WO2013021895A1 - Conductive material and connection structure - Google Patents
Conductive material and connection structure Download PDFInfo
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- WO2013021895A1 WO2013021895A1 PCT/JP2012/069587 JP2012069587W WO2013021895A1 WO 2013021895 A1 WO2013021895 A1 WO 2013021895A1 JP 2012069587 W JP2012069587 W JP 2012069587W WO 2013021895 A1 WO2013021895 A1 WO 2013021895A1
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- conductive material
- conductive
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- connection structure
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- H01B1/20—Conductive material dispersed in non-conductive organic material
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- C08L101/00—Compositions of unspecified macromolecular compounds
- C08L101/12—Compositions of unspecified macromolecular compounds characterised by physical features, e.g. anisotropy, viscosity or electrical conductivity
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- H01—ELECTRIC ELEMENTS
- H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
- 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
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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
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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
- 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
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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
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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
- H05K3/36—Assembling printed circuits with other printed circuits
- H05K3/361—Assembling flexible printed circuits with other printed circuits
Definitions
- the present invention relates to a conductive material including a plurality of conductive particles, and for example, electrically connects electrodes of various connection target members such as a flexible printed circuit board, a glass substrate, a glass epoxy substrate, a semiconductor chip, and an organic electroluminescence display element substrate.
- the present invention relates to a conductive material that can be used for connection.
- the present invention also relates to a connection structure using the conductive material.
- Pasty or film anisotropic conductive materials are widely known.
- anisotropic conductive material a plurality of conductive particles are dispersed in a binder resin or the like.
- the anisotropic conductive material may be connected between a flexible printed circuit board and a glass substrate (FOG (Film on Glass)), or connected between a semiconductor chip and a flexible printed circuit board (COF ( (Chip on Film)), connection between a semiconductor chip and a glass substrate (COG (Chip on Glass)), connection between a flexible printed circuit board and a glass epoxy substrate (FOB (Film on Board)), and the like.
- FOG Glass
- COF Chip on Film
- Patent Document 1 includes a resin component mainly composed of a thermosetting resin, a metal ion scavenger for capturing metal ions dissociated from an electrode, and conductive particles.
- An anisotropic conductive material containing is disclosed.
- the metal ion scavenger has a smaller particle size than the conductive particles.
- Patent Document 2 discloses an anisotropic conductive material including an insulating adhesive, conductive particles, and an inorganic ion exchanger.
- Patent Document 3 listed below discloses an anisotropic conductive material comprising an alicyclic epoxy resin, a diol, a styrenic thermoplastic elastomer having an epoxy group, an ultraviolet active cationic polymerization catalyst, and conductive particles. A material is disclosed.
- Patent Document 4 discloses an anisotropic conductive adhesive sheet including a curing agent, a curable insulating resin, conductive particles, and ion scavenger particles.
- Patent Document 4 it is described that there are a cation type, an anion type, and a both ion type regarding the types of ions exchanged by the ion scavenger particles.
- patent document 4 since both the metal ion (positive ion) which causes the ion migration of an electrode terminal directly, and the anion which raises electrical conductivity and produces a metal ion can be exchanged. Both ion types are described as being preferred.
- an anisotropic conductive material containing conductive particles is disposed on the glass substrate.
- the semiconductor chips are stacked, and heated and pressurized.
- the anisotropic conductive material is cured, and the electrodes are electrically connected via the conductive particles to obtain a connection structure.
- connection structure When a connection structure is produced using a conventional anisotropic conductive material as described in Patent Documents 1 to 4, migration occurs when the obtained connection structure is used in a state of being energized under high humidity. Sometimes. For this reason, the insulation reliability of the connection structure may be low.
- connection structure using a conventional anisotropic conductive material containing a cation generator as described in Patent Document 3 has a problem that migration is likely to occur due to use in a state of being energized under high humidity. .
- the object of the present invention is to improve the conduction reliability and insulation reliability of the resulting connection structure when the electrodes of the connection target members are electrically connected despite the use of a cation generator. It is to provide a conductive material that can be formed, and a connection structure using the conductive material.
- the curable component includes a curable component, a cation exchanger, an anion exchanger, and conductive particles, and the curable component includes a curable compound and a cation generator.
- a conductive material is provided.
- the neutral exchange capacity of the cation exchanger is 2 meq / g or more, and the neutral exchange capacity of the anion exchanger is 1 meq / g or more.
- the cation exchanger preferably contains a zirconium atom.
- the anion exchanger preferably contains a magnesium atom and an aluminum atom.
- the content of the cation exchanger is 0.01 parts by weight or more and 5 parts by weight or less with respect to 100 parts by weight of the curable compound, and
- the content of the anion exchanger is 0.01 parts by weight or more and 5 parts by weight or less.
- the conductive particles include resin particles and a conductive layer disposed on the surface of the resin particles, and at least the outer surface of the conductive layer is A low melting point metal layer having a melting point of 450 ° C. or lower.
- a flux is further included.
- the conductive material according to the present invention is preferably a conductive material used for connecting a connection target member having a copper electrode.
- the conductive material according to the present invention is preferably an anisotropic conductive material.
- a connection structure according to the present invention includes a first connection target member, a second connection target member, and a connection part that electrically connects the first and second connection target members,
- the connection part is formed of the conductive material described above.
- the first connection target member has a first electrode on the surface
- the second connection target member has a second electrode on the surface
- the first electrode and the second electrode are electrically connected by the conductive particles
- at least one of the first electrode and the second electrode is a copper electrode.
- the conductive material according to the present invention includes a curable component and a conductive particle containing a curable compound and a cation generator, and further includes both a cation exchanger and an anion exchanger.
- FIG. 1 is a front sectional view schematically showing a connection structure using a conductive material according to an embodiment of the present invention.
- FIGS. 2A to 2C are front sectional views for explaining each step of obtaining a connection structure using the conductive material according to one embodiment of the present invention.
- the conductive material according to the present invention includes a curable component, a cation exchanger, an anion exchanger, and conductive particles.
- the curable component contains a curable compound and a cation generator.
- the electrode of the connection target member is used although the cation generator is used.
- the gaps are electrically connected, the conduction reliability and the insulation reliability of the obtained connection structure can be improved.
- the connection structure is used in a state of being energized under high humidity, migration hardly occurs in the conductive portions and the electrodes in the conductive particles, and high insulation reliability can be sufficiently ensured.
- the curable component contains a curable compound and a curing agent.
- the curing agent contains a cation generator.
- the conductive material contains a cation generator, migration in the connection structure tends to occur.
- the conductive material according to the present invention includes a curable component containing a curable compound and a cation generator and conductive particles, and further includes both a cation exchanger and an anion exchanger. Although the cation generator is used, migration in the connection structure can be effectively suppressed, and insulation reliability can be effectively increased.
- the present inventors have found that by using a cation generator, the conduction reliability can be effectively increased as compared to the case where a thermosetting agent other than the cation generator (such as an imidazole compound) is used. .
- the present inventors can use both a cation exchanger and an anion exchanger to use a cation exchanger alone, an anion exchanger alone, or both ion exchangers. It has been found that the occurrence of migration can be suppressed considerably effectively and the insulation reliability can be effectively increased in a conductive material containing a cation generator as compared with the case where is used alone.
- the conductive material according to the present invention does not include a conductive material containing only a cation exchanger as an ion exchanger.
- the conductive material according to the present invention does not include a conductive material containing only an anion exchanger as an ion exchanger.
- the conductive material according to the present invention does not include a conductive material that includes both ion exchangers and does not include both a cation exchanger and an anion exchanger as an ion exchanger.
- a cationic curing system for low temperature rapid curing.
- the cation generator is used because the ionic component contained in the molecular structure of the cation generator tends to diffuse into the composition and the cation curable compound such as an epoxy compound may contain chlorine ions. When used, electrode corrosion due to a small amount of ionic components is likely to occur. For this reason, when a cation generator is used, there is a problem in connection reliability between electrodes.
- both the cation exchanger and the anion exchanger it is more effective to use both the cation exchanger and the anion exchanger than the above-described both ion exchangers having an anion-positive amphoteric ion capturing ability.
- the reason for this is not clear, but it is conceivable that a compound having an yin and yang amphoteric ion trapping ability cancels the trapping ability because the sites having the respective yin and yang trapping ability are close to each other, thereby reducing the effect.
- a method of curing the conductive material As a method of curing the conductive material according to the present invention, a method of irradiating the conductive material with light, a method of heating the conductive material, a method of heating the conductive material after irradiating the conductive material with light, and heating the conductive material Then, a method of irradiating the conductive material with light can be mentioned.
- a method of irradiating the conductive material with light can be mentioned.
- the photocuring speed and the thermosetting speed are different, light irradiation and heating may be performed simultaneously.
- the method of heating a conductive material after irradiating light to a conductive material is preferable.
- the curable compound may be a curable compound (thermosetting compound or light and thermosetting compound) curable by heating, and is curable by irradiation with light (photocurable compound, Or light and thermosetting compounds).
- the curable compound is preferably a curable compound (thermosetting compound or light and thermosetting compound) that can be cured by heating.
- the conductive material is a conductive material curable by heating, and may include a curable compound (thermosetting compound or light and thermosetting compound) curable by heating as the curable compound.
- the curable compound curable by heating may be a curable compound (thermosetting compound) that is not cured by light irradiation, and is curable by both light irradiation and heating (light and light). Thermosetting compound).
- the conductive material is a conductive material that can be cured by both light irradiation and heating
- the curable compound is a curable compound that can be cured by light irradiation (a photocurable compound, or light and heat). It is preferable to further contain a curable compound).
- the conductive material can be semi-cured (B-staged) by light irradiation to reduce the fluidity of the conductive material, and then the conductive material can be cured by heating.
- the curable compound that can be cured by light irradiation may be a curable compound (photocurable compound) that is not cured by heating, and is a curable compound that can be cured by both light irradiation and heating (light and light). Thermosetting compound).
- the conductive material according to the present invention includes a curing agent.
- the conductive material according to the present invention includes a cation generator as the curing agent.
- the cation generator may be a cation generator that generates cations by heating (thermal cation generator, or light and thermal cation generator), and a cation generator that generates cations by light irradiation (photo cation generation). Agent, or light and thermal cation generator).
- the curable compound is preferably a cation generator that generates cations by heating (thermal cation generator, or light and thermal cation generator).
- the conductive material according to the present invention may contain a photocuring initiator.
- the conductive material according to the present invention preferably contains a photoradical generator as the photocuring initiator.
- the conductive material includes a thermosetting compound as the curable compound, and preferably further includes a photocurable compound or light and a thermosetting compound.
- the conductive material preferably contains a thermosetting compound and a photocurable compound as the curable compound.
- the curable compound contained in the conductive material is not particularly limited.
- a conventionally known curable compound can be used as the curable compound.
- hardenable compound only 1 type may be used and 2 or more types may be used together.
- the curable compound contains a curable compound having an epoxy group.
- the curable compound having an epoxy group is an epoxy compound.
- the said curable compound which has an epoxy group only 1 type may be used and 2 or more types may be used together.
- the curable compound having an epoxy group preferably has an aromatic ring.
- the aromatic ring include a benzene ring, naphthalene ring, anthracene ring, phenanthrene ring, tetracene ring, chrysene ring, triphenylene ring, tetraphen ring, pyrene ring, pentacene ring, picene ring, and perylene ring.
- the said aromatic ring is a benzene ring, a naphthalene ring, or an anthracene ring, and it is more preferable that it is a benzene ring or a naphthalene ring.
- a naphthalene ring is preferred because it has a planar structure and can be cured more rapidly.
- the content of the curable compound having an epoxy group is preferably 10% by weight or more, more preferably 20% by weight or more, in the total 100% by weight of the curable compound. , 100% by weight or less.
- the total amount of the curable compound may be the curable compound having the epoxy group.
- the content of the functional compound is preferably 99% by weight or less, more preferably 95% by weight or less, still more preferably 90% by weight or less, and particularly preferably 80% by weight or less.
- the curable compound may further contain another curable compound different from the curable compound having an epoxy group.
- the other curable compounds include curable compounds having an unsaturated double bond, phenol curable compounds, amino curable compounds, unsaturated polyester curable compounds, polyurethane curable compounds, silicone curable compounds, and polyimide curable compounds. Compounds and the like. As for said other curable compound, only 1 type may be used and 2 or more types may be used together.
- the curable compound may contain a curable compound having an unsaturated double bond.
- the curable compound having an unsaturated double bond is a cured product having a (meth) acryloyl group. It is preferable that it is an ionic compound.
- the curable compound having the (meth) acryloyl group is (meth) It preferably has one or two acryloyl groups.
- the curable compound having the (meth) acryloyl group is (meth) It preferably has one or two acryloyl groups.
- the curable compound having the (meth) acryloyl group has no epoxy group and has a (meth) acryloyl group, and has a epoxy group and a curable compound having a (meth) acryloyl group.
- the curable compound having the (meth) acryloyl group an ester compound obtained by reacting a (meth) acrylic acid and a compound having a hydroxyl group, an epoxy obtained by reacting (meth) acrylic acid and an epoxy compound ( A (meth) acrylate, a urethane (meth) acrylate obtained by reacting a (meth) acrylic acid derivative having a hydroxyl group with an isocyanate, or the like is preferably used.
