WO2018151131A1 - 接着剤フィルム - Google Patents
接着剤フィルム Download PDFInfo
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- WO2018151131A1 WO2018151131A1 PCT/JP2018/005012 JP2018005012W WO2018151131A1 WO 2018151131 A1 WO2018151131 A1 WO 2018151131A1 JP 2018005012 W JP2018005012 W JP 2018005012W WO 2018151131 A1 WO2018151131 A1 WO 2018151131A1
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- conductive particles
- adhesive
- adhesive layer
- film
- conductive
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/10—Adhesives in the form of films or foils without carriers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J201/00—Adhesives based on unspecified macromolecular compounds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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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
- H01R11/00—Individual connecting elements providing two or more spaced connecting locations for conductive members which are, or may be, thereby interconnected, e.g. end pieces for wires or cables supported by the wire or cable and having means for facilitating electrical connection to some other wire, terminal, or conductive member, blocks of binding posts
- H01R11/01—Individual connecting elements providing two or more spaced connecting locations for conductive members which are, or may be, thereby interconnected, e.g. end pieces for wires or cables supported by the wire or cable and having means for facilitating electrical connection to some other wire, terminal, or conductive member, blocks of binding posts characterised by the form or arrangement of the conductive interconnection between the connecting locations
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0831—Gold
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/085—Copper
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0862—Nickel
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/318—Applications of adhesives in processes or use of adhesives in the form of films or foils for the production of liquid crystal displays
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/20—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive itself
- C09J2301/208—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive itself the adhesive layer being constituted by at least two or more adjacent or superposed adhesive layers, e.g. multilayer adhesive
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/408—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the adhesive layer
Definitions
- the present invention relates to an adhesive film.
- conductive particles are dispersed in an adhesive for connection between a liquid crystal display and TCP (Tape Carrier Package), connection between an FPC (Flexible Printed Circuit) and TCP, or connection between an FPC and a printed wiring board.
- Adhesive is used. Such an adhesive is required to further improve conductivity and reliability.
- Patent Document 1 describes a conductive film provided with a conductive film containing predetermined dendritic silver-coated copper powder particles on a base film, and the conductive film does not contain silver powder. However, it is disclosed that sufficient conductive properties can be obtained.
- An object of the present invention is to provide an adhesive film having excellent reliability.
- One aspect of the present invention is a first adhesive layer containing first conductive particles that are dendritic conductive particles, conductive particles other than the first conductive particles, and a non-conductive core and And a second adhesive layer containing second conductive particles that are conductive particles having a conductive layer provided on the core.
- the first adhesive layer may further contain second conductive particles.
- the volume ratio of the second conductive particles in the first adhesive layer may be smaller than the volume ratio of the second conductive particles in the second adhesive layer.
- the first adhesive layer may not contain the second conductive particles.
- the adhesive film includes the first adhesive layer, the second adhesive layer, and the third adhesive layer in this order, and the third adhesive layer includes: It may be an adhesive film containing third conductive particles that are dendritic conductive particles.
- the third adhesive layer may further contain second conductive particles.
- the volume ratio of the second conductive particles in the third adhesive layer may be smaller than the volume ratio of the second conductive particles in the second adhesive layer.
- the third adhesive layer may not contain the second conductive particles.
- the conductive layer may contain at least one selected from the group consisting of gold, nickel and palladium.
- an adhesive film having excellent reliability can be provided.
- FIG. 1 is a schematic cross-sectional view showing an embodiment (first embodiment) of an adhesive film.
- an adhesive film 1 ⁇ / b> A according to the first embodiment includes a first adhesive layer 2 and a second adhesive layer 3 provided on one surface of the first adhesive layer 2. Is provided.
- the first adhesive layer 2 contains a first adhesive component 4 and first conductive particles 5 dispersed in the first adhesive component 4.
- the second adhesive layer 3 contains a second adhesive component 6 and second conductive particles 7 dispersed in the second adhesive component 6.
- the first adhesive component 4 and the second adhesive component 6 may be the same or different from each other. From the viewpoint of obtaining a stable adhesive force against changes in the environmental temperature, It is the same kind.
- the first adhesive component 4 and the second adhesive component 6 may each be an adhesive component described below.
