WO2007058159A1 - Composition d'adhésif, matériau de connexion de circuits, structure de connexion et procédé de connexion d'éléments de circuits - Google Patents

Composition d'adhésif, matériau de connexion de circuits, structure de connexion et procédé de connexion d'éléments de circuits Download PDF

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Publication number
WO2007058159A1
WO2007058159A1 PCT/JP2006/322628 JP2006322628W WO2007058159A1 WO 2007058159 A1 WO2007058159 A1 WO 2007058159A1 JP 2006322628 W JP2006322628 W JP 2006322628W WO 2007058159 A1 WO2007058159 A1 WO 2007058159A1
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WIPO (PCT)
Prior art keywords
circuit
particles
connection
adhesive composition
conductive
Prior art date
Application number
PCT/JP2006/322628
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English (en)
Japanese (ja)
Inventor
Tomomi Yokozumi
Masaki Fujii
Kenzou Takemura
Original Assignee
Hitachi Chemical Company, Ltd.
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 Hitachi Chemical Company, Ltd. filed Critical Hitachi Chemical Company, Ltd.
Priority to KR1020117009581A priority Critical patent/KR20110048079A/ko
Priority to KR1020087011623A priority patent/KR101049609B1/ko
Priority to CN2006800430380A priority patent/CN101309993B/zh
Priority to JP2007545234A priority patent/JP4877230B2/ja
Publication of WO2007058159A1 publication Critical patent/WO2007058159A1/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
    • H01R4/00—Electrically-conductive connections between two or more conductive members in direct contact, i.e. touching one another; Means for effecting or maintaining such contact; Electrically-conductive connections having two or more spaced connecting locations for conductors and using contact members penetrating insulation
    • H01R4/04—Electrically-conductive connections between two or more conductive members in direct contact, i.e. touching one another; Means for effecting or maintaining such contact; Electrically-conductive connections having two or more spaced connecting locations for conductors and using contact members penetrating insulation using electrically conductive adhesives
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
    • C09J9/02—Electrically-conducting adhesives
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    • 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
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    • H01R12/00—Structural associations of a plurality of mutually-insulated electrical connecting elements, specially adapted for printed circuits, e.g. printed circuit boards [PCB], flat or ribbon cables, or like generally planar structures, e.g. terminal strips, terminal blocks; Coupling devices specially adapted for printed circuits, flat or ribbon cables, or like generally planar structures; Terminals specially adapted for contact with, or insertion into, printed circuits, flat or ribbon cables, or like generally planar structures
    • H01R12/50—Fixed connections
    • H01R12/51—Fixed connections for rigid printed circuits or like structures
    • H01R12/52—Fixed connections for rigid printed circuits or like structures connecting to other rigid printed circuits or like structures
    • 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
    • H05K2201/0218—Composite particles, i.e. first metal coated with second metal
    • 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
    • H05K2201/0263—Details about a collection of particles
    • H05K2201/0266—Size distribution

Definitions

  • the present invention relates to an adhesive composition, a circuit connection material and a connection structure, and a circuit member connection method.
  • circuit electrodes formed on circuit members have been increased in density and definition.
  • fine pitches such as multiple electrodes and narrow pitches. Since connection between circuit members formed with fine circuits is difficult with conventional solder rubber connectors, an adhesive composition having anisotropic conductivity is used.
  • the above-mentioned adhesive composition is generally composed of an adhesive component and conductive particles dispersed and dispersed therein.
  • the adhesive composition is arranged between a pair of circuit members arranged opposite to each other, and the circuit electrodes facing each other are electrically connected to each other by pressurizing the whole in the direction of sandwiching the adhesive composition.
  • a pair of circuit members are bonded and fixed between the adjacent electrodes while ensuring electrical insulation.
  • various conductive fine particles are used as the conductive particles of the adhesive composition.
  • examples thereof include fine metal powder, or plastic fine particles whose surface is coated with a metal thin film.
  • the metal fine powder when metal fine powder is used as the conductive particles, the metal fine powder has a sufficiently high hardness, so that even if an oxide film is formed on the surface of the circuit electrode, This The circuit electrodes can be connected by breaking. However, it can be said that metal fine powders are generally not suitable for fine pitching in this case where the particle size distribution is wide.
  • the resistance value of the connection portion increases with time. This is considered to be due to the fact that the metal fine powder cannot sufficiently follow the increase in the distance between the circuit electrodes due to temperature fluctuations and relaxation of the connection state of the connection structure.
  • the linear thermal expansion coefficient of fine metal powder is smaller than that of the cured product of the adhesive component, and thus this phenomenon force S may occur after a thermal cycle test in which temperature rise and fall are repeated.
  • Patent Documents 1 and 2 describe conductive particles in which protrusions are provided on the surface of a conductive thin film.
  • Patent Document 3 describes a conductive particle in which metal particles are further adhered to the surface of a metal thin film.
  • Patent Documents 4 and 5 describe conductive particles obtained by metal plating on uneven plastic particles.
  • Patent Document 1 Japanese Patent Laid-Open No. 2000-195339
  • Patent Document 2 Japanese Patent Laid-Open No. 2000-243132
  • Patent Document 3 Japanese Patent Laid-Open No. 63-301408
  • Patent Document 4 Japanese Patent Laid-Open No. 4 36902
  • Patent Document 5 Japanese Patent Laid-Open No. 11-73818
  • the conductive particles of Patent Documents 1 and 2 are manufactured by depositing protrusions in an electroless plating process for forming a metal thin film. In this case, it is difficult to sufficiently control the protrusion size and the number of protrusions. For this reason, it can be said that it is difficult to achieve sufficiently high connection reliability due to the unevenness of the protrusions.
  • the conductive particles of Patent Document 3 have insufficient adhesion between the metal thin film and the metal particles adhering to the surface, and the metal particles may fall off. If the metal particles fall off, the initial resistance value of the connection structure becomes high or the insulation with the adjacent circuit electrode becomes insufficient, making it difficult to achieve sufficiently high connection reliability.