- the “(meth) acryloyl group” refers to an acryloyl group and a methacryloyl group.
- the “(meth) acryl” refers to acryl and methacryl.
- the “(meth) acrylate” refers to acrylate and methacrylate.
- the ester compound obtained by reacting the above (meth) acrylic acid with a compound having a hydroxyl group is not particularly limited.
- the ester compound any of a monofunctional ester compound, a bifunctional ester compound, and a trifunctional or higher functional ester compound can be used.
- the curable compound having an epoxy group and a (meth) acryloyl group is obtained by converting a part of the epoxy group of the compound having two or more epoxy groups into a (meth) acryloyl group.
- a compound is preferred.
- This curable compound is a partially (meth) acrylated epoxy compound.
- the curable compound preferably contains a reaction product of a compound having two or more epoxy groups and (meth) acrylic acid.
- This reaction product is obtained by reacting a compound having two or more epoxy groups with (meth) acrylic acid in the presence of a catalyst such as an acidic catalyst according to a conventional method. It is preferable that 20% or more of the epoxy group is converted (conversion rate) to a (meth) acryloyl group.
- the conversion is more preferably 30% or more, preferably 80% or less, more preferably 70% or less. Most preferably, 40% or more and 60% or less of the epoxy groups are converted to (meth) acryloyl groups.
- Examples of the partially (meth) acrylated epoxy compound include bisphenol type epoxy (meth) acrylate, cresol novolac type epoxy (meth) acrylate, carboxylic acid anhydride-modified epoxy (meth) acrylate, and phenol novolac type epoxy (meth) acrylate. Is mentioned.
- a modified phenoxy resin obtained by converting a part of epoxy groups of a phenoxy resin having two or more epoxy groups into (meth) acryloyl groups may be used. That is, a modified phenoxy resin having an epoxy group and a (meth) acryloyl group may be used.
- the curable compound may be a crosslinkable compound or a non-crosslinkable compound.
- crosslinkable compound examples include 1,4-butanediol di (meth) acrylate, 1,6-hexanediol di (meth) acrylate, 1,9-nonanediol di (meth) acrylate, (poly ) Ethylene glycol di (meth) acrylate, (poly) propylene glycol di (meth) acrylate, neopentyl glycol di (meth) acrylate, pentaerythritol di (meth) acrylate, glycerol methacrylate acrylate, pentaerythritol tri (meth) acrylate, tri Examples include methylolpropane trimethacrylate, allyl (meth) acrylate, vinyl (meth) acrylate, divinylbenzene, polyester (meth) acrylate, and urethane (meth) acrylate.
- non-crosslinkable compound examples include ethyl (meth) acrylate, n-propyl (meth) acrylate, isopropyl (meth) acrylate, n-butyl (meth) acrylate, isobutyl (meth) acrylate, t-butyl (meth) ) Acrylate, pentyl (meth) acrylate, hexyl (meth) acrylate, heptyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, n-octyl (meth) acrylate, isooctyl (meth) acrylate, nonyl (meth) acrylate, decyl (Meth) acrylate, undecyl (meth) acrylate, dodecyl (meth) acrylate, tridecyl (meth) acrylate, tetradecyl (meth) acrylate,
- the conductive material preferably contains the photocurable compound and the thermosetting compound in a weight ratio of 1:99 to 90:10, more preferably 5:95 to 60:40, and more preferably 10:90. More preferably, it is contained at about 40:60.
- the conductive material includes a curing agent.
- the curing agent may be a thermosetting agent or a photocuring initiator.
- the curing agent includes a cation generator.
- Conventionally known cation generators can be used as the cation generator.
- the cation generator is preferably used as a thermal cation generator for at least thermally curing the conductive material, not as a photo cation generator for only photocuring the conductive material.
- the cation generator is preferably used as a thermal cation generator for thermosetting the conductive material, not as a photo cation generator for photocuring the conductive material.
- the said cation generator only 1 type may be used and 2 or more types may be used together.
- iodonium salts and sulfonium salts are preferably used.
- commercially available products of the above cation generator include San-Aid SI-45L, SI-60L, SI-80L, SI-100L, SI-110L, SI-150L manufactured by Sanshin Chemical Co., Ltd., K- manufactured by Enomoto Kasei Co., Ltd. PURE, Adeka optomer SP-150, SP-170 manufactured by ADEKA, and the like can be mentioned.
- Preferred anion moieties of the cation generator include PF 6 , BF 4 , and B (C 6 F 5 ) 4 .
- cation generator examples include 2-butenyldimethylsulfonium tetrakis (pentafluorophenyl) borate, 2-butenyldimethylsulfonium tetrafluoroborate, 2-butenyldimethylsulfonium.
- the cation generator preferably releases inorganic acid ions by heating or releases organic acid ions containing boron atoms by heating.
- the cation generator is preferably a component that releases inorganic acid ions by heating, and is also preferably a component that releases organic acid ions containing boron atoms by heating.
- the cation generator that releases inorganic acid ions by heating is preferably a compound having SbF 6- or PF 6- as the anion moiety.
- the cation generator is preferably a compound having SbF 6 ⁇ as the anion moiety, and is preferably a compound having PF 6 ⁇ as the anion moiety.
- the anion portion of the cation generator is preferably represented by B (C 6 X 5 ) 4 — .
- the cation generator that releases an organic acid ion containing a boron atom is preferably a compound having an anion moiety represented by the following formula (1).
- X represents a halogen atom.
- X in the formula (1) is preferably a chlorine atom, a bromine atom or a fluorine atom, and more preferably a fluorine atom.
- the anion portion of the cation generator is preferably represented by B (C 6 F 5 ) 4 — .
- the cation generator that releases an organic acid ion containing a boron atom is more preferably a compound having an anion moiety represented by the following formula (1A).
- the content of the cation generator is not particularly limited.
- the content of the cation generator is preferably 0.01 parts by weight or more, more preferably 0.05 parts by weight or more, still more preferably 5 parts by weight or more, particularly preferably 100 parts by weight of the curable compound. It is 10 parts by weight or more, preferably 40 parts by weight or less, more preferably 30 parts by weight or less, and still more preferably 20 parts by weight or less.
- the content of the cation generator relative to the curable compound is not less than the above lower limit and not more than the above upper limit, the conductive material is sufficiently cured.
- the content of the cation generator is preferably 0.01 parts by weight or more, more preferably 0.05 parts by weight or more, and still more preferably 5 parts by weight with respect to 100 parts by weight of the curable compound curable by heating. Above, particularly preferably 10 parts by weight or more, preferably 40 parts by weight or less, more preferably 30 parts by weight or less, and still more preferably 20 parts by weight or less.
- the content of the cation generator relative to the curable compound curable by heating is not less than the above lower limit and not more than the above upper limit, the conductive material is sufficiently thermally cured.
- the conductive material preferably includes both the cation generator and the thermal radical generator.
- the thermal radical generator is not particularly limited.
- a conventionally known thermal radical generator can be used.
- the said thermal radical generator only 1 type may be used and 2 or more types may be used together.
- the “thermal radical generator” means a compound that generates radical species by heating.
- the thermal radical generator is not particularly limited, and examples thereof include azo compounds and peroxides.
- the peroxide include diacyl peroxide compounds, peroxyester compounds, hydroperoxide compounds, peroxydicarbonate compounds, peroxyketal compounds, dialkyl peroxide compounds, and ketone peroxide compounds.
- azo compound examples include 2,2′-azobisisobutyronitrile, 2,2′-azobis (2-methylbutyronitrile), and 2,2′-azobis (2,4-dimethylvaleronitrile).
- diacyl peroxide compound examples include benzoyl peroxide, diisobutyryl peroxide, di (3,5,5-trimethylhexanoyl) peroxide, dilauroyl peroxide, and disuccinic acid peroxide.
- peroxyester compounds include cumyl peroxyneodecanoate, 1,1,3,3-tetramethylbutylperoxyneodecanoate, tert-hexylperoxyneodecanoate, and tert-butylperoxyneo.
- hydroperoxide compound examples include cumene hydroperoxide and p-menthane hydroperoxide.
- peroxydicarbonate compound examples include di-sec-butyl peroxydicarbonate, di (4-t-butylcyclohexyl) peroxydicarbonate, di-n-propyl peroxydicarbonate, diisopropyl peroxycarbonate, and di- (2-ethylhexyl) peroxycarbonate and the like.
- Other examples of the peroxide include methyl ethyl ketone peroxide, potassium persulfate, and 1,1-bis (tert-butylperoxy) -3,3,5-trimethylcyclohexane.
- the decomposition temperature for obtaining the 10-hour half-life of the thermal radical generator is preferably 30 ° C or higher, more preferably 40 ° C or higher, preferably 90 ° C or lower, more preferably 80 ° C or lower, still more preferably 70 ° C or lower. It is. If the decomposition temperature for obtaining the 10-hour half-life of the thermal radical generator is less than 30 ° C., the storage stability of the conductive material tends to be reduced, and if it exceeds 90 ° C., The action tends to make it difficult to sufficiently cure the conductive material.
- the content of the thermosetting agent is not particularly limited.
- the content of the thermosetting agent is preferably 0.01 parts by weight or more, more preferably 0.05 parts by weight or more, with respect to 100 parts by weight of the curable compound curable by heating in the curable compound. More preferably 5 parts by weight or more, particularly preferably 10 parts by weight or more, preferably 40 parts by weight or less, more preferably 30 parts by weight or less, still more preferably 20 parts by weight or less.
- the content of the thermosetting agent is not less than the above lower limit and not more than the above upper limit, the conductive material can be sufficiently thermoset.
- thermosetting agent When the thermosetting agent is only a cation generator, the content of the thermosetting agent indicates the content of the cation generator, and the thermosetting agent is a cation generator and other thermosetting agents (thermal radicals). In the case of including both of the generator and the like, the total content of the cation generator and the other thermosetting agent is shown.
- the content of the thermal radical generator is preferably 0.01 with respect to 100 parts by weight of the curable compound curable by heating in the curable compound. Part by weight or more, more preferably 0.05 part by weight or more, preferably 10 parts by weight or less, more preferably 5 parts by weight or less.
- the content of the thermal radical generator is not less than the above lower limit and not more than the above upper limit, the conductive material can be sufficiently thermoset.
- the conductive material may contain a photocuring initiator as the curing agent.
- the photocuring initiator includes the above-described photocation generator (photocation generator or light and thermal cation generator).
- the photocuring initiator is not particularly limited.
- a conventionally known photocuring initiator can be used as the photocuring initiator.
- the conductive material preferably contains a photoradical generator. As for the said photocuring initiator, only 1 type may be used and 2 or more types may be used together.
- the photocuring initiator other than the cation generator is not particularly limited, and is not limited to acetophenone photocuring initiator (acetophenone photoradical generator), benzophenone photocuring initiator (benzophenone photoradical generator), thioxanthone, ketal light. Examples thereof include a curing initiator (ketal photo radical generator), halogenated ketone, acyl phosphinoxide, and acyl phosphonate.
- acetophenone photocuring initiator examples include 4- (2-hydroxyethoxy) phenyl (2-hydroxy-2-propyl) ketone, 2-hydroxy-2-methyl-1-phenylpropan-1-one, methoxy Examples include acetophenone, 2,2-dimethoxy-1,2-diphenylethane-1-one, and 2-hydroxy-2-cyclohexylacetophenone.
- ketal photocuring initiator examples include benzyldimethyl ketal.
- the content of the photocuring initiator is not particularly limited.
- the content of the photocuring initiator is preferably 0.1 parts by weight or more, more preferably 0.2 parts by weight with respect to 100 parts by weight of the curable compound that can be cured by light irradiation in the curable compound. Part or more, preferably 2 parts by weight or less, more preferably 1 part by weight or less.
- the conductive material can be appropriately photocured. By irradiating the conductive material with light and forming a B-stage, the flow of the conductive material can be suppressed.
- the content of the photocuring initiator indicates the content of the cation generating agent, and the photocuring initiator is a cation generator and another photocuring initiator. When both are included, the total content of the cation generator and the other photocuring initiator is shown.
- the cation exchanger and the anion exchanger contained in the conductive material are not particularly limited. As for the said cation exchanger, only 1 type may be used and 2 or more types may be used together. As for the said anion exchanger, only 1 type may be used and 2 or more types may be used together.
- the cation exchanger examples include Zr-based cation exchangers and Sb-based cation exchangers. From the viewpoint of further suppressing migration in the connection structure and further improving the insulation reliability, the cation exchanger is preferably a Zr-based cation exchanger, and preferably contains a zirconium atom.
- Examples of commercially available products of the cation exchanger include IXE-100 and IXE-300 (both of which are manufactured by Toagosei Co., Ltd.).
- the anion exchanger examples include Bi-based anion exchangers, Mg—Al-based anion exchangers, and Zr-based anion exchangers.
- the cation exchanger is preferably an Mg—Al anion exchanger, and includes magnesium atoms and aluminum atoms. It is preferable to include.