- the adhesive component is made of, for example, a material that is curable by heat or light, and may be an epoxy adhesive, a radical curable adhesive, a thermoplastic adhesive such as polyurethane or polyvinyl ester, and the like. Since the adhesive component is excellent in heat resistance and moisture resistance after bonding, it may be composed of a crosslinkable material.
- an epoxy adhesive containing an epoxy resin, which is a thermosetting resin, as a main component is preferably used in that it can be cured for a short time, has good connection workability, and has excellent adhesiveness.
- a radical curable adhesive has characteristics such as excellent curability at a low temperature and in a short time as compared with an epoxy-based adhesive, and thus is appropriately used depending on the application.
- the epoxy adhesive contains, for example, a thermosetting material such as an epoxy resin and a curing agent, and may further contain a thermoplastic resin, a coupling agent, a filler, and the like as necessary.
- epoxy resin examples include bisphenol A type epoxy resin, bisphenol F type epoxy resin, bisphenol S type epoxy resin, phenol novolac type epoxy resin, cresol novolak type epoxy resin, bisphenol A novolak type epoxy resin, bisphenol F novolak type epoxy resin.
- These epoxy resins may be halogenated, may be hydrogenated, and may have a structure in which an acryloyl group or a methacryloyl group is added to a side chain.
- These epoxy resins are used individually by 1 type or in combination of 2 or more types.
- the curing agent is not particularly limited as long as it can cure the epoxy resin, and examples thereof include an anion polymerizable catalyst type curing agent, a cationic polymerizable catalyst type curing agent, and a polyaddition type curing agent. Can be mentioned.
- the curing agent is preferably an anion or cation polymerizable catalyst type curing agent because it is excellent in rapid curing and does not require chemical equivalent consideration.
- Anionic or cationic polymerizable catalyst-type curing agents include, for example, imidazole series, hydrazide series, boron trifluoride-amine complex, onium salts (aromatic sulfonium salts, aromatic diazonium salts, aliphatic sulfonium salts, etc.), amine imides, It may be diaminomaleonitrile, melamine and derivatives thereof, polyamine salts, dicyandiamide, and the like, and may be modified products thereof.
- Examples of the polyaddition type curing agent include polyamine, polymercaptan, polyphenol, and acid anhydride.
- hardeners are coated with a polymer material such as polyurethane or polyester, a metal thin film such as nickel or copper, or an inorganic material such as calcium silicate and microencapsulated. This is preferable because it can be extended.
- curing agent is used individually by 1 type or in combination of 2 or more types.
- the content of the curing agent may be 0.05 to 20 parts by mass with respect to 100 parts by mass of the total amount of the thermosetting material and the thermoplastic resin blended as necessary.
- the radical curable adhesive contains, for example, a radical polymerizable material and a radical polymerization initiator (also referred to as a curing agent), and further contains a thermoplastic resin, a coupling agent, a filler and the like as necessary. It's okay.
- the radical polymerizable material for example, any substance having a functional group that is polymerized by radicals can be used without particular limitation.
- the radical polymerizable material includes, for example, an acrylate (including a corresponding methacrylate, the same applies hereinafter) compound, an acryloxy (including a corresponding methacryloxy, the same applies hereinafter) compound, a maleimide compound, a citraconic imide resin, and a nadiimide resin. It may be a radically polymerizable substance such as These radically polymerizable substances may be in a monomer or oligomer state, or in a mixture of a monomer and an oligomer.
- acrylate compound examples include methyl acrylate, ethyl acrylate, isopropyl acrylate, isobutyl acrylate, ethylene glycol diacrylate, diethylene glycol diacrylate, trimethylolpropane triacrylate, tetramethylol methane tetraacrylate, 2-hydroxy-1,3-diacrylate.
- a radically polymerizable substance such as an acrylate compound may be used together with a polymerization inhibitor such as hydroquinone or methyl ether hydroquinone as necessary.
- a radical polymerizable substance such as an acrylate compound preferably has at least one substituent such as a dicyclopentenyl group, a tricyclodecanyl group, and a triazine ring from the viewpoint of improving heat resistance.
- the radical polymerizable substance other than the acrylate compound for example, compounds described in International Publication No. 2009/063827 can be preferably used.
- a radically polymerizable substance is used individually by 1 type or in combination of 2 or more types.
- radical polymerization initiator for example, any compound that decomposes by heating or light irradiation to generate free radicals can be used without particular limitation.