  • the conductive particles of Patent Documents 4 and 5 have irregularities formed of plastic particles themselves. For this reason, when an oxide film is formed on the surface of the circuit electrode, it cannot be fully penetrated, and the initial resistance value of the connection structure may be increased.
  • the present invention has been made in view of such a situation, and even if the electrode to be connected is easily formed with an oxide film on the surface and has a metal material force, the initial resistance of the connection structure is provided. It is an object of the present invention to provide an adhesive composition capable of sufficiently reducing the value and a circuit connecting material using the same.
  • the adhesive composition of the present invention comprises an adhesive component and conductive particles dispersed in the adhesive component, and the conductive particles constitute a central portion of the conductive particles.
  • arranged on the surface of the substrate particles means that the metal fine particles are arranged in contact with the surface of the substrate particles. It is meant to include things that are placed in a state of being touched and touched. Multiple metal particles
  • the conductive particles disposed at the above positions can be produced by forming metal adhesion layers by plating after attaching metal fine particles to the substrate particles.
  • the conductive particles of the adhesive composition of the present invention include a metal plating layer that integrally covers the base particles and the metal fine particles. For this reason, the metal fine particles having high adhesion between the metal fine particles and the substrate particles are sufficiently suppressed from falling off the conductive particle force. As a result, the circuit electrodes can be more reliably electrically connected to each other and sufficiently insulated from the adjacent circuit electrodes.
  • the average particle size of the metal fine particles is preferably 200 to 1000 nm.
  • the average particle size of the base particles is preferably 1 to 10 / ⁇ ⁇ .
  • the “average particle diameter” in the present invention means a value measured as follows. That is, the arbitrarily selected metal fine particles are observed with a scanning electron microscope (S ⁇ ), and the maximum diameter and the minimum diameter are measured. The square root of the product of the maximum and minimum diameters is the particle size of the particles. The particle size is measured as described above for 50 arbitrarily selected particles, and the average value is taken as the average particle size.
  • the number of metal fine particles is preferably 10 to 40 per base particle. Further, when the number of metal fine particles is 10 to 40, there is an advantage that both suppression of an increase in connection resistance value and insulation with adjacent circuit electrodes are achieved at a high level.
  • the number of metal fine particles per base particle means a value measured as follows. In other words, arbitrarily selected conductive particles The number of protrusions on the surface of the conductive particles that can be imaged and observed by EM is counted as the number of metal fine particles. The number of metal particles of one conductive particle is calculated by doubling the obtained count. The number of metal fine particles is measured as described above for 50 arbitrarily selected conductive particles, and the average value is taken as the number of metal fine particles per substrate particle.
  • the base particles have a material strength with a compressive elastic modulus of 100 to 1000 kgf Zmm 2 at 20% compression deformation of the particle diameter.
  • the substrate particles have the hardness as described above, even if an oxide film is formed on the surface of the circuit electrode, the metal fine particles disposed on the inner side of the metal plating layer are formed on the oxide film. Can be broken through more reliably. In addition to this, even if the distance between the circuit electrodes becomes wider due to temperature fluctuations, the substrate particles can sufficiently follow the increase in the distance between the circuit electrodes. Therefore, the increase in connection resistance can be sufficiently suppressed.
  • the base particles preferably have a compression recovery rate force of 0% or more after being compressed at a maximum load of 5 mN. If the base particles have a compression recovery rate as described above, the base particles sufficiently follow the increase in the distance between the circuit electrodes even if the distance between the circuit electrodes becomes wide due to temperature fluctuations. be able to. Therefore, the increase in connection resistance can be sufficiently suppressed.
  • the circuit connection material of the present invention is the adhesive composition of the present invention, which bonds circuit members together and electrically connects circuit electrodes of each circuit member.
  • connection structure of the present invention includes a pair of circuit members arranged opposite to each other and a cured product of the circuit connection material of the present invention, and each circuit member is interposed between the pair of circuit members. A connecting portion that bonds the circuit members together so that the circuit electrodes are electrically connected to each other.
  • the present invention also includes the circuit connection material of the present invention interposed between a pair of circuit members arranged opposite to each other, and the whole is heated and pressurized to form a cured product of the circuit connection material.
  • the pair of circuit members and the connection portion are formed.
  • an oxide film is easily formed on the surface of the electrode to be connected! ⁇ Metal material Even if it is strong, it is possible to provide an adhesive composition that can sufficiently reduce the initial resistance value of the connection structure, and a circuit connection material using the same. Furthermore, according to the present invention, it is possible to provide a connection structure in which circuit members are connected with a low connection resistance, and a circuit member connection method for obtaining the connection structure.
  • FIG. 1 is a cross-sectional view showing a state in which a circuit connecting material according to the present invention is used between circuit electrodes and the circuit electrodes are connected to each other.
  • FIG. 2 is a cross-sectional view showing an embodiment of a circuit connection material according to the present invention.
  • FIG. 3 is a cross-sectional view showing one embodiment of conductive particles contained in the circuit connection material according to the present invention.
  • FIG. 4 is a cross-sectional view showing a state in which the circuit connection material according to the present invention is provided on a support.
  • FIG. 5 is a cross-sectional view showing a state in which the circuit connecting material according to the present invention is supported by a support.
  • FIG. 6 is a schematic diagram showing an embodiment of a circuit member connecting method according to the present invention in a schematic sectional view.
  • (meta) attalate means “attalate” and the corresponding “metatalate”.
  • FIG. 1 is a schematic cross-sectional view showing a connection structure in which the adhesive composition according to the present invention is used as a circuit connection material and circuit electrode members are connected.
  • the connection structure 100 shown in FIG. 1 includes a first circuit member 30 and a second circuit member 40 that face each other, and is between the first circuit member 30 and the second circuit member 40. Is provided with a connecting portion 50a for connecting them.
