Example 1 except that the types of monomer components used in the production of the polymer particles and the blending amounts thereof were changed as shown in Tables 1 and 2 below, a polymer seed particle dispersion, Polymer particles, conductive particles, anisotropic conductive films, and connection structures were produced.
  • Example 17 The following electroless nickel plating process was performed using the polymer particles obtained in Example 1.
  • Electroless nickel plating process The resulting polymer particles were treated with a 10 wt% solution of ion adsorbent for 5 minutes and then added to a 0.01 wt% palladium sulfate aqueous solution. Thereafter, dimethylamine borane was added for reduction treatment, filtration, and washing to obtain polymer particles with palladium attached.
  • a 1% by weight sodium succinate solution in which sodium succinate was dissolved in 500 mL of ion-exchanged water was prepared.
  • 10 g of polymer particles with palladium attached were added and mixed to prepare a slurry.
  • Sulfuric acid was added to the slurry, and the pH of the slurry was adjusted to 5.
  • a nickel plating solution containing 10% by weight of nickel sulfate, 10% by weight of sodium hypophosphite, 4% by weight of sodium hydroxide and 20% by weight of sodium succinate was prepared.
  • the slurry adjusted to pH 5 was heated to 80 ° C., and then the nickel plating solution was continuously added dropwise to the slurry and stirred for 20 minutes to advance the plating reaction. After confirming that hydrogen was no longer generated, the plating reaction was completed.
  • a late nickel plating solution containing 20% by weight of nickel sulfate, 5% by weight of dimethylamine borane and 5% by weight of sodium hydroxide was prepared.
  • the late nickel plating solution was continuously added dropwise to the solution that had undergone the plating reaction with the previous nickel plating solution, and the plating reaction was allowed to proceed by stirring for 1 hour. In this way, a nickel layer was formed on the surface of the polymer particles to obtain conductive particles.
  • the nickel layer had a thickness of 0.1 ⁇ m.
  • An anisotropic conductive film and a connection structure were produced in the same manner as in Example 1 except that the obtained conductive particles were used.
  • Example 18 The following electroless palladium plating process was performed using the conductive particles obtained in Example 17 except that the thickness of the nickel layer was adjusted to 0.07 ⁇ m.
  • Electroless palladium plating process 10 g of the obtained conductive particles were added to 500 mL of ion-exchanged water and sufficiently dispersed by an ultrasonic treatment machine to obtain a particle suspension. While stirring the suspension at 50 ° C., 0.02 mol / L of palladium sulfate, 0.04 mol / L of ethylenediamine as a complexing agent, 0.06 mol / L of sodium formate as a reducing agent, and pH 10.0 containing a crystal modifier. The electroless plating solution was gradually added to perform electroless palladium plating. When the thickness of the palladium layer reached 0.03 ⁇ m, the electroless palladium plating was finished. Next, by washing and vacuum drying, conductive particles having a palladium layer laminated on the surface of the nickel layer were obtained.
  • An anisotropic conductive film and a connection structure were produced in the same manner as in Example 1 except that the obtained conductive particles were used.
  • the nickel layer had a thickness of 0.07 ⁇ m, and the palladium layer had a thickness of 0.03 ⁇ m.
  • Example 19 An electroless nickel plating step was performed in the same manner as in Example 17 except that the polymer particles obtained in Example 1 were changed to the polymer particles obtained in Example 5, and nickel was formed on the surface of the polymer particles. A layer was formed to obtain conductive particles.
  • An anisotropic conductive film and a connection structure were produced in the same manner as in Example 1 except that the obtained conductive particles were used.
  • Example 20 The nickel layer was prepared to have a thickness of 0.07 ⁇ m, and the conductive particles obtained in Example 17 were changed to the conductive particles obtained in Example 19 in the same manner as in Example 18, An electroless palladium plating step was performed to obtain conductive particles having a palladium layer laminated on the surface of the nickel layer.
  • An anisotropic conductive film and a connection structure were produced in the same manner as in Example 1 except that the obtained conductive particles were used.
  • Examples 21 to 46 and Comparative Examples 5 to 8 In the same manner as in Example 1 except that the types of monomer components used in the production of the polymer particles and the blending amounts thereof were changed as shown in Tables 3 and 4 below, a polymer seed particle dispersion, Polymer particles, conductive particles, anisotropic conductive films, and connection structures were produced.
  • Example 47 In a dispersion obtained by uniformly dispersing 1252 g of ion-exchanged water and 2135 g of a 5.5% by weight aqueous solution of polyvinyl alcohol, 38 g of dimethylol-tricyclodecane diacrylate, 152 g of divinylbenzene, and perbutyl O (as a polymerization initiator) 5.9 g (manufactured by Nippon Oil & Fats Co., Ltd.) was added and mixed to obtain a mixture.
  • the obtained mixed solution was polymerized at 70 ° C. for 5 hours, and then the particles were taken out by suction filtration. The particles were washed with ion-exchanged water and acetone to remove the dispersion medium and then dried to obtain polymer particles.
  • the average particle size of the obtained polymer particles was 240 ⁇ m, and the CV value was 0.42%.
  • the polymer particles were electroless nickel plated to form a base nickel plating layer having a thickness of 0.3 ⁇ m on the surface of the polymer particles.
  • the polymer particles on which the base nickel plating layer was formed were subjected to electrolytic copper plating to form a copper layer having a thickness of 10 ⁇ m.