- anion exchangers examples include IXE-500, IXE-530 and IXE-550, IXE-700F and IXE-800 (all of which are manufactured by Toagosei Co., Ltd.).
- the neutral exchange capacity of the cation exchanger is preferably 1 meq / g or more, more preferably 2 meq / g or more, preferably 10 meq / g or less, more preferably 4 meq / g or less.
- the neutral exchange capacity of the cation exchanger is not less than the above lower limit and not more than the above upper limit, migration in the connection structure can be further suppressed, and insulation reliability can be further enhanced.
- the neutral exchange capacity of the anion exchanger is preferably 0.1 meq / g or more, more preferably 1 meq / g or more, preferably 10 meq / g or less, more preferably 5 meq / g or less.
- the neutral exchange capacity of the anion exchanger is not less than the above lower limit and not more than the above upper limit, migration in the connection structure can be further suppressed, and insulation reliability can be further enhanced.
- the median diameter of the cation exchanger is preferably 0.1 ⁇ m or more, more preferably 0.5 ⁇ m or more, preferably 10 ⁇ m or less, more preferably 3 ⁇ m or less.
- the median diameter of the cation exchanger is not less than the above lower limit and not more than the above upper limit, migration in the connection structure can be further suppressed, and insulation reliability can be further enhanced.
- the median diameter of the anion exchanger is preferably 0.1 ⁇ m or more, more preferably 0.5 ⁇ m or more, preferably 10 ⁇ m or less, more preferably 3 ⁇ m or less.
- the median diameter of the anion exchanger is not less than the above lower limit and not more than the above upper limit, migration in the connection structure can be further suppressed, and insulation reliability can be further enhanced.
- the content of the cation exchanger is preferably 0.01 parts by weight or more, more preferably 0.1 parts by weight or more, preferably 5 parts by weight or less, more preferably 100 parts by weight of the curable compound. 4 parts by weight or less.
- the content of the cation exchanger is not less than the above lower limit and not more than the above upper limit, migration in the connection structure can be further suppressed, and insulation reliability can be further enhanced.
- the content of the anion exchanger is preferably 0.01 parts by weight or more, more preferably 0.1 parts by weight or more, preferably 5 parts by weight or less, more preferably 100 parts by weight of the curable compound. 4 parts by weight or less.
- the content of the anion exchanger is not less than the above lower limit and not more than the above upper limit, migration in the connection structure can be further suppressed, and insulation reliability can be further enhanced.
- the conductive material preferably contains the cation exchanger and the anion exchanger in a weight ratio of 9: 1 to 1: 9, more preferably 8: 2 to 2: 8, and 6: More preferably, it is contained in a ratio of 4 to 4: 6.
- the conductive particles contained in the conductive material electrically connect the electrodes of the first and second connection target members, for example.
- the conductive particles are not particularly limited as long as they are conductive particles.
- the said electroconductive particle should just have an electroconductive part on the electroconductive surface.
- the surface of the conductive part of the conductive particles may be covered with an insulating layer.
- the surface of the conductive part of the conductive particles may be covered with insulating particles. In these cases, the insulating layer or insulating particles between the conductive portion and the electrode are excluded when the connection target member is connected.
- the conductive particles include organic particles, inorganic particles excluding metal particles, organic-inorganic hybrid particles, or metal particles whose surfaces are covered with a conductive layer (metal layer), and substantially only metal. Examples thereof include metal particles.
- the conductive particles are preferably conductive particles in which the surfaces of inorganic particles or organic-inorganic hybrid particles excluding organic particles, metal particles, and the like are coated with a conductive layer.
- the conductive part and the metal layer are not particularly limited. Gold, silver, copper, nickel, palladium, tin, etc. are mentioned as a metal which comprises the said electroconductive part.
- the metal layer include a gold layer, a silver layer, a copper layer, a nickel layer, a palladium layer, and a metal layer containing tin.
- the conductive particle is composed of a resin particle and a conductive layer (on the surface of the resin particle ( First conductive layer).
- the conductive particles are preferably conductive particles having at least a conductive outer surface made of a low melting point metal. More preferably, the conductive particles include resin particles and a conductive layer disposed on the surface of the resin particles, and at least the outer surface of the conductive layer is a low melting point metal layer.
- the low melting point metal layer is a layer containing a low melting point metal.
- the low melting point metal is a metal having a melting point of 450 ° C. or lower.
- the melting point of the low melting point metal is preferably 300 ° C. or lower, more preferably 160 ° C. or lower.
- the low melting point metal preferably contains tin. In 100% by weight of the low melting point metal or the metal contained in the low melting point metal layer, the content of tin is preferably 30% by weight or more, more preferably 40% by weight or more, still more preferably 70% by weight or more, particularly preferably 90% by weight. % Or more. When the content of tin is not less than the above lower limit, the connection reliability between the low melting point metal and the electrode is further enhanced.
- the tin content is determined using a high-frequency inductively coupled plasma emission spectrometer (“ICP-AES” manufactured by Horiba, Ltd.) or a fluorescent X-ray analyzer (“EDX-800HS” manufactured by Shimadzu). It can be measured.
- ICP-AES high-frequency inductively coupled plasma emission spectrometer
- EDX-800HS fluorescent X-ray analyzer
- the outer surface of the conductive part is a low melting point metal
- the low melting point metal is melted and joined to the electrodes, and the low melting point metal conducts between the electrodes.
- the connection resistance is low.
- the use of conductive particles having at least a conductive outer surface made of a low-melting-point metal increases the bonding strength between the low-melting-point metal and the electrode. Further, the moisture and heat resistance is further enhanced.
- the low melting point metal constituting the low melting point metal layer is not particularly limited.
- the low melting point metal is preferably tin or an alloy containing tin.
- the alloy include a tin-silver alloy, a tin-copper alloy, a tin-silver-copper alloy, a tin-bismuth alloy, a tin-zinc alloy, and a tin-indium alloy.
- the low melting point metal is preferably tin, a tin-silver alloy, a tin-silver-copper alloy, a tin-bismuth alloy, or a tin-indium alloy because of excellent wettability with respect to the electrode. More preferably, the alloy is a tin-indium alloy.
- the low melting point metal is preferably solder.
- the low melting point metal layer is preferably a solder layer.
- the material which comprises this solder is not specifically limited, Based on JIS Z3001: welding term, it is preferable that it is a filler material whose liquidus is 450 degrees C or less.
- the solder composition include metal compositions containing zinc, gold, lead, copper, tin, bismuth, indium and the like. Of these, a tin-indium system (117 ° C. eutectic) or a tin-bismuth system (139 ° C. eutectic) which is low-melting and lead-free is preferable. That is, the solder preferably does not contain lead, and is preferably a solder containing tin and indium or a solder containing tin and bismuth.
- the low melting point metal is nickel, copper, antimony, aluminum, zinc, iron, gold, titanium, phosphorus, germanium, tellurium, cobalt, bismuth, manganese. Further, it may contain a metal such as chromium, molybdenum and palladium. From the viewpoint of further increasing the bonding strength between the low melting point metal and the electrode, the low melting point metal preferably contains nickel, copper, antimony, aluminum, or zinc. From the viewpoint of further increasing the bonding strength between the low melting point metal and the electrode, the content of these metals for increasing the bonding strength is preferably 100% by weight of the metal contained in the low melting point metal or the low melting point metal layer. It is 0.0001% by weight or more, preferably 1% by weight or less.
- the conductive particles include resin particles and a conductive layer disposed on the surface of the resin particles, and the outer surface of the conductive layer is a low-melting metal layer, and the resin particles and the low-melting metal In addition to the low melting point metal layer, it is preferable to have a second conductive layer between the layers (such as solder layers). In this case, the low melting point metal layer is a part of the entire conductive layer, and the second conductive layer is a part of the entire conductive layer. In the case of using the conductive particles, it is preferable to bring the second conductive layer into contact with the electrode.
- the second conductive layer different from the low melting point metal layer preferably contains a metal.
- the metal constituting the second conductive layer is not particularly limited. Examples of the metal include gold, silver, copper, platinum, palladium, zinc, lead, aluminum, cobalt, indium, nickel, chromium, titanium, antimony, bismuth, germanium and cadmium, and alloys thereof. Further, tin-doped indium oxide (ITO) may be used as the metal. As for the said metal, only 1 type may be used and 2 or more types may be used together.
- the second conductive layer is preferably a nickel layer, a palladium layer, a copper layer or a gold layer, more preferably a nickel layer or a gold layer, and even more preferably a copper layer.
- the conductive particles preferably have a nickel layer, a palladium layer, a copper layer, or a gold layer, more preferably have a nickel layer or a gold layer, and still more preferably have a copper layer.
- a low melting point metal layer can be more easily formed on the surface of these preferable conductive layers.
- the second conductive layer may be a low melting point metal layer such as a solder layer.
- the conductive particles may have a plurality of low melting point metal layers.
- the thickness of the low melting point metal layer is preferably 0.1 ⁇ m or more, more preferably 0.5 ⁇ m or more, still more preferably 1 ⁇ m or more, preferably 50 ⁇ m or less, more preferably 10 ⁇ m or less, still more preferably 5 ⁇ m or less, particularly preferably. 3 ⁇ m or less.
- the conductivity is sufficiently high.
- the thickness of the low melting point metal layer is not more than the above upper limit, the difference in thermal expansion coefficient between the resin particles and the low melting point metal layer becomes small, and the low melting point metal layer is hardly peeled off.
- the total thickness of the conductive layer is preferably 0.1 ⁇ m or more, more preferably 0.5 ⁇ m or more, Preferably it is 1 micrometer or more, Preferably it is 50 micrometers or less, More preferably, it is 10 micrometers or less, More preferably, it is 5 micrometers or less, Most preferably, it is 3 micrometers or less.
- the average particle diameter of the conductive particles is preferably 0.5 ⁇ m or more, more It is preferably 1 ⁇ m or more, preferably 100 ⁇ m or less, more preferably 20 ⁇ m or less, still more preferably 15 ⁇ m or less, particularly preferably 10 ⁇ m or less, and most preferably less than 5 ⁇ m.
- the average particle diameter of the conductive particles is most preferably 1 ⁇ m or more and less than 5 ⁇ m.
- the resin particles can be properly used depending on the electrode size or land diameter of the substrate to be mounted.
- the ratio of the average particle diameter C of the conductive particles to the average particle diameter A of the resin particles is more than 1.0, preferably 3.0 or less.
- the ratio of the resin particles to the average particle size B with respect to the average particle size B of the conductive particle portion excluding the solder layer is greater than 1.0, preferably 2.0 or less.
- the average particle diameter B of the conductive particle portion excluding the solder layer having the average particle diameter C of the conductive particles including the solder layer is more than 1.0, preferably 2.0 or less.
- the ratio (B / A) is within the above range or the ratio (C / B) is within the above range, electrodes that are more reliably connected between the upper and lower electrodes and that are adjacent in the lateral direction The short circuit between them can be further suppressed.
- Conductive materials for FOB and FOF applications are anisotropic conductive materials:
- the conductive material is preferably used for connection between a flexible printed board and a glass epoxy board (FOB (Film on Board)) or between a flexible printed board and a flexible printed board (FOF (Film on Film)). It is done.
- FOB Glass epoxy board
- FOF Flexible printed board
- the L & S which is the size of the part with the electrode (line) and the part without the electrode (space), is generally 100 to 500 ⁇ m.
- the average particle diameter of resin particles used for FOB and FOF applications is preferably 10 to 100 ⁇ m. When the average particle diameter of the resin particles is 10 ⁇ m or more, the thickness of the conductive material and the connection portion disposed between the electrodes is sufficiently increased, and the adhesive force is further increased. When the average particle diameter of the resin particles is 100 ⁇ m or less, a short circuit is more unlikely to occur between adjacent electrodes.
- Conductive materials for flip chip applications (anisotropic conductive materials): The conductive material is suitably used for flip chip applications.
- the land diameter is generally 15 to 80 ⁇ m.
- the average particle diameter of the resin particles used for flip chip applications is preferably 1 to 15 ⁇ m.
- the average particle diameter of the resin particles is 1 ⁇ m or more, the thickness of the solder layer disposed on the surface of the resin particles can be sufficiently increased, and the electrodes can be more reliably electrically connected. it can.
- the average particle diameter of the resin particles is 10 ⁇ m or less, a short circuit is more unlikely to occur between adjacent electrodes.
- Conductive material for COF anisotropic conductive material: The conductive material is preferably used for connection between a semiconductor chip and a flexible printed board (COF (Chip on Film)).
- the L & S which is the dimension between the part with the electrode (line) and the part without the electrode (space), is generally 10 to 50 ⁇ m.
- the average particle diameter of resin particles used for COF applications is preferably 1 to 10 ⁇ m. When the average particle diameter of the resin particles is 1 ⁇ m or more, the thickness of the solder layer disposed on the surface of the resin particles can be sufficiently increased, and the electrodes can be more reliably electrically connected. it can. When the average particle diameter of the resin particles is 10 ⁇ m or less, a short circuit is more unlikely to occur between adjacent electrodes.
- the “average particle diameter” of the conductive particles and the resin particles indicates a number average particle diameter.
- the average particle diameter of the conductive particles can be obtained by observing 50 arbitrary conductive particles with an electron microscope or an optical microscope and calculating an average value.