  • the first circuit member 30 includes a circuit board (first circuit board) 31 and a circuit electrode (first circuit electrode) 32 formed on the main surface 31a of the circuit board 31.
  • the second circuit member 40 includes a circuit board (second circuit board) 41 and a circuit electrode (second circuit electrode) 42 formed on the main surface 41 a of the circuit board 41.
  • the surfaces of the circuit electrodes 32 and 42 are flat.
  • “the surface of the circuit electrode is flat” means that the unevenness of the surface of the circuit electrode is sufficiently small, and the unevenness of the surface is preferably 20 nm or less.
  • the connecting portion 50a includes a cured product 20a of an adhesive component contained in the circuit connecting material and conductive particles 10 dispersed therein.
  • the circuit electrode 32 and the circuit electrode 42 facing each other are electrically connected through the conductive particles 10.
  • the conductive particles are in direct contact with both the 10-force circuit electrodes 32 and 42.
  • connection resistance between the circuit electrodes 32 and 42 is sufficiently reduced, and a good electrical connection between the circuit electrodes 32 and 42 becomes possible.
  • the cured product 20a has electrical insulation, and insulation between adjacent circuit electrodes is ensured. Therefore, the current flow between the circuit electrodes 32 and 42 can be made smooth, and the functions of the circuit can be fully exhibited.
  • FIG. 2 is a schematic cross-sectional view showing a preferred embodiment when the adhesive composition according to the present invention is used as a circuit connecting material.
  • the shape of the circuit connecting material 50 shown in FIG. 2 is a film shape.
  • the circuit connecting material 50 is dispersed in the adhesive component 20 and the adhesive component 20.
  • the circuit connecting material 50 is produced by applying an adhesive composition containing an adhesive component and conductive particles on a film-like support using a coating apparatus, and drying with hot air for a predetermined time.
  • FIG. 3 is a cross-sectional view showing the form of conductive particles contained in the circuit connection material according to the present invention.
  • the conductive particle 10 shown in FIG. 3 covers the surface of the base particle 1 constituting the central portion, the plurality of metal fine particles 2 provided on the base particle 1, and the base particle 1 and the metal fine particle 2. And a metal plating layer 3 formed as described above. Metal fine particles 2 are located inside metal plating layer 3
  • Examples of the material of the base particle 1 include metals and organic polymer compounds.
  • Examples of the metal constituting the base particle 1 include nickel, copper, gold, silver, cobalt, and alloys thereof.
  • Examples of the organic polymer compound constituting the base particle 1 include acrylic resin, styrene resin, benzoguanamine resin, silicone resin, polybutadiene resin, and copolymers thereof. Even so.
  • connection portion may increase. From the viewpoint of efficiently preventing such an increase in resistance value, it is preferable to use particles having organic polymer compound power as the base particle 1.
  • the particles having the organic polymer compound force tend to recover to a spherical shape due to the flat shape force even if the particles are crushed into a flat shape between the circuit electrodes when the circuit electrodes are connected to each other. For this reason, the conductive particles 10 can sufficiently follow the expansion of the circuit electrode interval due to temperature fluctuations. From this viewpoint, it is preferable that the compression recovery rate after the base particle 1 is compressed at the maximum load of 5 mN is 40% or more.
  • the particles made of an organic compound having a compression recovery rate as described above include acrylic resin, styrene resin, benzoguanamine resin, silicone resin, polybutadiene resin, or particles having a copolymer power thereof. Raising It is done. If the compression recovery rate is less than 40%, there is a tendency that the follow-up to the expansion of the distance between the circuit electrodes is insufficient.
  • the compression recovery rate can be measured with an H-100 micro hardness tester manufactured by Fischer Instrument Co., Ltd.
  • the material of the base particles 1, at 20% compression deformation of particle diameter, even for use preferably has a 100 ⁇ 1 OOOkgf Zmm 2, more preferably compressive modulus of 100 ⁇ 800kgf Zmm 2 Is done.
  • the particles made of an organic compound having the above hardness include acrylic resin, styrene resin, benzoguanamine resin, silicone resin, polybutadiene resin, or particles having a copolymer power thereof. .
  • the compression elastic modulus at the time of 20% compression deformation is less than lOOkgfZmm 2
  • the oxide film on the surface is sufficiently penetrated. Cannot be achieved, and the resistance value of the connection portion tends to increase.
  • the compressive modulus exceeds 1 OOOkgfZmm 2
  • the substrate particles 1 tend not to be sufficiently deformed into a flat shape when the opposing circuit electrodes are pressurized. If the deformation of the base particle 1 is insufficient, the contact area with the circuit electrode becomes insufficient, and the resistance value of the connection portion becomes high.
  • the substrate particles 1 when the substrate particles 1 are pressed at a high pressure in order to sufficiently deform the substrate particles 1 into a flat shape, the particles may be crushed and connection may be insufficient.
  • the compression elastic modulus can be measured with an H-100 micro hardness tester manufactured by Fisher Instruments Co., Ltd.
  • the base particles 1 may be the same or different types of materials between the particles, and the same particles may be used alone or in combination of two or more types. ,.
  • the average particle diameter of the base particle 1 is a force 1 that can be appropriately designed depending on the application and the like: 1 to: L0 m is preferable 2 to 8 ⁇ m is more preferable 3 More preferably, it is ⁇ 5 ⁇ m.
  • L0 m is preferable 2 to 8 ⁇ m is more preferable 3 More preferably, it is ⁇ 5 ⁇ m.
  • the metal constituting the metal fine particles for example, Ni, Ag, Au, Cu, Co, Zn, Al, Sb, U, Ga, Ca, Sn, Se, Fe, Th, Be, Mg, Mn and These alloys are mentioned. Of these metals, Ni, Ag, Au, and Cu are preferred from the viewpoint of conductivity and corrosion resistance, and Ni is more preferred. These can be used alone or in combination of two or more.