- the radical polymerization initiator may be, for example, a peroxide compound or an azo compound. These compounds are appropriately selected depending on the intended connection temperature, connection time, pot life, and the like.
- the radical polymerization initiator preferably includes diacyl peroxide, peroxydicarbonate, peroxyester, peroxyketal, dialkyl peroxide, hydroperoxide, silyl peroxide, and the like.
- peroxyesters dialkyl peroxides, hydroperoxides, silyl peroxides, and the like.
- Peroxyesters are more preferable from the viewpoint of obtaining high reactivity.
- the radical polymerization initiators for example, the compounds described in International Publication No. 2009/063827 can be suitably used.
- a radical polymerization initiator is used individually by 1 type or in combination of 2 or more types.
- the content of the radical polymerization initiator may be 0.1 to 10 parts by mass with respect to 100 parts by mass of the total amount of the radical polymerizable material and the thermoplastic resin blended as necessary.
- thermoplastic resin blended as necessary in the epoxy adhesive and the radical curable adhesive facilitates imparting excellent film formability to the adhesive, for example.
- the thermoplastic resin include phenoxy resin, polyvinyl formal resin, polystyrene resin, polyvinyl butyral resin, polyester resin, polyamide resin, xylene resin, polyurethane resin, polyester urethane resin, phenol resin, terpene phenol resin, and the like.
- the thermoplastic resin for example, compounds described in International Publication No. 2009/063827 can be preferably used.
- the thermoplastic resin is preferably a phenoxy resin because it is excellent in adhesiveness, compatibility, heat resistance, mechanical strength, and the like.
- a thermoplastic resin is used individually by 1 type or in combination of 2 or more types.
- the content of the thermoplastic resin may be 5 to 80 parts by mass with respect to 100 parts by mass of the total amount of the thermoplastic resin and the thermosetting material when blended in the epoxy adhesive.
- the content of the thermoplastic resin may be 5 to 80 parts by mass with respect to 100 parts by mass of the total amount of the thermoplastic resin and the radical polymerizable substance when blended in the radical curable adhesive.
- the adhesive component examples include a thermal radical curable adhesive containing a thermoplastic resin, a radical polymerizable material containing a radical polymerizable substance that is liquid at 30 ° C., and a radical polymerization initiator.
- the thermal radical curable adhesive has a lower viscosity than the above-described adhesive component.
- the content of the radical polymerizable substance in the thermal radical curable adhesive is preferably 20 to 80 parts by mass, more preferably 30 to 80 parts by mass with respect to 100 parts by mass of the total amount of the thermoplastic resin and the radical polymerizable substance. More preferably, it is 40 to 80 parts by mass.
- the adhesive component may be an epoxy adhesive containing a thermoplastic resin, a thermosetting material containing an epoxy resin that is liquid at 30 ° C., and a curing agent.
- the content of the epoxy resin in the epoxy adhesive is preferably 20 to 80 parts by mass, more preferably 40 to 80 parts by mass with respect to 100 parts by mass of the total amount of the thermoplastic resin and the thermosetting material.
- the amount is preferably 30 to 80 parts by mass.
- the adhesive film 1A is used for connection between an IC chip and a glass substrate, a flexible printed circuit board (FPC) or the like, from the viewpoint of suppressing warpage of the substrate due to a difference in linear expansion coefficient between the IC chip and the substrate.
- the adhesive composition preferably further contains a component that exhibits an internal stress relaxation action. Specific examples of such components include acrylic rubber and elastomer components.
- the adhesive composition may be a radical curable adhesive as described in WO 98/44067.
- the content of the first adhesive component 4 in the first adhesive layer 2 (the volume ratio of the first adhesive component 4 in the first adhesive layer 2) is the total of the first adhesive layer 2. On a product basis, it may be 75% by mass or more or 85% by volume or more, and may be 98% by volume or less or 92% by volume or less.
- the content of the second adhesive component 6 in the second adhesive layer 3 (volume ratio of the second adhesive component 6 in the second adhesive layer 3) is the entire second adhesive layer 3. On a product basis, it may be 80% by mass or more or 90% by mass or more, and may be 98% by volume or less or 95% by volume or less.
- the first adhesive layer 2 contains the first conductive particles 5.