- the surface of the conductive part in the conductive particles may be insulated by an insulating material, insulating particles, flux, or the like. It is preferable that the insulating material, the insulating particles, the flux, and the like are removed from the connection portion by being softened and flowed by heat at the time of connection. Thereby, the short circuit between electrodes can be suppressed.
- the content of the conductive particles is not particularly limited.
- the content of the conductive particles in 100% by weight of the conductive material is preferably 0.1% by weight or more, more preferably 0.5% by weight or more, still more preferably 1% by weight or more, preferably 40% by weight or less. More preferably, it is 30 weight% or less, More preferably, it is 19 weight% or less.
- a conductive particle can be easily arrange
- the conductive material may contain a flux. By using the flux, the oxide film formed on the electrode surface can be effectively removed. As a result, the conduction reliability in the connection structure is further increased. Note that the conductive material does not necessarily include a flux.
- the above flux is not particularly limited.
- a flux generally used for soldering or the like can be used.
- the flux include zinc chloride, a mixture of zinc chloride and an inorganic halide, a mixture of zinc chloride and an inorganic acid, a molten salt, phosphoric acid, a derivative of phosphoric acid, an organic halide, hydrazine, an organic acid, and pine resin.
- Etc. As for the said flux, only 1 type may be used and 2 or more types may be used together.
- Examples of the molten salt include ammonium chloride.
- Examples of the organic acid include lactic acid, citric acid, stearic acid, and glutamic acid.
- Examples of the pine resin include activated pine resin and non-activated pine resin.
- the flux is preferably rosin. By using rosin, the connection resistance between the electrodes is further reduced.
- the above rosins are rosins whose main component is abietic acid.
- the flux is preferably a rosin, and more preferably abietic acid. By using this preferable flux, the connection resistance between the electrodes is further reduced.
- the flux may be dispersed in a binder resin or may be attached on the surface of the conductive particles.
- the content of the flux is preferably 0.5% by weight or more, preferably 30% by weight or less, more preferably 25% by weight or less.
- the content of the flux is not less than the above lower limit and not more than the above upper limit, the oxide film formed on the electrode surface can be more effectively removed. Further, when the content of the flux is equal to or more than the lower limit, the effect of adding the flux is more effectively expressed.
- the content of the flux is not more than the above upper limit, the hygroscopic property of the cured product is further lowered, and the reliability of the connection structure is further enhanced.
- the conductive material preferably contains a filler.
- a filler By using the filler, the thermal expansion coefficient of the cured material of the conductive material can be suppressed.
- Specific examples of the filler include silica, aluminum nitride, alumina, glass, boron nitride, silicon nitride, silicone, carbon, graphite, graphene, and talc.
- a filler only 1 type may be used and 2 or more types may be used together. When a filler having a high thermal conductivity is used, the main curing time is shortened.
- the conductive material may contain a solvent.
- the solvent include ethyl acetate, methyl cellosolve, toluene, acetone, methyl ethyl ketone, cyclohexane, n-hexane, tetrahydrofuran and diethyl ether.
- the conductive material according to the present invention is preferably an anisotropic conductive material.
- the conductive material according to the present invention is preferably a conductive material used for electrical connection of electrodes.
- the conductive material according to the present invention is also preferably a conductive material used for electrical connection of electrodes in an organic electroluminescence display element.
- the conductive material according to the present invention is a paste-like or film-like conductive material, and is preferably a paste-like conductive material.
- the paste-like conductive material is a conductive paste.
- the film-like conductive material is a conductive film.
- the conductive material is a conductive film
- a film that does not include conductive particles may be laminated on the conductive film that includes the conductive particles.
- the conductive paste is preferably an anisotropic conductive paste.
- the conductive film is preferably an anisotropic conductive film.
- the conductive material according to the present invention is a conductive paste, and is preferably a conductive paste applied on the connection target member in a paste state.
- the viscosity of the conductive paste at 25 ° C. is preferably 20 Pa ⁇ s or more, more preferably 100 Pa ⁇ s or more, preferably 1000 Pa ⁇ s or less, more preferably 700 Pa ⁇ s or less, and further preferably 600 Pa ⁇ s or less. .
- the viscosity is equal to or higher than the lower limit, sedimentation of conductive particles in the conductive paste can be suppressed.
- the viscosity is equal to or lower than the upper limit, the dispersibility of the conductive particles is further increased.
- the viscosity of the conductive paste before coating is within the above range, after applying the conductive paste on the first connection target member, the flow of the conductive paste before curing can be further suppressed, and the voids are further reduced. It becomes difficult to occur.
- the viscosity of the conductive paste at 25 ° C. may be 300 Pa ⁇ s or less.
- the paste form includes liquid.
- the conductive material according to the present invention is preferably a conductive material used for connecting a connection target member having a copper electrode.
- a connection target member having a copper electrode is connected using a conductive material, there is a problem that migration is likely to occur due to the copper electrode in the connection structure.
- the conductive material according to the present invention even if a connection target member having a copper electrode is connected, migration in the connection structure can be effectively suppressed, and insulation reliability can be effectively increased. it can.
- the conductive material according to the present invention can be used for bonding various connection target members.
- the conductive material is preferably used for obtaining a connection structure in which the first and second connection target members are electrically connected.
- the conductive material is more preferably used to obtain a connection structure in which the electrodes of the first and second connection target members are electrically connected.
- FIG. 1 is a front sectional view schematically showing an example of a connection structure using a conductive material according to an embodiment of the present invention.
- a connection structure 1 shown in FIG. 1 includes a first connection target member 2, a second connection target member 4, and a connection portion that electrically connects the first and second connection target members 2 and 4. 3.
- the connecting portion 3 is a cured product layer and is formed by curing a conductive material including the conductive particles 5.
- the connecting portion 3 is preferably formed by curing an anisotropic conductive material.
- the first connection object member 2 has a plurality of first electrodes 2b on the surface 2a (upper surface).
- the second connection target member 4 has a plurality of second electrodes 4b on the surface 4a (lower surface).
- the first electrode 2 b and the second electrode 4 b are electrically connected by one or a plurality of conductive particles 5. Therefore, the first and second connection target members 2 and 4 are electrically connected by the conductive particles 5.
- connection between the first and second electrodes 2b and 4b is usually made by connecting the first connection target member 2 and the second connection target member 4 with the first and second electrodes 2b and 4b through a conductive material. Is carried out by applying pressure when the conductive material is cured after being overlapped so as to face each other. Generally, the conductive particles 5 are compressed by pressurization.
- the first and second connection target members are not particularly limited. Specific examples of the first and second connection target members include electronic components such as semiconductor chips, capacitors, and diodes, and electronic components such as printed boards, flexible printed boards, and glass boards. .
- the conductive material is preferably a conductive material used for connecting electronic components.
- connection structure 1 shown in FIG. 1 can be obtained, for example, through the states shown in FIGS. 2 (a) to 2 (c) as follows.
- a first connection target member 2 having a first electrode 2b on the surface 2a (upper surface) is prepared.
- a conductive material including a plurality of conductive particles 5 is disposed on the surface 2 a of the first connection target member 2, and the conductive material layer 3 ⁇ / b> A is formed on the surface 2 a of the first connection target member 2.
- the conductive material layer 3A is cured by irradiating the conductive material layer 3A with light.
- the conductive material layer 3A is irradiated with light to advance the curing of the conductive material layer 3A, so that the conductive material layer 3A is B-staged. That is, as shown in FIG. 2B, the B-staged conductive material layer 3B is formed on the surface 2a of the first connection target member 2.
- the B-staged conductive material layer 3B is a semi-cured product in a semi-cured state.
- the B-staged conductive material layer 3B is not completely cured, and thermal curing can be further advanced. However, the conductive material layer 3A may be cured at one time by irradiating the conductive material layer 3A with light or heating the conductive material layer 3A without making the conductive material layer 3A B-staged.
- the light irradiation intensity when irradiating with light is preferably within a range of 0.1 to 8000 mW / cm 2 .
- the integrated light quantity is preferably 0.1 to 20000 J / cm 2 .
- the light source used when irradiating light is not specifically limited. Examples of the light source include a light source having a sufficient light emission distribution at a wavelength of 420 nm or less. Specific examples of the light source include a low-pressure mercury lamp, a medium-pressure mercury lamp, a high-pressure mercury lamp, an ultrahigh-pressure mercury lamp, a chemical lamp, a black light lamp, a microwave excitation mercury lamp, a metal halide lamp, and an LED lamp.
- the second connection target member 4 is laminated on the upper surface 3a of the conductive material layer 3B which is B-staged.
- the second connection target member 4 is laminated so that the first electrode 2b on the surface 2a of the first connection target member 2 and the second electrode 4b on the surface 4a of the second connection target member 4 face each other. To do.
- the conductive material layer 3 ⁇ / b> B that has been B-staged is heated to further cure the conductive material layer 3 ⁇ / b> B that has been B-staged to form the connection portion 3.
- the B-staged conductive material layer 3B may be heated before the second connection target member 4 is laminated.
- the heating temperature for curing the conductive material layer 3A or the B-staged conductive material layer 3B by heating is preferably 50 ° C. or higher, more preferably 80 ° C. or higher, even more preferably 100 ° C. or higher, and still more preferably 140. It is preferably at least 160 ° C, more preferably at most 250 ° C, and even more preferably at most 200 ° C.
- the heating temperature May be 120 ° C. or lower.
- the contact area between the first and second electrodes 2b, 4b and the conductive particles 5 can be increased. it can. For this reason, conduction reliability can be improved. Further, by compressing the conductive particles 5, even if the distance between the first and second electrodes 2b and 4b increases, the particle diameter of the conductive particles 5 increases so as to follow this expansion.
- connection target member 2 and the second connection target member 4 are connected via the connection portion 3 by curing the B-staged conductive material layer 3B. Further, the first electrode 2 b and the second electrode 4 b are electrically connected through the conductive particles 5. In this way, the connection structure 1 shown in FIG. 1 using a conductive material can be obtained. Here, since photocuring and thermosetting are used in combination, the conductive material can be cured in a short time.
- the conductive material according to the present invention includes, for example, a connection between a flexible printed circuit board and a glass substrate (FOG (Film on Glass)), a connection between a semiconductor chip and a flexible printed circuit board (COF (Chip on Film)), and a semiconductor chip and glass. It can be used for connection with a substrate (COG (Chip on Glass)) or connection between a flexible printed circuit board and a glass epoxy substrate (FOB (Film on Board)).
- the said electrically-conductive material is suitable for a FOG use or a COG use, and is more suitable for a COG use.
- the conductive material according to the present invention is preferably a conductive material used for connection between a flexible printed circuit board and a glass substrate or a connection between a semiconductor chip and a glass substrate, and is used for connection between the flexible printed circuit board and the glass substrate. More preferably, it is a conductive material.
- the second connection target member and the first connection target member are a flexible printed circuit board and a glass substrate, or a semiconductor chip and a glass substrate. More preferably, they are a flexible printed circuit board and a glass substrate.
- connection structure according to the present invention is also preferably an organic electroluminescence display element.
- the electrodes in the organic electroluminescence display element may be electrically connected by conductive particles contained in the conductive material.
- At least one of the first electrode and the second electrode is a copper electrode. Both the first electrode and the second electrode are preferably copper electrodes. In this case, the effect of suppressing migration by the conductive material according to the present invention is further obtained, and the insulation reliability in the connection structure is further increased.
- the electrode width is preferably 5 ⁇ m or more, more preferably 10 ⁇ m or more, preferably 500 ⁇ m or less, more preferably 300 ⁇ m or less.
- the inter-electrode width is preferably 3 ⁇ m or more, more preferably 10 ⁇ m or more, preferably 500 ⁇ m or less, more preferably 300 ⁇ m or less.
- L / S (line / space) as electrode width / interelectrode width is preferably 5 ⁇ m / 5 ⁇ m or more, more preferably 10 ⁇ m / 10 ⁇ m or more, preferably 500 ⁇ m / 500 ⁇ m or less, more preferably 300 ⁇ m / 300 ⁇ m or less. is there.
- L / S line / space
- the conductive material according to the present invention even if a fine electrode is connected, the occurrence of insulation failure can be effectively suppressed, and insulation reliability can be sufficiently secured.
- IXE-100 Zr-based cation exchanger, neutral exchange capacity 3.3 meq / g, manufactured by Toagosei Co., Ltd.
- IXE-700F Mg-Al anion exchanger, neutral exchange capacity 4.5 meq / g, manufactured by Toagosei Co., Ltd.
- IXE-300 Sb cation exchanger, neutral exchange capacity 2.3 meq / g, manufactured by Toagosei Co., Ltd.
- IXE-500 Bi anion exchanger, neutral exchange capacity 1.8 meq / g, manufactured by Toagosei Co., Ltd.
- IXE-530 Bi anion exchanger, neutral exchange capacity 1.8 meq / g, manufactured by Toagosei Co., Ltd.
- IXE-633 Sb, Bi-based both ion exchangers, neutral exchange capacity 1.8 meq / g, manufactured by Toagosei Co., Ltd.