  • the average particle size of the metal fine particles 2 is a force that can be appropriately designed according to the application and the like.
  • the force is 200-10 OOnm, preferably S.
  • the force is preferably 400 to 800 nm, more preferably S, more preferably 400 to 500 nm. More preferably.
  • the average particle size is less than 200 nm, when connecting a metal circuit electrode having an oxide film formed on the surface, the oxide film cannot be sufficiently penetrated, and the resistance value of the connection portion tends to increase. There is.
  • the average particle size exceeds lOOOnm, there is a tendency that the insulation with the adjacent circuit becomes insufficient.
  • the number of the metal fine particles 2 disposed on the surface of the base particle 1 inside the metal plating layer 3 is preferably 10 to 40 per base particle 10 to 30 More preferably, it is 10-20. If the number of metal fine particles 2 is less than 10, the increase in connection resistance tends to be insufficient. On the other hand, if the number of metal fine particles 2 exceeds 40, the insulation between adjacent circuits tends to be insufficient.
  • the metal plating layer 3 covers at least a part of the surface of the base particle 1 and the metal fine particle 2. However, from the viewpoint of more reliably preventing the metal fine particles 2 from falling off, it is preferable that the surfaces of the base particle 1 and the metal fine particles 2 are substantially covered.
  • the thickness of the metal plating layer 3 is preferably from 80 to 200 nm, more preferably from 100 to 150 nm, and even more preferably from 100 to: LOnm. If the thickness of the metal plating layer 3 is less than 80 nm, the resistance value of the connection portion tends to increase. On the other hand, when the thickness of the metal plating layer 3 exceeds 200 nm, the insulation with an adjacent circuit tends to be insufficient.
  • Examples of the method for producing the conductive particles 10 include a method in which the metal fine particles 2 are physically attached to the surface of the substrate particles 1 and then a plating process is performed to form the metal plating layer 3.
  • the number of the metal fine particles 2 attached to the surface of the base particle 1 can be controlled by adjusting the amount of the metal fine particles 2 to be added.
  • the electroconductive particle 10 is manufactured by performing an electroless plating process with respect to this.
  • the adhesive component 20 includes: (a) a composition comprising an adhesive comprising a thermosetting resin; and (b) a thermosetting resin curing agent; and (c) free radicals by heating or light. Generated curing agent and (d) A composition containing an adhesive that also has a dical polymerizable material strength is preferred. Alternatively, a mixed composition of (a), (b), (c) and (d) above is preferred.
  • thermosetting resin is not particularly limited as long as it is a thermosetting resin that can be cured in an arbitrary temperature range, but an epoxy resin is preferable.
  • Epoxy resins include bisphenol A type epoxy resin, bisphenol F type epoxy resin, bisphenol S type epoxy resin, phenol novolac type epoxy resin, cresol novolac type epoxy resin, bisphenol A.
  • These epoxy resins may be halogenated or hydrogenated. These epoxy resins can be used alone or in combination of two or more.
  • Thermosetting resin curing agents include amine, phenol, acid anhydride, imidazole, hydrazide, dicyandiamide, boron trifluoride-amine complex, sulfo-um. Salt, iodonium salt, aminimide and the like. These may be used alone or in combination of two or more, and may be used by mixing a decomposition accelerator, an inhibitor and the like. In addition, it is preferable to use these curing agents coated with a polyurethane-based or polyester-based polymer substance and then micro-pressed because the pot life is extended.
  • the blending amount of the thermosetting resin curing agent is preferably about 0.1 to 60.0% by mass based on the total mass of the adhesive component. 1.0 to 20 More preferably 0% by mass. If the blending amount of the thermosetting resin curing agent is less than 0.1% by mass, the progress of the curing reaction tends to be insufficient, and it tends to be difficult to obtain good adhesive strength and connection resistance. . On the other hand, when the blending amount exceeds 60% by mass, the fluidity of the adhesive component tends to decrease, the pot life tends to be shortened, and the connection resistance value of the connection portion tends to increase.
  • Curing agents that generate free radicals by heating or light include those that generate free radicals by decomposition by heating or light, such as peroxide compounds and azo compounds.
  • the curing agent is appropriately selected depending on the intended connection temperature, connection time, pot life and the like. In terms of high reactivity and pot life, a half-life temperature of 10 hours is over 40 ° C and a half-life of 1 Organic peroxides with a minute temperature of 180 ° C or less are preferred.
  • the amount of curing agent which generates by Ri free radicals heating or light based on the total weight of the adhesive component, preferable to be 0.05 to 10 weight 0/0, 0. more preferably a 1 to 5 mass 0/0.
  • Curing agents that generate free radicals by heating or light are specifically diacyl peroxide, peroxydicarbonate, peroxyester, peroxyketal, dialkyl peroxide, hyde mouth A force such as peroxide can also be selected. In order to suppress corrosion of connection terminals of circuit members, it is preferable to select from peroxyesters, dialkyl peroxides, odorants, and peroxides that can provide high reactivity. Is more preferred.
  • disilver oxides include isobutyl peroxide, 2,4-dichlorobenzoic peroxide, 3, 5, 5-trimethylhexanoyl peroxide, octanoyl peroxide, and lauroyl peroxide.
  • examples thereof include oxide, stearoyl peroxide, succinic peroxide, benzoyl peroxide, and benzoyl peroxide.
  • peroxydicarbonates examples include di-n-propyl peroxydicarbonate, diisopropyl peroxydicarbonate, bis (4-tert-butylcyclohexyl) peroxydicarbonate, di-2- Examples include ethoxymethoxy baroxydicarbonate, di (2-ethylhexyloxy) dicarbonate, dimethoxybutyl dioxygen dicarbonate, di (3-methyl-3-methoxybutyl dioxy) dicarbonate, and the like.