  • electroplating was performed using an electrolytic plating solution containing tin and silver to form a low melting point metal layer having a thickness of 25 ⁇ m.
  • the average particle diameter of the conductive particles was 310 ⁇ m, and the CV value was 1.05%.
  • the contents of tin and silver in the metal layer on the surface of the polymer particles were determined by analysis using a fluorescent X-ray analyzer (“EDX-800HS” manufactured by Shimadzu Corporation).
  • Example 48 to 50 and Comparative Example 9 Polymer particles and conductive particles were produced in the same manner as in Example 47 except that the types of monomer components used in the production of the polymer particles and the blending amounts thereof were changed as shown in Table 5 below. did.
  • Example 51 to 90 Polymer particles were obtained in the same manner as in Example 1 except that the types of monomer components used in the production of the polymer particles and the blending amounts thereof were changed as shown in Tables 6 to 8 below.
  • an electroless nickel plating step was performed in the same manner as in Example 17 to form a nickel layer on the surface of the polymer particles, thereby obtaining conductive particles.
  • An anisotropic conductive film and a connection structure were produced in the same manner as in Example 1 except that the obtained conductive particles were used.
  • Example 91 to 130 Polymer particles were obtained in the same manner as in Example 1 except that the types of monomer components used in the preparation of the polymer particles and the blending amounts thereof were changed as shown in Tables 8 to 10 below.
  • the electroless nickel plating step and the electroless palladium plating step were performed in the same manner as in Examples 17 and 18 except that the obtained polymer particles were used so that the nickel layer had a thickness of 0.07 ⁇ m. Conductive particles were obtained in which a palladium layer was laminated on the surface of the nickel layer.
  • An anisotropic conductive film and a connection structure were produced in the same manner as in Example 1 except that the obtained conductive particles were used.
  • Average particle diameter of polymer particles The average particle diameter of the obtained polymer particles was measured using a Coulter counter (manufactured by Beckman Coulter).
  • compression elastic modulus of polymer particles The compression elastic modulus (10% K value, 20% K value and 30% K value) of the obtained polymer particles was measured using a micro compression tester (Fischer Scope H manufactured by Fischer). -100 ").
  • connection resistance value The connection resistance value between the opposing electrodes of the obtained connection structure was measured by a four-terminal method. The connection resistance value was evaluated according to the following evaluation criteria.
  • Connection resistance value is 2.0 ⁇ or less ⁇ : Connection resistance value exceeds 2.0 ⁇ , 3.0 ⁇ or less ⁇ : Connection resistance value exceeds 3.0 ⁇ , 5.0 ⁇ or less ⁇ : Connection resistance value is 5. Over 0 ⁇
  • the electrode provided on the glass substrate was observed from the glass substrate side of the obtained connection structure, and the presence or absence of formation of the impression of the electrode in contact with the conductive particles was determined as follows. It was evaluated according to the evaluation criteria. Moreover, the presence or absence of the space
  • Drop strength test A silicon chip (length 6 mm ⁇ width 6 mm) provided with 112 electrodes (diameter 280 ⁇ m) at intervals of 0.5 mm was prepared. A flux (“WS-9160-M7” manufactured by Cookson Electronics Co., Ltd.) was applied on the electrode of this silicon chip. The obtained electroconductive particle was arrange
  • a printed circuit board provided with a copper electrode (diameter 305 ⁇ m) was prepared.
  • a solder paste (“M705-GRN360-K2-V” manufactured by Senju Metal Industry Co., Ltd.) was applied to the printed circuit board. Fifteen silicon chips with conductive particles mounted on electrodes were mounted on a printed circuit board coated with solder paste to obtain a connection structure.
  • connection structure was subjected to a drop strength test and evaluated according to the following evaluation criteria.
  • the electrode is an electrode in which a copper layer, a nickel-phosphorus layer, and a gold layer are sequentially formed toward the outer surface.
  • Tables 1 to 4 and 6 to 10 showing the evaluation results of Examples 1 to 46 and 51 to 130 show that good results can be obtained when a two-layer flexible printed circuit board is used. Even when a three-layer flexible printed circuit board was used instead of the two-layer flexible printed circuit board, it was confirmed that good results were obtained by using the polymer particles and conductive particles of Examples 1 to 46 and 51 to 130. Further, it can be understood from Table 5 showing the evaluation results of Examples 47 to 50 that the disconnection of the electrode can be suppressed even when a drop impact is given.

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Abstract

Les particules de polymère ci-décrites permettent d'améliorer la fiabilité de la conduction électrique quand des éléments de connexion selon l'invention sont électriquement connectés les uns aux autres par des particules conductrices obtenues par formation d'une couche métallique sur les surfaces des particules de polymère ou d'un matériau conducteur anisotrope contenant les particules conductrices. Des particules conductrices contenant les particules de polymère selon l'invention sont également décrites. Plus spécifiquement, une particule de polymère est obtenue par polymérisation d'un monomère qui est un composé alicyclique ayant au moins deux structures de cycle. Une particule conductrice (5) comprend la particule de polymère et une couche de métal revêtue sur la surface de la particule de polymère.
PCT/JP2009/056226 2008-03-27 2009-03-27 Particule de polymère, particule conductrice, matériau conducteur anisotrope et structure de connexion WO2009119788A1 (fr)

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