- Example 1 Preparation of anisotropic conductive material: SI-60L as a cation generator is added to 40 parts by weight of a bisphenol A-modified epoxy resin (“EPICLON EXA-4850-150” manufactured by DIC) and 30 parts by weight of a bisphenol F epoxy resin (“EXA-835LV” manufactured by DIC).
- a bisphenol A-modified epoxy resin (“EPICLON EXA-4850-150” manufactured by DIC)
- EXA-835LV” manufactured by DIC
- connection structure A glass substrate (first connection target member) having an L / S of 50 ⁇ m / 50 ⁇ m and a 1 mm long aluminum electrode pattern formed on the upper surface was prepared.
- the anisotropic conductive paste immediately after preparation was applied using a dispenser so that it might become width 1.5mm and thickness 40 micrometers, and the anisotropic conductive paste layer was formed.
- the flexible printed circuit board was laminated on the anisotropic conductive paste layer so that the electrodes face each other.
- a 365 nm ultraviolet ray was irradiated for 3 seconds so that the light irradiation intensity was 3000 mW / cm 2, and the anisotropic conductive paste layer was semi-cured by photopolymerization to form a B stage.
- thermocompression bonding head was adjusted so that the temperature of the anisotropic conductive paste layer was 170 ° C. (the main pressure bonding temperature).
- a pressure-bonding head was placed and the anisotropic conductive paste layer was cured at 170 ° C. for 5 seconds under a pressure of 1 MPa to obtain a connection structure.
- Example 2 Example 1 except that the amount of (1) IXE-100 was changed to 0.01 parts by weight and the amount of (2) IXE-700F was changed to 0.01 parts by weight. Thus, an anisotropic conductive paste was obtained. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 1.
- Example 3 Similar to Example 1, except that the blending amount of (1) IXE-100 was changed to 5 parts by weight and that the blending amount of (2) IXE-700F was changed to 5 parts by weight. Conductive paste was obtained. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 1.
- Example 4 An anisotropic conductive paste was obtained in the same manner as in Example 1 except that (2) IXE-700F was changed to (4) IXE-500 (manufactured by Toagosei Co., Ltd.). Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 1.
- Example 5 (1) IXE-100 was changed to (3) IXE-300 (made by Toagosei Co., Ltd.) and (2) IXE-700F was changed to (4) IXE-500 (made by Toagosei Co., Ltd.) Except that, an anisotropic conductive paste was obtained in the same manner as in Example 1. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 1.
- Example 6 (1) IXE-100 was changed to (3) IXE-300 (made by Toagosei Co., Ltd.) and (2) IXE-700F was changed to (5) IXE-530 (made by Toagosei Co., Ltd.) Except that, an anisotropic conductive paste was obtained in the same manner as in Example 1. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 1.
- Example 1 An anisotropic conductive paste was obtained in the same manner as in Example 1 except that both (1) IXE-100 and (2) IXE-700F were not added. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 1.
- Example 2 An anisotropic conductive paste was obtained in the same manner as in Example 1 except that IXE-100 was not added. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 1.
- Example 3 An anisotropic conductive paste was obtained in the same manner as in Example 1 except that (2) IXE-700F was not added. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 1.
- Example 4 (Comparative Example 4) Example 1 was repeated except that 2 parts by weight of IXE-633 (manufactured by Toagosei Co., Ltd.) was added without adding both (1) IXE-100 and (2) IXE-700F. An anisotropic conductive paste was obtained. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 1.
- thermosetting agent imidazole compound, “2P-4MZ” manufactured by Shikoku Kasei Kogyo Co., Ltd.
- thermosetting agent imidazole compound, “2P-4MZ” manufactured by Shikoku Kasei Kogyo Co., Ltd.
- SI-60L which is a cation generator
- Moisture-resistant insulation reliability With a voltage of 20 V applied between the measurement terminals insulated from each other of the obtained connection structure, exposure was performed in an atmosphere of 85 ° C. and 85% RH for 500 hours, The change in resistance value between the measuring terminals was measured. The case where the resistance value was 10 5 ⁇ or less was judged as an insulation failure. Moisture resistance insulation reliability was judged according to the following criteria.
- Example 7 Production of conductive particles: Divinylbenzene resin particles having an average particle size of 10 ⁇ m (Micropearl SP-210, manufactured by Sekisui Chemical Co., Ltd.) were subjected to electroless nickel plating to form a base nickel plating layer having a thickness of 0.1 ⁇ m on the surface of the resin particles. Next, the resin particles on which the base nickel plating layer was formed were subjected to electrolytic copper plating to form a 1 ⁇ m thick copper layer. Furthermore, electrolytic plating was performed using an electrolytic plating solution containing tin and bismuth to form a solder layer having a thickness of 1 ⁇ m.
- Conductive particles B were prepared.
- SI-60L as a cation generator is added to 40 parts by weight of a bisphenol A-modified epoxy resin (“EPICLON EXA-4850-150” manufactured by DIC) and 30 parts by weight of a bisphenol F epoxy resin (“EXA-835LV” manufactured by DIC).
- a glass epoxy substrate (first connection target member) having a gold-plated Cu electrode pattern with an L / S of 100 ⁇ m / 100 ⁇ m and a length of 4 mm formed on the upper surface was prepared.
- a flexible printed circuit board (second connection target member) having a gold-plated Cu electrode pattern having a L / S of 100 ⁇ m / 100 ⁇ m and a length of 4 mm formed on the lower surface was prepared.
- the anisotropic conductive paste immediately after preparation was applied using a dispenser so that it might become width 1.5mm and thickness 40 micrometers, and the anisotropic conductive paste layer was formed.
- the flexible printed circuit board was laminated on the anisotropic conductive paste layer so that the electrodes face each other.
- a 365 nm ultraviolet ray was irradiated for 3 seconds so that the light irradiation intensity was 3000 mW / cm 2, and the anisotropic conductive paste layer was semi-cured by photopolymerization to form a B stage.
- thermocompression bonding head was adjusted so that the temperature of the anisotropic conductive paste layer was 170 ° C. (the main pressure bonding temperature).
- a pressure-bonding head was placed and the anisotropic conductive paste layer was cured at 170 ° C. for 5 seconds under a pressure of 1 MPa to obtain a connection structure.
- Example 8 The same as Example 7 except that the amount of (1) IXE-100 was changed to 0.01 parts by weight and that the amount of (2) IXE-700F was changed to 0.01 parts by weight. Thus, an anisotropic conductive paste was obtained. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
- Example 9 Anisotropic as in Example 7, except that the amount of (1) IXE-100 was changed to 5 parts by weight and that the amount of (2) IXE-700F was changed to 5 parts by weight. Conductive paste was obtained. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
- Example 10 An anisotropic conductive paste was obtained in the same manner as in Example 7 except that (2) IXE-700F was changed to (4) IXE-500 (manufactured by Toagosei Co., Ltd.). Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
- Example 11 (1) IXE-100 was changed to (3) IXE-300 (made by Toagosei Co., Ltd.) and (2) IXE-700F was changed to (4) IXE-500 (made by Toagosei Co., Ltd.) Except that, an anisotropic conductive paste was obtained in the same manner as in Example 7. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
- Example 12 (1) IXE-100 was changed to (3) IXE-300 (made by Toagosei Co., Ltd.) and (2) IXE-700F was changed to (5) IXE-530 (made by Toagosei Co., Ltd.) Except that, an anisotropic conductive paste was obtained in the same manner as in Example 7. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
- Example 13 An anisotropic conductive paste was obtained in the same manner as in Example 7 except that rosin as a flux was not blended. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
- Example 14 An anisotropic conductive paste was obtained in the same manner as in Example 7 except that the conductive particle B was changed to the conductive particle A. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
- Example 15 An anisotropic conductive paste was obtained in the same manner as in Example 8 except that the conductive particle B was changed to the conductive particle A. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
- Example 16 An anisotropic conductive paste was obtained in the same manner as in Example 9 except that the conductive particle B was changed to the conductive particle A. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
- Example 17 An anisotropic conductive paste was obtained in the same manner as in Example 10 except that the conductive particles B were changed to the conductive particles A. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
- Example 18 An anisotropic conductive paste was obtained in the same manner as in Example 11 except that the conductive particle B was changed to the conductive particle A. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
- Example 19 An anisotropic conductive paste was obtained in the same manner as in Example 12 except that the conductive particles B were changed to the conductive particles A. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
- thermosetting compound The type and amount of the thermosetting compound are 40 parts by weight of a bisphenol A-modified epoxy resin (DIC Corporation “EPICLON EXA-4850-150”) and a bisphenol F epoxy resin (DIC Corporation “EXA-835LV”) 30 weight parts. Parts, except that the bisphenol E epoxy resin ("R1710” manufactured by Printec Co., Ltd.) was changed to 70 parts by weight, and the conductive particles B were changed to the conductive particles A in the same manner as in Example 7, An anisotropic conductive paste was obtained. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
- Example 21 The type of cation generator was changed from SI-60L (Sun Shin Aid made by Sanshin Chemical Co., Ltd.) to CXC-1612 (K-PURE made by Enomoto Kasei Co., Ltd.), and the conductive particles B were changed to the conductive particles.
- An anisotropic conductive paste was obtained in the same manner as Example 7 except for changing to A. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
- Example 5 An anisotropic conductive paste was obtained in the same manner as in Example 7 except that both (1) IXE-100 and (2) IXE-700F were not added. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
- Example 7 An anisotropic conductive paste was obtained in the same manner as in Example 7 except that (2) IXE-700F was not added. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
- Example 7 was repeated except that 2 parts by weight of IXE-633 (manufactured by Toagosei Co., Ltd.) was added without adding both (1) IXE-100 and (2) IXE-700F. An anisotropic conductive paste was obtained. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
- IXE-633 manufactured by Toagosei Co., Ltd.
- thermosetting agent imidazole compound, “2P-4MZ” manufactured by Shikoku Kasei Kogyo Co., Ltd.
- SI-60L which is a cation generator
- connection structures of Examples, Comparative Examples, and Reference Examples using the conductive particles B the solder layer of the conductive particles B is solidified after melting at the time of manufacturing the connection structures, and the electrodes in the connection structures The copper layer of the electroconductive particle B was contacting.
- Example 7 and Example 14 are both “ ⁇ ”
- the conduction reliability evaluation results of Example 8 and Example 15 are both “ ⁇ ”.
- the evaluation results of conduction reliability between Example 10 and Example 17 are both “ ⁇ ”
- the evaluation results of conduction reliability between Example 11 and Example 18 are both “ ⁇ ”. 12 and the evaluation result of the conduction reliability of Example 19 were both “ ⁇ ”.
- connection resistance in the conduction reliability evaluation of Example 7 is 0.7 ⁇ lower than the connection resistance in the conduction reliability evaluation of Example 14, and the connection resistance in the conduction reliability evaluation of Example 8 is Example 15.
- the connection resistance in the evaluation of conduction reliability of Example 10 is 0.8 ⁇ lower than the connection resistance in the evaluation of conduction reliability of Example 17, 11 is 0.8 ⁇ lower than the connection resistance in the conduction reliability evaluation in Example 18, and the connection resistance in the conduction reliability evaluation in Example 12 is the conduction reliability in Example 19. It was 0.7 ⁇ lower than the connection resistance in the evaluation.
Abstract
Description
上記導電材料に含まれている硬化性化合物は特に限定されない。上記硬化性化合物として、従来公知の硬化性化合物が使用可能である。上記硬化性化合物は1種のみが用いられてもよく、2種以上が併用されてもよい。 (Curable compound)
The curable compound contained in the conductive material is not particularly limited. A conventionally known curable compound can be used as the curable compound. As for the said sclerosing | hardenable compound, only 1 type may be used and 2 or more types may be used together.
上記導電材料は、硬化剤を含む。該硬化剤は、熱硬化剤であってもよく、光硬化開始剤であってもよい。該硬化剤は、カチオン発生剤を含む。該カチオン発生剤として従来公知のカチオン発生剤が使用可能である。また、本発明では、カチオン発生剤は、導電材料を光硬化のみさせるための光カチオン発生剤として用いるのではなく、導電材料を少なくとも熱硬化させるための熱カチオン発生剤として用いることが好ましい。さらに、本発明では、カチオン発生剤は、導電材料を光硬化させるための光カチオン発生剤として用いるのではなく、導電材料を熱硬化させるための熱カチオン発生剤として用いることが好ましい。上記カチオン発生剤は、1種のみが用いられてもよく、2種以上が併用されてもよい。 (Curing agent)
The conductive material includes a curing agent. The curing agent may be a thermosetting agent or a photocuring initiator. The curing agent includes a cation generator. Conventionally known cation generators can be used as the cation generator. In the present invention, the cation generator is preferably used as a thermal cation generator for at least thermally curing the conductive material, not as a photo cation generator for only photocuring the conductive material. Furthermore, in the present invention, the cation generator is preferably used as a thermal cation generator for thermosetting the conductive material, not as a photo cation generator for photocuring the conductive material. As for the said cation generator, only 1 type may be used and 2 or more types may be used together.