  • peroxyesters include, for example, Tamil peroxyneodecanoate, 1, 1, 3, 3-tetramethylbutyl peroxyneodecanoate, 1-cyclohexylene 1-methyle Cilpoxyneodecanoate, t-hexyloxyneodecanoate, t-butylperoxybivalate, 1, 1, 3, 3—tetramethylbutylperoxy 2—ethylhexanoate, 2 , 5 Dimethyl-2,5 Bis (2-ethylhexylberoxy) hexane, 1-cyclohexyl lumine 1 Methylethylperoxy 2-ethyl hexanoate, t-hexyloxy 2-ethylhexanoate, t-butyl baroxy 2— Ethylhexanoate, t-butylperoxyisobutyrate, 1, 1 bis ( tert-butylperoxy) cyclohe
  • the peroxyketals include, for example, 1, 1 bis (t-hexyloxy) 3, 5, 5 trimethylcyclohexane, 1,1-bis (t-hexyloxy) cyclohexane, 1 , 1-bis (t-butylperoxy) 1,3,5,5 trimethylcyclohexane, 1,1- (t-butylperoxy) cyclododecane, 2,2-bis (t-butylperoxy) decane, and the like.
  • dialkyl peroxides examples include ⁇ , ⁇ , bis (t butyl peroxide) diisopropylbenzene, dicumyl peroxide, 2,5 dimethyl-2,5 di (t butyl peroxide) hexane, t butyl tamperper.
  • examples include oxides.
  • hydride peroxides examples include diisopropylbenzene hydride peroxide, cumene hydride peroxide, and the like.
  • curing agents that generate free radicals by heating or light can be used alone or in admixture of two or more, and can be used by mixing decomposition accelerators, inhibitors and the like. May be used.
  • the (d) radical polymerizable substance is a substance having a functional group that is polymerized by radicals, and examples thereof include (meth) acrylate and maleimide compounds.
  • Examples of (meth) acrylate include urethane (meth) acrylate, methyl (meth) acrylate, ethyl (meth) acrylate, isopropyl (meth) acrylate, isobutyl (meth) acrylate, ethylene Glycol di (meth) acrylate, diethylene glycol di (meth) acrylate, triethylene glycol di (meth) acrylate, trimethylol propane tri (meth) acrylate, tetramethylol methane tetra (meth) acrylate, 2-hydroxy 1,1,3 Di (meth) atalyloxypropane, 2,2 bis [4 — ((meth) atarioxymethoxy) phenol] propan, 2,2 bis [4 — (((meth)) talyloxypolyethoxy ) Fuel] propane, dicyclobe Ntu (meth) acrylate, tricyclode force-l (meth) acrylate
  • Such radically polymerizable substances can be used singly or in combination of two or more.
  • Adhesive component is particularly preferred to contain at least a radically polymerizable material that has a viscosity power of OOOOO to 1000000 mPa's at 25 ° C Radicals having a viscosity (25 ° C) of 100000 to 5000 OOmPa ⁇ s U, which preferably contains polymerizable substances.
  • the viscosity of the radically polymerizable substance can be measured using a commercially available E-type viscometer.
  • radical polymerizable substances it is preferable to use urethane acrylate or urethane meta acrylate from the viewpoint of adhesiveness. Further, it is particularly preferable to use a radically polymerizable substance having a Tg of 100 ° C. or more alone after crosslinking with an organic peroxide used for improving heat resistance.
  • a radically polymerizable substance a substance having a dicyclobenzyl group, a tricyclohexyl group and Z or a triazine ring in the molecule can be used.
  • a radically polymerizable substance having a tricyclodecanyl group or a triazine ring in the molecule is preferably used.
  • maleimide compounds include those containing at least two maleimide groups in the molecule, such as 1-methyl 2,4 bismaleimidobenzene, N, N, 1 m-phenylene bis.
  • a polymerization inhibitor such as hydroquinone or methyl ether neuroquinone may be used as appropriate.
  • the adhesive component 20 may contain a film-forming polymer. Based on the total mass of the adhesive component 20, the content of the film-forming polymer is preferably 2 to 80% by mass, more preferably 5 to 70% by mass. 10 to 60 More preferably, it is mass%.
  • Film-forming polymers include polystyrene, polyethylene, polyvinyl butyral, polyvinyl formal, polyimide, polyamide, polyester, polyvinyl chloride, polyphenylene oxide, urea resin, melamine resin, phenol resin, xylene resin. Fats, polyisocyanate resin, phenoxy resin, polyimide resin, polyester urethane resin, etc. are used.
  • a resin having a functional group such as a hydroxyl group is more preferable because it can improve adhesiveness.
  • those obtained by modifying these polymers with radically polymerizable functional groups can also be used.
  • the weight average molecular weight of the film-forming polymer is preferably 10,000 to 10000000!
  • the circuit connecting material 50 includes a filler, a softener, an accelerator, an anti-aging agent, a colorant, a flame retardant, a thixotropic agent, a coupling agent, a phenol resin, a melamine resin, and an isocyanine. It is also possible to contain gins.
  • the inclusion of a filler is preferable because improvement in connection reliability and the like can be obtained.
  • the filler can be used if its maximum diameter is smaller than the particle diameter of the conductive particles, and the range of 5 to 60% by volume is preferred. If it exceeds 60% by volume, the effect of improving reliability is saturated.
  • a compound containing one or more groups selected from the group consisting of a vinyl group, an acrylic group, an amino group, an epoxy group, and an isocyanate group is preferable in terms of improving adhesiveness.
  • the content of the conductive particles 10 is preferably 0.5 to 60 parts by volume when the total volume of the circuit connection material 50 is 100 parts by volume. Yo Use properly.
  • FIG. 4 is a cross-sectional view showing a state in which the circuit connecting material 50 according to the present invention is provided on the film-like support 60.
  • the support 60 include a polyethylene terephthalate film, a polyethylene naphthalate film, a polyethylene isophthalate film, a polybutylene terephthalate film, a polyolefin-based film, a polyacetate film, a polycarbonate film, a polyphenylene sulfide film, a polyamide film, It is possible to use various films such as a styrene acetate butyl copolymer film, a polychlorinated bulle film, a poly (vinylidene chloride) film, a synthetic rubber film, and a liquid crystal polymer film.
  • a support having a corona discharge treatment, an anchor coating treatment, an antistatic treatment or the like may be used on the surface of the film as necessary.
  • the surface of the support 60 is coated with a release treatment agent as necessary so that the support 60 can be easily peeled from the circuit connection material 50. Also good.
  • a release treatment agent silicone resin, copolymer of silicone and organic resin, alkyd resin, aminoalkyd resin, resin having long alkyl group, resin having fluoroalkyl group, shellac resin Various release treatment agents such as can be used
  • the film thickness of the support 60 is not particularly limited, but should be 4 to 200 / ⁇ ⁇ in consideration of storage and convenience of use of the produced circuit connecting material 50. Is preferred. Further, the film thickness of the support 60 is more preferably 15 to 75 / ⁇ ⁇ in consideration of material cost and productivity.
  • the circuit connection material is not limited to a single layer structure like the circuit connection material 50, and may be a multilayer structure in which a plurality of layers are laminated.
  • a circuit connection material having a multilayer structure can be produced by laminating a plurality of layers having different types of adhesive components and conductive particles or different contents thereof.
  • the circuit connection material includes a conductive particle-containing layer containing conductive particles and a conductive particle-free layer that does not contain conductive particles and is provided on at least one surface of the conductive particle-containing layer. You can have it.
  • FIG. 5 is a cross-sectional view showing a state in which the circuit connecting material having a two-layer structure is supported by the support.
  • the circuit connecting material 70 shown in FIG. 5 includes a conductive particle-containing layer 70a containing conductive particles. And a conductive particle non-containing layer 70b which does not contain conductive particles.
  • Support members 60a and 60b are provided on both outermost surfaces of the circuit connecting material 70, respectively.
  • the circuit connection material 70 forms a conductive particle-containing layer 70a on the surface of the support 60a, while forming a conductive particle-free layer 70b on the surface of the support 60b.
  • These layers are used as a conventionally known laminator or the like. It can produce by bonding together using.
  • the support bodies 60a and 60b are appropriately peeled off.
  • the circuit connection material 70 it is possible to sufficiently suppress the decrease in the number of conductive particles on the circuit electrode due to the flow of the adhesive component when the circuit members are joined. For this reason, for example, when an IC chip is mounted on a substrate, the number of conductive particles on the metal bumps (connection terminals) of the IC chip can be sufficiently secured.
  • the circuit connecting material 70 is arranged so that the surface provided with the metal bumps of the IC chip and the conductive particle-free layer 70b are in contact with the substrate on which the IC chip is to be mounted and the conductive particle-containing layer 70a, respectively. Is preferably arranged.
  • FIG. 6 is a process diagram showing an embodiment of a circuit member connection method according to the present invention in a schematic cross-sectional view, and shows a series of processes until the connection structure is manufactured by thermosetting the circuit connection material 50.
  • the above-described first circuit member 30 and a film-like circuit connection material 50 are prepared.
  • the circuit connecting material 50 is made of an adhesive composition containing the conductive particles 10.
  • the thickness of the circuit connecting material 50 is preferably 5 to 50 ⁇ m. If the thickness of the circuit connecting material 50 is less than 5 m, the circuit connecting material 50 tends to be insufficiently filled between the first and second circuit electrodes 32 and 42. On the other hand, when the thickness exceeds 50 m, it tends to be difficult to ensure conduction between the first and second circuit electrodes 32 and 42.
  • circuit connection material 50 is placed on the surface of the first circuit member 30 on which the circuit electrodes 32 are formed. Then, the circuit connection material 50 is pressurized in the directions of arrows A and B in FIG. 6 (a), and the circuit connection material 50 is temporarily connected to the first circuit member 30 (FIG. 6 (b)).
  • the pressure at this time is not particularly limited as long as it does not damage the circuit member, but it is generally preferably 0.1 to 30. OMPa. You can also pressurize while heating
  • the heating temperature is a temperature at which the circuit connecting material 50 is not substantially cured. In general, the heating temperature is preferably 50 to 190 ° C. These heating and pressurization are preferably performed in the range of 0.5 to 120 seconds.
  • the second circuit member 40 is placed on the circuit connection material 50 so that the second circuit electrode 42 faces the first circuit member 30. Put it on. Then, while heating the film-like circuit connecting material 50, the whole is pressurized in the directions of arrows A and B in FIG. 6 (c).
  • the heating temperature at this time is a temperature at which the circuit connecting material 50 can be cured.
  • the heating temperature is preferably 60 to 180 ° C, and more preferably 80 to 160 ° C, more preferably 70 to 170 ° C. If the heating temperature is less than 60 ° C, the curing rate tends to be slow, and if it exceeds 180 ° C, unwanted side reactions tend to proceed.
  • the heating time is preferably 0.1 to 180 seconds, more preferably 0.5 to 180 seconds, and still more preferably 1 to 180 seconds.
  • the adhesive portion 50a is formed by curing the circuit connection material 50, and a connection body 100 as shown in FIG. 1 is obtained.
  • the connection conditions are appropriately selected depending on the intended use, adhesive composition, and circuit members.
  • the circuit connection material 50 may be appropriately irradiated with actinic rays or energy rays.
  • actinic rays or energy rays include ultraviolet light, visible light, and infrared light.
  • energy lines include electron beams, X-rays, ⁇ -rays, and microwaves.
  • FX-293 (trade name, manufactured by Toto Kasei Co., Ltd.) was used as a phenoxy resin.
  • NiZAu-plated polystyrene particles described above are electrolessly bonded after attaching Ni fine particles (metal fine particles) with an average particle size of 400 nm to the surface of polystyrene particles (base particles) with an average particle size of 3 ⁇ m.