上記導電材料に含まれている陽イオン交換体及び陰イオン交換体は特に限定されない。上記陽イオン交換体は、1種のみが用いられてもよく、2種以上が併用されてもよい。上記陰イオン交換体は、1種のみが用いられてもよく、2種以上が併用されてもよい。 (Ion exchanger)
The cation exchanger and the anion exchanger contained in the conductive material are not particularly limited. As for the said cation exchanger, only 1 type may be used and 2 or more types may be used together. As for the said anion exchanger, only 1 type may be used and 2 or more types may be used together.
上記導電材料に含まれている導電性粒子は、例えば、第1,第2の接続対象部材の電極間を電気的に接続する。上記導電性粒子は、導電性を有する粒子であれば特に限定されない。上記導電性粒子は、導電部を導電性の表面に有していればよい。導電性粒子の導電部の表面が絶縁層により被覆されていてもよい。導電性粒子の導電部の表面が、絶縁性粒子により被覆されていてもよい。これらの場合には、接続対象部材の接続時に、導電部と電極との間の絶縁層又は絶縁性粒子が排除される。 (Conductive particles)
The conductive particles contained in the conductive material electrically connect the electrodes of the first and second connection target members, for example. The conductive particles are not particularly limited as long as they are conductive particles. The said electroconductive particle should just have an electroconductive part on the electroconductive surface. The surface of the conductive part of the conductive particles may be covered with an insulating layer. The surface of the conductive part of the conductive particles may be covered with insulating particles. In these cases, the insulating layer or insulating particles between the conductive portion and the electrode are excluded when the connection target member is connected.
上記導電材料は、フレキシブルプリント基板とガラスエポキシ基板との接続(FOB(Film on Board))との接続、又はフレキシブルプリント基板とフレキシブルプリント基板との接続(FOF(Film on Film))に好適に用いられる。 Conductive materials for FOB and FOF applications (anisotropic conductive materials):
The conductive material is preferably used for connection between a flexible printed board and a glass epoxy board (FOB (Film on Board)) or between a flexible printed board and a flexible printed board (FOF (Film on Film)). It is done.
上記導電材料は、フリップチップ用途に好適に用いられる。 Conductive materials for flip chip applications (anisotropic conductive materials):
The conductive material is suitably used for flip chip applications.
上記導電材料は、半導体チップとフレキシブルプリント基板との接続(COF(Chip on Film))に好適に用いられる。 Conductive material for COF (anisotropic conductive material):
The conductive material is preferably used for connection between a semiconductor chip and a flexible printed board (COF (Chip on Film)).
上記導電材料はフラックスを含んでいてもよい。該フラックスの使用により、電極表面に形成された酸化膜を効果的に除去できる。この結果、接続構造体における導通信頼性がより一層高くなる。なお、上記導電材料は、フラックスを必ずしも含んでいなくてもよい。 (flux)
The conductive material may contain a flux. By using the flux, the oxide film formed on the electrode surface can be effectively removed. As a result, the conduction reliability in the connection structure is further increased. Note that the conductive material does not necessarily include a flux.
上記導電材料は、フィラーを含むことが好ましい。フィラーの使用により、導電材料の硬化物の熱線膨張率を抑制できる。上記フィラーの具体例としては、シリカ、窒化アルミニウム、アルミナ、ガラス、窒化ボロン、窒化ケイ素、シリコーン、カーボン、グラファイト、グラフェン及びタルク等が挙げられる。フィラーは1種のみが用いられてもよく、2種以上が併用されてもよい。熱伝導率が高いフィラーを用いると、本硬化時間が短くなる。 (Other ingredients)
The conductive material preferably contains a filler. By using the filler, the thermal expansion coefficient of the cured material of the conductive material can be suppressed. Specific examples of the filler include silica, aluminum nitride, alumina, glass, boron nitride, silicon nitride, silicone, carbon, graphite, graphene, and talc. As for a filler, only 1 type may be used and 2 or more types may be used together. When a filler having a high thermal conductivity is used, the main curing time is shortened.
本発明に係る導電材料は、異方性導電材料であることが好ましい。本発明に係る導電材料は、電極の電気的な接続に用いられる導電材料であることが好ましい。本発明に係る導電材料は、有機エレクトロルミネッセンス表示素子における電極の電気的な接続に用いられる導電材料であることも好ましい。本発明に係る導電材料は、ペースト状又はフィルム状の導電材料であり、ペースト状の導電材料であることが好ましい。ペースト状の導電材料は、導電ペーストである。フィルム状の導電材料は、導電フィルムである。導電材料が導電フィルムである場合、該導電性粒子を含む導電フィルムに、導電性粒子を含まないフィルムが積層されてもよい。上記導電ペーストは、異方性導電ペーストであることが好ましい。上記導電フィルムは、異方性導電フィルムであることが好ましい。 (Details and applications of conductive materials)
The conductive material according to the present invention is preferably an anisotropic conductive material. The conductive material according to the present invention is preferably a conductive material used for electrical connection of electrodes. The conductive material according to the present invention is also preferably a conductive material used for electrical connection of electrodes in an organic electroluminescence display element. The conductive material according to the present invention is a paste-like or film-like conductive material, and is preferably a paste-like conductive material. The paste-like conductive material is a conductive paste. The film-like conductive material is a conductive film. When the conductive material is a conductive film, a film that does not include conductive particles may be laminated on the conductive film that includes the conductive particles. The conductive paste is preferably an anisotropic conductive paste. The conductive film is preferably an anisotropic conductive film.
(1)IXE-100(Zr系陽イオン交換体、中性交換容量3.3meq/g、東亞合成社製)
(2)IXE-700F(Mg-Al系陰イオン交換体、中性交換容量4.5meq/g、東亞合成社製)
(3)IXE-300(Sb系陽イオン交換体、中性交換容量2.3meq/g、東亞合成社製)
(4)IXE-500(Bi系陰イオン交換体、中性交換容量1.8meq/g、東亞合成社製)
(5)IXE-530(Bi系陰イオン交換体、中性交換容量1.8meq/g、東亞合成社製)
(6)IXE-633(Sb,Bi系両イオン交換体、中性交換容量1.8meq/g、東亞合成社製) (Ion exchanger)
(1) IXE-100 (Zr-based cation exchanger, neutral exchange capacity 3.3 meq / g, manufactured by Toagosei Co., Ltd.)
(2) IXE-700F (Mg-Al anion exchanger, neutral exchange capacity 4.5 meq / g, manufactured by Toagosei Co., Ltd.)
(3) IXE-300 (Sb cation exchanger, neutral exchange capacity 2.3 meq / g, manufactured by Toagosei Co., Ltd.)
(4) IXE-500 (Bi anion exchanger, neutral exchange capacity 1.8 meq / g, manufactured by Toagosei Co., Ltd.)
(5) IXE-530 (Bi anion exchanger, neutral exchange capacity 1.8 meq / g, manufactured by Toagosei Co., Ltd.)
(6) IXE-633 (Sb, Bi-based both ion exchangers, neutral exchange capacity 1.8 meq / g, manufactured by Toagosei Co., Ltd.)
(1)異方性導電材料の調製:
ビスフェノールA変性エポキシ樹脂(DIC社製「EPICLON EXA-4850-150」)40重量部、及びビスフェノールFエポキシ樹脂(DIC社製「EXA-835LV」)30重量部に、カチオン発生剤であるSI-60L(三新化学社製のサンエイド)3重量部と、光硬化性化合物であるエポキシアクリレート(ダイセル・サイテック社製「EBECRYL3702」)20重量部と、光硬化開始剤であるアシルホスフィンオキサイド系化合物(チバ・ジャパン社製「DAROCUR TPO」)1重量部と、フィラーである平均粒子径0.25μmのシリカ10重量部と、平均粒子径10μmの導電性粒子A4重量部と、イオン交換体である上記(1)IXE-100(東亞合成社製)1重量部と、上記(2)IXE-700F(東亞合成社製)1重量部とを添加し、遊星式攪拌機を用いて2000rpmで5分間攪拌することにより、異方性導電ペーストを得た。なお、用いた導電性粒子Aは、ジビニルベンゼン樹脂粒子の表面にニッケルめっき層が形成されており、かつ該ニッケルめっき層の表面に金めっき層が形成されている金属層を有する導電性粒子である。 (Example 1)
(1) Preparation of anisotropic conductive material:
SI-60L as a cation generator is added to 40 parts by weight of a bisphenol A-modified epoxy resin (“EPICLON EXA-4850-150” manufactured by DIC) and 30 parts by weight of a bisphenol F epoxy resin (“EXA-835LV” manufactured by DIC). 3 parts by weight (Sun Aid manufactured by Sanshin Chemical Co., Ltd.), 20 parts by weight of epoxy acrylate (“EBECRYL 3702” manufactured by Daicel Cytec Co., Ltd.) which is a photocurable compound, and acylphosphine oxide compound (Ciba) which is a photocuring initiator -"DAROCUR TPO" manufactured by Japan Co., Ltd.) 1 part by weight, 10 parts by weight of silica having an average particle diameter of 0.25 μm as filler, 4 parts by weight of conductive particles A having an average particle diameter of 10 μm, and the above (ion exchanger) 1) 1 part by weight of IXE-100 (manufactured by Toagosei Co., Ltd.) and (2) IXE-70 F was added and (Toagosei Co., Ltd.) 1 part by weight, by stirring for 5 minutes at 2000rpm using a planetary stirrer to obtain an anisotropic conductive paste. The conductive particles A used are conductive particles having a metal layer in which a nickel plating layer is formed on the surface of divinylbenzene resin particles and a gold plating layer is formed on the surface of the nickel plating layer. is there.
L/Sが50μm/50μm、長さ1mmのアルミニウム電極パターンが上面に形成されたガラス基板(第1の接続対象部材)を用意した。また、L/Sが50μm/50μm、長さ2mmの金メッキされたCu電極パターンが下面に形成されたフレキシブルプリント基板(第2の接続対象部材)を用意した。 (2) Fabrication of connection structure (FOG):
A glass substrate (first connection target member) having an L / S of 50 μm / 50 μm and a 1 mm long aluminum electrode pattern formed on the upper surface was prepared. In addition, a flexible printed circuit board (second connection target member) having a gold-plated Cu electrode pattern with a L / S of 50 μm / 50 μm and a length of 2 mm formed on the lower surface was prepared.
上記(1)IXE-100の配合量を0.01重量部に変更したこと、並びに上記(2)IXE-700Fの配合量を0.01重量部へ変更したこと以外は実施例1と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例1と同様にして、接続構造体を得た。 (Example 2)
Example 1 except that the amount of (1) IXE-100 was changed to 0.01 parts by weight and the amount of (2) IXE-700F was changed to 0.01 parts by weight. Thus, an anisotropic conductive paste was obtained. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 1.
上記(1)IXE-100の配合量を5重量部に変更したこと、並びに上記(2)IXE-700Fの配合量を5重量部へ変更したこと以外は実施例1と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例1と同様にして、接続構造体を得た。 (Example 3)
Similar to Example 1, except that the blending amount of (1) IXE-100 was changed to 5 parts by weight and that the blending amount of (2) IXE-700F was changed to 5 parts by weight. Conductive paste was obtained. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 1.
上記(2)IXE-700Fを上記(4)IXE-500(東亞合成社製)に変更したこと以外は実施例1と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例1と同様にして、接続構造体を得た。 (Example 4)
An anisotropic conductive paste was obtained in the same manner as in Example 1 except that (2) IXE-700F was changed to (4) IXE-500 (manufactured by Toagosei Co., Ltd.). Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 1.
上記(1)IXE-100を上記(3)IXE-300(東亞合成社製)に変更したこと、並びに上記(2)IXE-700Fを上記(4)IXE-500(東亞合成社製)に変更したこと以外は実施例1と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例1と同様にして、接続構造体を得た。 (Example 5)
(1) IXE-100 was changed to (3) IXE-300 (made by Toagosei Co., Ltd.) and (2) IXE-700F was changed to (4) IXE-500 (made by Toagosei Co., Ltd.) Except that, an anisotropic conductive paste was obtained in the same manner as in Example 1. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 1.
上記(1)IXE-100を上記(3)IXE-300(東亞合成社製)に変更したこと、並びに上記(2)IXE-700Fを上記(5)IXE-530(東亞合成社製)に変更したこと以外は実施例1と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例1と同様にして、接続構造体を得た。 (Example 6)
(1) IXE-100 was changed to (3) IXE-300 (made by Toagosei Co., Ltd.) and (2) IXE-700F was changed to (5) IXE-530 (made by Toagosei Co., Ltd.) Except that, an anisotropic conductive paste was obtained in the same manner as in Example 1. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 1.
上記(1)IXE-100、及び上記(2)IXE-700Fの双方を添加しなかったこと以外は、実施例1と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例1と同様にして、接続構造体を得た。 (Comparative Example 1)
An anisotropic conductive paste was obtained in the same manner as in Example 1 except that both (1) IXE-100 and (2) IXE-700F were not added. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 1.
上記(1)IXE-100を添加しなかったこと以外は、実施例1と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例1と同様にして、接続構造体を得た。 (Comparative Example 2)
(1) An anisotropic conductive paste was obtained in the same manner as in Example 1 except that IXE-100 was not added. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 1.