  • the Ni layer was formed by the above, and the Au layer was finally formed.
  • the number of protrusions due to Ni fine particles was 32.
  • the compression modulus of polystyrene particles at 20% compression deformation was 750 kgfZmm 2 , and the compression recovery rate after compression at a maximum load of 5 mN was 70%.
  • the above-mentioned adhesive composition was applied on a support (film thickness 50 m) having PET (polyethylene terephthalate) force. Thereafter, this was dried at 70 ° C. for 10 minutes to obtain a conductive particle-containing layer (film thickness: 25 ⁇ m) provided on the support.
  • a 60 mass parts adhesive component solution was placed on a PET support (film thickness 50 m). Applied. Thereafter, this was dried at 70 ° C. for 10 minutes to obtain a conductive particle-free layer (film thickness: 25 ⁇ m) provided on the support.
  • NiZAu-plated polystyrene particles were prepared as follows. NiZAu-plated polystyrene particles were formed by depositing Ni fine particles with an average particle size of 200 nm on the surface of the same polystyrene particles used in Example 1, forming an Ni layer by electroless plating, and finally Au A layer was formed. Me As a result of observing the conductive particles after the adhesion treatment with a SEM at a magnification of 6000, the number of protrusions attributed to the Ni fine particles was 20.
  • NiZAu-plated polystyrene particles were prepared as follows. NiZAu-plated polystyrene particles were formed by depositing Ni fine particles with an average particle size of 800 nm on the same polystyrene particles used in Example 1, forming an Ni layer by electroless plating, and finally Au A layer was formed. As a result of observing the conductive particles after the plating treatment with a SEM at a magnification of 6000, the number of protrusions attributed to the Ni fine particles was 15.
  • NiZAu-plated polystyrene particles were prepared as follows. NiZAu-plated polystyrene particles are formed by depositing Ni fine particles with an average particle size of 400 nm on the surface of polystyrene particles with a compression modulus of 300 kgfZmm 2 at 20% compression deformation, and then forming a Ni layer by electroless plating. Finally, an Au layer was formed. As a result of observing the conductive particles after plating at a magnification of 6000 by SEM, the number of protrusions attributed to Ni fine particles was 30.
  • NiZAu-plated polystyrene particles were prepared as follows.
  • NiZAu-plated polystyrene particles have an average particle size on the surface of polystyrene particles that has a compression modulus of 600 kgfZmm 2 at 20% compression deformation and a compression recovery rate force s of 40% after compression at a maximum load of 5 mN.
  • After depositing 400nm Ni fine particles a Ni layer was formed by electroless plating, and finally an Au layer was formed.
  • the number of protrusions attributed to Ni fine particles was 30.
  • NiZAu-plated polystyrene particles were prepared as follows. NiZAu-plated polystyrene particles have an average particle size of 4 m and a compression modulus of 700 kgfZmm 2 at 20% compression deformation. After attaching Ni fine particles having an average particle diameter of 400 nm to the surface of the particles, a Ni layer was formed by electroless plating, and finally an Au layer was formed. As a result of observing the conductive particles after plating treatment with SEM at a magnification of 6000, the number of protrusions attributed to Ni fine particles was 32 o
  • NiZAu-plated polystyrene particles were prepared as follows. NiZAu-plated polystyrene particles have an average particle size of 3 m, and after attaching Ni fine particles with an average particle size of 160 nm to the surface of polystyrene particles with a compression modulus of 450 kgfZmm 2 at 20% compression deformation, A Ni layer was formed by electroless plating, and finally an Au layer was formed. As a result of observing the conductive particles after plating treatment with SEM at a magnification of 6000, the number of protrusions attributed to Ni fine particles was 8 o
  • NiZAu-plated polystyrene particles were prepared as follows. NiZAu-plated polystyrene particles have an average particle size of 3 m, and after attaching Ni fine particles with an average particle size of 230 nm to the surface of polystyrene particles with a compression modulus of 500 kgfZmm 2 at 20% compression deformation, A Ni layer was formed by electroless plating, and finally an Au layer was formed. As a result of observing the conductive particles after plating treatment with SEM at a magnification of 6000, the number of protrusions due to Ni fine particles was 47 o
  • NiZAu-plated polystyrene particles were prepared as follows. NiZAu-plated polystyrene particles have an average particle size of 3 m, and after Ni particles with an average particle size of 200 nm are attached to the surface of polystyrene particles with a compression modulus of 90 kgfZmm 2 at 20% compression deformation, A Ni layer was formed by electroless plating, and finally an Au layer was formed. As a result of observing the conductive particles after plating treatment with SEM at a magnification of 6000, the number of protrusions attributed to Ni fine particles was 23. [0103] (Example 10)
  • NiZAu-plated polystyrene particles were prepared as follows.
  • NiZAu-plated polystyrene particles have a compression recovery rate of 25% after compression at a maximum load of 5 mN, and a compression elastic modulus force of 20% compression deformation on the surface of polystyrene particles with an S400 kgfZmm 2 average particle size of 400 nm.
  • a Ni layer was formed by electroless plating, and finally an Au layer was formed.
  • the number of protrusions attributed to the Ni fine particles was 30.
  • a circuit connecting material was obtained in the same manner as in Example 1 except that instead of the Ni / Au plated polystyrene particles, Au plated polystyrene particles prepared as described below were used. On the surface of the same polystyrene particles used in Example 1, an Au layer was formed by electroless plating to produce Au-plated polystyrene particles.
  • NiZAu-plated polystyrene particles were prepared as follows. NiZAu-plated polystyrene particles are formed by applying electroless nickel plating to the same polystyrene particle surface used in Example 1 to form a Ni layer and depositing Ni lumps, and then attaching the Au layer. Produced. As a result of observing the conductive particles after plating treatment with a SEM at a magnification of 6000, the number of protrusions attributed to the Ni mass was 35.