上記(2)IXE-700Fを添加しなかったこと以外は、実施例1と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例1と同様にして、接続構造体を得た。 (Comparative Example 3)
An anisotropic conductive paste was obtained in the same manner as in Example 1 except that (2) IXE-700F was not added. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 1.
上記(1)IXE-100、及び上記(2)IXE-700Fの双方を添加せずに、IXE-633(東亞合成社製)2重量部を添加したこと以外は、実施例1と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例1と同様にして、接続構造体を得た。 (Comparative Example 4)
Example 1 was repeated except that 2 parts by weight of IXE-633 (manufactured by Toagosei Co., Ltd.) was added without adding both (1) IXE-100 and (2) IXE-700F. An anisotropic conductive paste was obtained. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 1.
カチオン発生剤であるSI-60Lを添加せずに、熱硬化剤(イミダゾール化合物、四国化成工業社製「2P-4MZ」)10重量部を添加したこと以外は、実施例1と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例1と同様にして、接続構造体を得た。 (Reference Example 1)
In the same manner as in Example 1 except that 10 parts by weight of a thermosetting agent (imidazole compound, “2P-4MZ” manufactured by Shikoku Kasei Kogyo Co., Ltd.) was added without adding SI-60L as a cation generator. An anisotropic conductive paste was obtained. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 1.
カチオン発生剤であるSI-60Lを添加せずに、熱硬化剤(イミダゾール化合物、四国化成工業社製「2P-4MZ」)10重量部を添加したこと、並びに上記(1)IXE-100、及び上記(2)IXE-700Fの双方を添加しなかったこと以外は、実施例1と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例1と同様にして、接続構造体を得た。 (Reference Example 2)
The addition of 10 parts by weight of a thermosetting agent (imidazole compound, “2P-4MZ” manufactured by Shikoku Kasei Kogyo Co., Ltd.) without adding SI-60L, which is a cation generator, and (1) IXE-100, and An anisotropic conductive paste was obtained in the same manner as in Example 1 except that both (2) IXE-700F were not added. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 1.
(1)導通信頼性(接続抵抗値)
得られた接続構造体の上下の電極間の接続抵抗をそれぞれ、4端子法により測定した。100箇所の接続抵抗の平均値を算出した。なお、電圧=電流×抵抗の関係から、一定の電流を流した時の電圧を測定することにより接続抵抗を求めることができる。得られた接続構造体の導通信頼性を下記の基準で判定した。 (Evaluation of Examples 1 to 6, Comparative Examples 1 to 4 and Reference Examples 1 and 2)
(1) Conduction reliability (connection resistance value)
The connection resistance between the upper and lower electrodes of the obtained connection structure was measured by a four-terminal method. The average value of the connection resistance at 100 locations was calculated. Note that the connection resistance can be obtained by measuring the voltage when a constant current is passed from the relationship of voltage = current × resistance. The conduction reliability of the obtained connection structure was determined according to the following criteria.
○○:3Ω未満
○:3Ω以上、5Ω未満
×:5Ω以上 [Judgment criteria for conduction reliability]
○○: Less than 3Ω ○: 3Ω or more, less than 5Ω ×: 5Ω or more
得られた接続構造体の互いに絶縁された測定用端子間に20Vの電圧を印加した状態で、85℃及び85%RHの雰囲気下にて500時間暴露し、この間、測定用端子間の抵抗値変化を測定した。抵抗値が105Ω以下となった場合を絶縁不良と判断した。耐湿絶縁信頼性を下記基準で判定した。 (2) Moisture-resistant insulation reliability With a voltage of 20 V applied between the measurement terminals insulated from each other of the obtained connection structure, exposure was performed in an atmosphere of 85 ° C. and 85% RH for 500 hours, The change in resistance value between the measuring terminals was measured. The case where the resistance value was 10 5 Ω or less was judged as an insulation failure. Moisture resistance insulation reliability was judged according to the following criteria.
○○:10個の接続構造体のうち、絶縁不良が生じている接続構造体がなく、かつ耐湿絶縁信頼性試験後の平均抵抗値が107Ω以上
○:10個の接続構造体のうち、絶縁不良が生じている接続構造体がなく、かつ耐湿絶縁信頼性試験後の平均抵抗値が106Ω以上、107Ω未満
△:10個の接続構造体のうち、絶縁不良が生じている接続構造体がなく、かつ耐湿絶縁信頼性試験後の平均抵抗値が105Ω以上、106Ω未満
×:10個の接続構造体のうち、絶縁不良が生じている接続構造体が1個以上ある [Criteria for moisture-resistant insulation reliability]
◯: Of the 10 connection structures, there is no connection structure in which insulation failure occurs, and the average resistance value after the moisture-proof insulation reliability test is 10 7 Ω or more. ◯: Of the 10 connection structures There is no connection structure in which insulation failure has occurred, and the average resistance value after the moisture-proof insulation reliability test is 10 6 Ω or more and less than 10 7 Ω Δ: Among 10 connection structures, insulation failure has occurred There is no connection structure, and the average resistance value after the moisture-proof insulation reliability test is 10 5 Ω or more and less than 10 6 Ω x: Of the 10 connection structures, 1 is the connection structure in which insulation failure occurs There are more than
(1)導電性粒子の作製:
平均粒子径10μmのジビニルベンゼン樹脂粒子(積水化学工業社製、ミクロパールSP-210)を無電解ニッケルめっきし、樹脂粒子の表面上に厚さ0.1μmの下地ニッケルめっき層を形成した。次いで、下地ニッケルめっき層が形成された樹脂粒子を電解銅めっきし、厚さ1μmの銅層を形成した。更に、錫及びビスマスを含有する電解めっき液を用いて、電解めっきし、厚さ1μmのはんだ層を形成した。このようにして、樹脂粒子の表面上に厚み1μmの銅層が形成されており、該銅層の表面に厚み1μmのはんだ層(錫:ビスマス=43重量%:57重量%)が形成されている導電性粒子Bを作製した。 (Example 7)
(1) Production of conductive particles:
Divinylbenzene resin particles having an average particle size of 10 μm (Micropearl SP-210, manufactured by Sekisui Chemical Co., Ltd.) were subjected to electroless nickel plating to form a base nickel plating layer having a thickness of 0.1 μm on the surface of the resin particles. Next, the resin particles on which the base nickel plating layer was formed were subjected to electrolytic copper plating to form a 1 μm thick copper layer. Furthermore, electrolytic plating was performed using an electrolytic plating solution containing tin and bismuth to form a solder layer having a thickness of 1 μm. Thus, a 1 μm thick copper layer is formed on the surface of the resin particles, and a 1 μm thick solder layer (tin: bismuth = 43 wt%: 57 wt%) is formed on the surface of the copper layer. Conductive particles B were prepared.
ビスフェノールA変性エポキシ樹脂(DIC社製「EPICLON EXA-4850-150」)40重量部、及びビスフェノールFエポキシ樹脂(DIC社製「EXA-835LV」)30重量部に、カチオン発生剤であるSI-60L(三新化学社製のサンエイド)3重量部と、光硬化性化合物であるエポキシアクリレート(ダイセル・サイテック社製「EBECRYL3702」)20重量部と、光硬化開始剤であるアシルホスフィンオキサイド系化合物(チバ・ジャパン社製「DAROCUR TPO」)1重量部と、フィラーである平均粒子径0.25μmのシリカ10重量部と、フラックスであるロジン3重量部と、得られた導電性粒子B4重量部と、イオン交換体である上記(1)IXE-100(東亞合成社製)1重量部と、上記(2)IXE-700F(東亞合成社製)1重量部とを添加し、遊星式攪拌機を用いて2000rpmで5分間攪拌することにより、異方性導電ペーストを得た。 (2) Preparation of anisotropic conductive material:
SI-60L as a cation generator is added to 40 parts by weight of a bisphenol A-modified epoxy resin (“EPICLON EXA-4850-150” manufactured by DIC) and 30 parts by weight of a bisphenol F epoxy resin (“EXA-835LV” manufactured by DIC). 3 parts by weight (Sun Aid manufactured by Sanshin Chemical Co., Ltd.), 20 parts by weight of epoxy acrylate (“EBECRYL 3702” manufactured by Daicel Cytec Co., Ltd.) which is a photocurable compound, and acylphosphine oxide compound (Ciba) which is a photocuring initiator -"DAROCUR TPO" manufactured by Japan Co., Ltd.) 1 part by weight, 10 parts by weight of silica having an average particle diameter of 0.25 μm as a filler, 3 parts by weight of rosin as a flux, and 4 parts by weight of the obtained
L/Sが100μm/100μm、長さ4mmの金メッキされたCu電極パターンが上面に形成されたガラスエポキシ基板(第1の接続対象部材)を用意した。また、L/Sが100μm/100μm、長さ4mmの金メッキされたCu電極パターンが下面に形成されたフレキシブルプリント基板(第2の接続対象部材)を用意した。 (2) Production of Connection Structure (FOB) A glass epoxy substrate (first connection target member) having a gold-plated Cu electrode pattern with an L / S of 100 μm / 100 μm and a length of 4 mm formed on the upper surface was prepared. In addition, a flexible printed circuit board (second connection target member) having a gold-plated Cu electrode pattern having a L / S of 100 μm / 100 μm and a length of 4 mm formed on the lower surface was prepared.
上記(1)IXE-100の配合量を0.01重量部に変更したこと、並びに上記(2)IXE-700Fの配合量を0.01重量部へ変更したこと以外は実施例7と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例7と同様にして、接続構造体を得た。 (Example 8)
The same as Example 7 except that the amount of (1) IXE-100 was changed to 0.01 parts by weight and that the amount of (2) IXE-700F was changed to 0.01 parts by weight. Thus, an anisotropic conductive paste was obtained. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
上記(1)IXE-100の配合量を5重量部に変更したこと、並びに上記(2)IXE-700Fの配合量を5重量部へ変更したこと以外は実施例7と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例7と同様にして、接続構造体を得た。 Example 9
Anisotropic as in Example 7, except that the amount of (1) IXE-100 was changed to 5 parts by weight and that the amount of (2) IXE-700F was changed to 5 parts by weight. Conductive paste was obtained. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
上記(2)IXE-700Fを上記(4)IXE-500(東亞合成社製)に変更したこと以外は実施例7と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例7と同様にして、接続構造体を得た。 (Example 10)
An anisotropic conductive paste was obtained in the same manner as in Example 7 except that (2) IXE-700F was changed to (4) IXE-500 (manufactured by Toagosei Co., Ltd.). Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
上記(1)IXE-100を上記(3)IXE-300(東亞合成社製)に変更したこと、並びに上記(2)IXE-700Fを上記(4)IXE-500(東亞合成社製)に変更したこと以外は実施例7と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例7と同様にして、接続構造体を得た。 (Example 11)
(1) IXE-100 was changed to (3) IXE-300 (made by Toagosei Co., Ltd.) and (2) IXE-700F was changed to (4) IXE-500 (made by Toagosei Co., Ltd.) Except that, an anisotropic conductive paste was obtained in the same manner as in Example 7. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
上記(1)IXE-100を上記(3)IXE-300(東亞合成社製)に変更したこと、並びに上記(2)IXE-700Fを上記(5)IXE-530(東亞合成社製)に変更したこと以外は実施例7と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例7と同様にして、接続構造体を得た。 Example 12
(1) IXE-100 was changed to (3) IXE-300 (made by Toagosei Co., Ltd.) and (2) IXE-700F was changed to (5) IXE-530 (made by Toagosei Co., Ltd.) Except that, an anisotropic conductive paste was obtained in the same manner as in Example 7. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
フラックスであるロジンを配合しなかったこと以外は実施例7と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例7と同様にして、接続構造体を得た。 (Example 13)
An anisotropic conductive paste was obtained in the same manner as in Example 7 except that rosin as a flux was not blended. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
上記導電性粒子Bを上記導電性粒子Aへ変更したこと以外は実施例7と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例7と同様にして、接続構造体を得た。 (Example 14)
An anisotropic conductive paste was obtained in the same manner as in Example 7 except that the conductive particle B was changed to the conductive particle A. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
上記導電性粒子Bを上記導電性粒子Aへ変更したこと以外は実施例8と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例7と同様にして、接続構造体を得た。 (Example 15)
An anisotropic conductive paste was obtained in the same manner as in Example 8 except that the conductive particle B was changed to the conductive particle A. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
上記導電性粒子Bを上記導電性粒子Aへ変更したこと以外は実施例9と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例7と同様にして、接続構造体を得た。 (Example 16)
An anisotropic conductive paste was obtained in the same manner as in Example 9 except that the conductive particle B was changed to the conductive particle A. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
上記導電性粒子Bを上記導電性粒子Aへ変更したこと以外は実施例10と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例7と同様にして、接続構造体を得た。 (Example 17)
An anisotropic conductive paste was obtained in the same manner as in Example 10 except that the conductive particles B were changed to the conductive particles A. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
上記導電性粒子Bを上記導電性粒子Aへ変更したこと以外は実施例11と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例7と同様にして、接続構造体を得た。 (Example 18)
An anisotropic conductive paste was obtained in the same manner as in Example 11 except that the conductive particle B was changed to the conductive particle A. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
上記導電性粒子Bを上記導電性粒子Aへ変更したこと以外は実施例12と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例7と同様にして、接続構造体を得た。 (Example 19)
An anisotropic conductive paste was obtained in the same manner as in Example 12 except that the conductive particles B were changed to the conductive particles A. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
熱硬化性化合物の種類及び配合量を、ビスフェノールA変性エポキシ樹脂(DIC社製「EPICLON EXA-4850-150」)40重量部、及びビスフェノールFエポキシ樹脂(DIC社製「EXA-835LV」)30重量部から、ビスフェノールEエポキシ樹脂(プリンテック社製「R1710」)70重量部に変更したこと、並びに上記導電性粒子Bを上記導電性粒子Aに変更したこと以外は実施例7と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例7と同様にして、接続構造体を得た。 (Example 20)
The type and amount of the thermosetting compound are 40 parts by weight of a bisphenol A-modified epoxy resin (DIC Corporation “EPICLON EXA-4850-150”) and a bisphenol F epoxy resin (DIC Corporation “EXA-835LV”) 30 weight parts. Parts, except that the bisphenol E epoxy resin ("R1710" manufactured by Printec Co., Ltd.) was changed to 70 parts by weight, and the conductive particles B were changed to the conductive particles A in the same manner as in Example 7, An anisotropic conductive paste was obtained. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
カチオン発生剤の種類を、SI-60L(三新化学社製のサンエイド)から、CXC-1612(楠本化成社製のK-PURE)に変更したこと、並びに上記導電性粒子Bを上記導電性粒子Aに変更したこと以外は実施例7と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例7と同様にして、接続構造体を得た。 (Example 21)
The type of cation generator was changed from SI-60L (Sun Shin Aid made by Sanshin Chemical Co., Ltd.) to CXC-1612 (K-PURE made by Enomoto Kasei Co., Ltd.), and the conductive particles B were changed to the conductive particles. An anisotropic conductive paste was obtained in the same manner as Example 7 except for changing to A. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
上記(1)IXE-100、及び上記(2)IXE-700Fの双方を添加しなかったこと以外は、実施例7と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例7と同様にして、接続構造体を得た。 (Comparative Example 5)
An anisotropic conductive paste was obtained in the same manner as in Example 7 except that both (1) IXE-100 and (2) IXE-700F were not added. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
上記(1)IXE-100を添加しなかったこと以外は、実施例7と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例7と同様にして、接続構造体を得た。 (Comparative Example 6)
(1) An anisotropic conductive paste was obtained in the same manner as in Example 7 except that IXE-100 was not added. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
上記(2)IXE-700Fを添加しなかったこと以外は、実施例7と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例7と同様にして、接続構造体を得た。 (Comparative Example 7)
An anisotropic conductive paste was obtained in the same manner as in Example 7 except that (2) IXE-700F was not added. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
上記導電性粒子Bを上記導電性粒子Aへ変更したこと以外は、比較例5と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例7と同様にして、接続構造体を得た。 (Comparative Example 8)
An anisotropic conductive paste was obtained in the same manner as in Comparative Example 5 except that the conductive particles B were changed to the conductive particles A. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
上記導電性粒子Bを上記導電性粒子Aへ変更したこと以外は、比較例6と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例7と同様にして、接続構造体を得た。 (Comparative Example 9)
An anisotropic conductive paste was obtained in the same manner as in Comparative Example 6 except that the conductive particles B were changed to the conductive particles A. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
上記導電性粒子Bを上記導電性粒子Aへ変更したこと以外は、比較例7と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例7と同様にして、接続構造体を得た。 (Comparative Example 10)
An anisotropic conductive paste was obtained in the same manner as in Comparative Example 7 except that the conductive particles B were changed to the conductive particles A. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
上記(1)IXE-100、及び上記(2)IXE-700Fの双方を添加せずに、IXE-633(東亞合成社製)2重量部を添加したこと以外は、実施例7と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例7と同様にして、接続構造体を得た。 (Comparative Example 11)
Example 7 was repeated except that 2 parts by weight of IXE-633 (manufactured by Toagosei Co., Ltd.) was added without adding both (1) IXE-100 and (2) IXE-700F. An anisotropic conductive paste was obtained. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
カチオン発生剤であるSI-60Lを添加せずに、熱硬化剤(イミダゾール化合物、四国化成工業社製「2P-4MZ」)10重量部を添加したこと以外は、実施例7と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例7と同様にして、接続構造体を得た。 (Reference Example 3)
In the same manner as in Example 7 except that 10 parts by weight of a thermosetting agent (imidazole compound, “2P-4MZ” manufactured by Shikoku Kasei Kogyo Co., Ltd.) was added without adding SI-60L as a cation generator. An anisotropic conductive paste was obtained. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
カチオン発生剤であるSI-60Lを添加せずに、熱硬化剤(イミダゾール化合物、四国化成工業社製「2P-4MZ」)10重量部を添加したこと、並びに上記(1)IXE-100、及び上記(2)IXE-700Fの双方を添加しなかったこと以外は、実施例7と同様にして、異方性導電ペーストを得た。得られた異方性導電ペーストを用いて、実施例7と同様にして、接続構造体を得た。 (Reference Example 4)
The addition of 10 parts by weight of a thermosetting agent (imidazole compound, “2P-4MZ” manufactured by Shikoku Kasei Kogyo Co., Ltd.) without adding SI-60L, which is a cation generator, and (1) IXE-100, and An anisotropic conductive paste was obtained in the same manner as in Example 7 except that both (2) IXE-700F were not added. Using the obtained anisotropic conductive paste, a connection structure was obtained in the same manner as in Example 7.
(1)導通信頼性(接続抵抗値)
得られた接続構造体の上下の電極間の接続抵抗をそれぞれ、4端子法により測定した。10個の接続構造体の接続抵抗の平均値を算出した。なお、電圧=電流×抵抗の関係から、一定の電流を流した時の電圧を測定することにより接続抵抗を求めることができる。得られた接続構造体の導通信頼性を下記の基準で判定した。 (Evaluation of Examples 7 to 21, Comparative Examples 5 to 11 and Reference Examples 3 and 4)
(1) Conduction reliability (connection resistance value)
The connection resistance between the upper and lower electrodes of the obtained connection structure was measured by a four-terminal method. The average connection resistance of 10 connection structures was calculated. Note that the connection resistance can be obtained by measuring the voltage when a constant current is passed from the relationship of voltage = current × resistance. The conduction reliability of the obtained connection structure was determined according to the following criteria.
○○:8Ω未満
○:8Ω以上、10Ω未満
×:10Ω以上 [Judgment criteria for conduction reliability]
○○: Less than 8Ω ○: 8Ω or more, less than 10Ω ×: 10Ω or more
得られた接続構造体の互いに絶縁された測定用端子間に15Vの電圧を印加した状態で、85℃及び85%RHの雰囲気下にて500時間暴露し、この間、測定用端子間の抵抗値変化を測定した。抵抗値が105Ω以下となった場合を絶縁不良と判断した。耐湿絶縁信頼性を下記基準で判定した。 (2) Moisture-resistant insulation reliability With a voltage of 15 V applied between the measurement terminals insulated from each other of the obtained connection structure, it was exposed in an atmosphere of 85 ° C. and 85% RH for 500 hours, The change in resistance value between the measuring terminals was measured. The case where the resistance value was 10 5 Ω or less was judged as an insulation failure. Moisture resistance insulation reliability was judged according to the following criteria.
○○:10個の接続構造体のうち、絶縁不良が生じている接続構造体がなく、かつ耐湿絶縁信頼性試験後の平均抵抗値が107Ω以上
○:10個の接続構造体のうち、絶縁不良が生じている接続構造体がなく、かつ耐湿絶縁信頼性試験後の平均抵抗値が106Ω以上、107Ω未満
△:10個の接続構造体のうち、絶縁不良が生じている接続構造体がなく、かつ耐湿絶縁信頼性試験後の平均抵抗値が105Ω以上、106Ω未満
×:10個の接続構造体のうち、絶縁不良が生じている接続構造体が1個以上ある [Criteria for moisture-resistant insulation reliability]
◯: Of the 10 connection structures, there is no connection structure in which insulation failure occurs, and the average resistance value after the moisture-proof insulation reliability test is 10 7 Ω or more. ◯: Of the 10 connection structures There is no connection structure in which insulation failure has occurred, and the average resistance value after the moisture-proof insulation reliability test is 10 6 Ω or more and less than 10 7 Ω Δ: Among 10 connection structures, insulation failure has occurred There is no connection structure, and the average resistance value after the moisture-proof insulation reliability test is 10 5 Ω or more and less than 10 6 Ω x: Of the 10 connection structures, 1 is the connection structure in which insulation failure occurs There are more than
2…第1の接続対象部材
2a…表面
2b…第1の電極
3…接続部
3a…上面
3A…導電材料層
3B…Bステージ化された導電材料層
4…第2の接続対象部材
4a…表面
4b…第2の電極
5…導電性粒子 DESCRIPTION OF
Claims (11)
- 硬化性成分と、陽イオン交換体と、陰イオン交換体と、導電性粒子とを含み、
前記硬化性成分が、硬化性化合物と、カチオン発生剤とを含有する、導電材料。 Including a curable component, a cation exchanger, an anion exchanger, and conductive particles;
The electrically conductive material in which the said sclerosing | hardenable component contains a sclerosing | hardenable compound and a cation generator. - 前記陽イオン交換体の中性交換容量が2meq/g以上であり、かつ前記陰イオン交換体の中性交換容量が1meq/g以上である、請求項1に記載の導電材料。 The conductive material according to claim 1, wherein the neutral exchange capacity of the cation exchanger is 2 meq / g or more and the neutral exchange capacity of the anion exchanger is 1 meq / g or more.
- 前記陽イオン交換体がジルコニウム原子を含む、請求項1又は2に記載の導電材料。 The conductive material according to claim 1 or 2, wherein the cation exchanger contains a zirconium atom.
- 前記陰イオン交換体が、マグネシウム原子とアルミニウム原子とを含む、請求項1~3のいずれか1項に記載の導電材料。 The conductive material according to any one of claims 1 to 3, wherein the anion exchanger includes a magnesium atom and an aluminum atom.
- 前記硬化性化合物100重量部に対して、前記陽イオン交換体の含有量が0.01重量部以上、5重量部以下であり、かつ前記陰イオン交換体の含有量が0.01重量部以上、5重量部以下である、請求項1~4のいずれか1項に記載の導電材料。 The content of the cation exchanger is 0.01 parts by weight or more and 5 parts by weight or less with respect to 100 parts by weight of the curable compound, and the content of the anion exchanger is 0.01 parts by weight or more. The conductive material according to any one of claims 1 to 4, which is 5 parts by weight or less.
- 前記導電性粒子が、樹脂粒子と、前記樹脂粒子の表面上に配置された導電層とを有し、
前記導電層の少なくとも外側の表面が、融点が450℃以下である低融点金属層である、請求項1~5のいずれか1項に記載の導電材料。 The conductive particles have resin particles and a conductive layer disposed on the surface of the resin particles,
The conductive material according to any one of claims 1 to 5, wherein at least the outer surface of the conductive layer is a low melting point metal layer having a melting point of 450 ° C or lower. - フラックスをさらに含む、請求項1~6のいずれか1項に記載の導電材料。 The conductive material according to any one of claims 1 to 6, further comprising a flux.
- 銅電極を有する接続対象部材を接続するために用いられる導電材料である、請求項1~7のいずれか1項に記載の導電材料。 The conductive material according to any one of claims 1 to 7, which is a conductive material used for connecting a connection target member having a copper electrode.
- 異方性導電材料である、請求項1~8のいずれか1項に記載の導電材料。 The conductive material according to any one of claims 1 to 8, which is an anisotropic conductive material.
- 第1の接続対象部材と、第2の接続対象部材と、前記第1,第2の接続対象部材を電気的に接続している接続部とを備え、
前記接続部が、請求項1~9のいずれか1項に記載の導電材料により形成されている、接続構造体。 A first connection target member, a second connection target member, and a connection portion that electrically connects the first and second connection target members;
A connection structure in which the connection portion is formed of the conductive material according to any one of claims 1 to 9. - 前記第1の接続対象部材が表面に第1の電極を有し、
前記第2の接続対象部材が表面に第2の電極を有し、
前記第1の電極と前記第2の電極とが、前記導電性粒子により電気的に接続されており、
前記第1の電極及び前記第2の電極の内の少なくとも一方が、銅電極である、請求項10に記載の接続構造体。 The first connection object member has a first electrode on a surface;
The second connection object member has a second electrode on the surface,
The first electrode and the second electrode are electrically connected by the conductive particles;
The connection structure according to claim 10, wherein at least one of the first electrode and the second electrode is a copper electrode.
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JP2015168803A (en) * | 2014-03-10 | 2015-09-28 | 日立化成株式会社 | Conductive adhesive composition, connection body, solar cell module and method of producing the same |
JP2018178125A (en) * | 2018-06-26 | 2018-11-15 | 日立化成株式会社 | Conductive adhesive composition, connection body, solar cell module and method for producing the same |
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JPWO2022107511A1 (en) * | 2020-11-20 | 2022-05-27 | ||
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