  • the support on the conductive particle-containing layer side is peeled off so that the conductive particle-containing layer is free of glass.
  • the circuit connection material was placed on the glass substrate so as to abut on the glass substrate, and pre-compression was performed.
  • the IC chip was placed so that the gold bumps were in contact with the conductive particle-free layer.
  • the IC chip was placed, it was connected by pressing in the direction to sandwich the circuit connection material while heating.
  • the pre-bonding conditions were a temperature of 70 ° C, a pressure of 0.5 MPa (in terms of bump area), and a holding time of 1 second.
  • the connection conditions were a temperature of 210 ° C, a pressure of 70 MPa (in terms of bump area), and a holding time of 5 seconds.
  • the price was based on the following criteria.
  • A: R is less than 1 ⁇
  • Tables 1 and 2 show the evaluation results of the initial connection resistance when the circuit connection materials of Examples 1 to 9 and Comparative Example 1 are used as the circuit connection material, respectively.
  • connection structure after thermal cycle test After the initial connection resistance was evaluated, a thermal cycle test in which the temperature was raised and lowered was performed on the connection structure, and the connection resistance after the thermal cycle test was evaluated.
  • the thermal cycle test was performed by repeating the process of raising the connection structure from room temperature to 100 ° C, then lowering to 40 ° C and then raising the temperature to room temperature 20 times. Resistance value of connection structure after thermal cycle test
  • connection resistance after the thermal cycle test was evaluated based on the following criteria.
  • A: R is less than 3 ⁇
  • Tables 1 and 2 show the evaluation results of the connection resistance after the thermal cycle test when the circuit connection materials of Examples 1 to 9 and Comparative Example 1 are used as the circuit connection material, respectively.
  • the ITO substrate is an ITO electrode (surface resistance ⁇ 20 Q / U) formed by vapor-depositing indium stannate (ITO) on a glass substrate (thickness 0.7 mm).
  • the support on the conductive particle-containing layer side was peeled off, and a circuit connecting material was placed on the ITO substrate so that the conductive particle-containing layer was in contact with the ITO substrate, and pre-compression was performed.
  • the IC chip was placed so that the gold bumps were in contact with the conductive particle-free layer.
  • the pre-bonding conditions were a temperature of 70 ° C, a pressure of 0.5 MPa (in terms of bump area), and a holding time of 1 second.
  • the connection conditions were a temperature of 210 ° C, a pressure of 70 MPa (in terms of bump area), and a holding time of 5 seconds.
  • R is 1 ⁇ 10 1 () ⁇ or more
  • R is 1 ⁇ 10 9 to 1 ⁇ 10 10 ⁇
  • R is less than 1 ⁇ 10 9 ⁇ .
  • Tables 1 and 2 show the evaluation results of the insulating properties when the circuit connection materials of Examples 1 to 9 and Comparative Example 1 are used as the circuit connection materials, respectively.
  • the circuit connection material of Example 16 was evaluated as A for all evaluation items.
  • the circuit connecting material according to Example 16 it was shown that both low initial connection resistance and good insulation with the adjacent circuit electrode can be achieved at a high level.
  • the evaluation of the connection resistance after the thermal cycle test is A, it was shown that the increase in connection resistance can be sufficiently suppressed.
  • the circuit connection material of Comparative Example 1 in which no protrusion due to Ni fine particles was provided had an initial connection resistance evaluation of B, and a connection resistance evaluation after the thermal cycle test of C.
  • the circuit electrodes are made of a metal material on which an oxide film is easily formed. Even in such a case, it has been shown that a circuit connection material capable of sufficiently reducing the initial resistance value of the connection structure can be provided.
  • an adhesive capable of sufficiently reducing the initial resistance value of the connection structure even when the electrode to be connected is made of a metal material capable of easily forming an oxide film on the surface.
  • a composition and a circuit connecting material using the composition can be provided. Furthermore, according to the present invention, it is possible to provide a connection structure in which circuit members are connected with a low connection resistance, and a circuit member connection method for obtaining the connection structure.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Computer Hardware Design (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Physics & Mathematics (AREA)
  • Dispersion Chemistry (AREA)
  • Power Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Conductive Materials (AREA)
  • Parts Printed On Printed Circuit Boards (AREA)
  • Combinations Of Printed Boards (AREA)

Abstract

Composition d'adhésif comprenant un composant adhésif et des particules conductrices (10) dispersées dans le composant adhésif. La particule conductrice (10) comprend une particule de matériau de base (1) constituant la partie centrale, une couche de placage métallique (3) recouvrant au moins une partie de la surface de la particule de matériau de base (1), et une pluralité de fines particules de métal (2) agencées à l'intérieur de la couche de placage métallique (3) et sur la surface de la particule de matériau de base (1).
PCT/JP2006/322628 2005-11-18 2006-11-14 Composition d'adhésif, matériau de connexion de circuits, structure de connexion et procédé de connexion d'éléments de circuits WO2007058159A1 (fr)

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KR1020087011623A KR101049609B1 (ko) 2005-11-18 2006-11-14 접착제 조성물, 회로 접속 재료, 접속 구조 및 회로부재의접속방법
CN2006800430380A CN101309993B (zh) 2005-11-18 2006-11-14 粘接剂组合物、电路连接材料、连接结构及电路部件连接方法
JP2007545234A JP4877230B2 (ja) 2005-11-18 2006-11-14 接着剤組成物、回路接続材料、接続構造及び回路部材の接続方法

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CN101309993B (zh) 2012-06-27
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KR20080072658A (ko) 2008-08-06
TW200730599A (en) 2007-08-16
CN101309993A (zh) 2008-11-19
KR20110048079A (ko) 2011-05-09
JP2011231326A (ja) 2011-11-17
TW201202375A (en) 2012-01-16
JP4877230B2 (ja) 2012-02-15
JPWO2007058159A1 (ja) 2009-04-30

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