- the first conductive particles 5 have a dendritic shape (also called a dendritic shape), and include one main axis and a plurality of branches that branch two-dimensionally or three-dimensionally from the main axis.
- the 1st electroconductive particle 5 may be formed with metals, such as copper and silver, for example, may be the silver covering copper particle by which a copper particle is coat
- the first conductive particles 5 may be known ones, and are specifically available as, for example, ACBY-2 (Mitsui Metal Mining Co., Ltd.) or CE-1110 (Fukuda Metal Foil Powder Co., Ltd.). .
- the first conductive particles 5 can be manufactured by a known method (for example, the method described in Patent Document 1 described above).
- the content of the first conductive particles 5 in the first adhesive layer 2 is based on the total volume of the first adhesive layer 2 2 volume% or more or 8 volume% or more, and may be 25 volume% or less or 15 volume% or less.
- the thickness of the first adhesive layer 2 may be, for example, 5 ⁇ m or more, 7 ⁇ m or more, or 10 ⁇ m or more, and may be 30 ⁇ m or less, 25 ⁇ m or less, or 20 ⁇ m or less.
- the second adhesive layer 3 contains second conductive particles 7 that are conductive particles other than the first conductive particles 5.
- the second conductive particle 7 has a non-conductive nucleus and a conductive layer provided on the nucleus.
- the core is made of a nonconductive material such as glass, ceramic, or resin, and is preferably made of resin. Examples of the resin include acrylic resin, styrene resin, silicone resin, polybutadiene resin, and a copolymer of monomers constituting these resins.
- the average particle size of the nuclei may be, for example, 2 to 30 ⁇ m.
- the conductive layer is made of, for example, gold, silver, copper, nickel, palladium, or an alloy thereof. From the viewpoint of excellent conductivity, the conductive layer preferably contains at least one selected from gold, nickel and palladium, more preferably contains gold or palladium, and more preferably contains gold.
- the conductive layer is formed by, for example, plating the above metal on the core.
- the thickness of the conductive layer may be 10 to 400 nm, for example.
- the average particle diameter of the second conductive particles 7 is preferably 30 ⁇ m or less, more preferably 25 ⁇ m or less, and even more preferably 20 ⁇ m or less, from the viewpoint that the adhesive film 1A can be suitably thinned.
- the average particle diameter of the second conductive particles 7 may be, for example, 1 ⁇ m or more.
- the average particle diameter of the second conductive particles 7 is measured by a particle size distribution measuring device (Microtrack (product name, Nikkiso Co., Ltd.)) using a laser diffraction / scattering method.
- the content of the second conductive particles 7 in the second adhesive layer 3 is based on the total volume of the second adhesive layer 3 2 volume% or more or 5 volume% or more, and 20 volume% or less or 10 volume% or less.
- the thickness of the second adhesive layer 3 may be, for example, 5 ⁇ m or more, 7 ⁇ m or more, or 10 ⁇ m or more, and may be 30 ⁇ m or less, 25 ⁇ m or less, or 20 ⁇ m or less.
- the first adhesive layer 2 contains only the first conductive particles 5 as conductive particles
- the second adhesive layer 3 contains only the second conductive particles 7 as conductive particles.
- the first adhesive layer may further contain other conductive particles such as the second conductive particles 7
- the second adhesive layer may include other conductive particles such as the first conductive particles 5. It may further contain conductive particles.
- the volume ratio of the second conductive particles 7 in the first adhesive layer is a viewpoint of obtaining an adhesive film with further excellent reliability. Accordingly, the volume ratio of the second conductive particles 7 in the second adhesive layer is preferably smaller than the volume ratio.
- the content of the second conductive particles 7 in the first adhesive layer is, for example, 10% by volume or less, 5% by volume or less, or 2% by volume or less based on the total volume of the first adhesive layer. Good. From the same viewpoint, the first adhesive layer preferably does not contain the second conductive particles 7 as in the first embodiment.
- the adhesive film 1A can be obtained, for example, by forming the first adhesive layer 2 and the second adhesive layer 3 separately and then laminating them.
- the first adhesive layer 2 and the second adhesive layer 3 are obtained, for example, by applying a paste adhesive composition on a resin film such as a PET (polyethylene terephthalate) film and drying it.
- the paste-like adhesive composition is obtained, for example, by heating or dissolving a mixture containing the adhesive components 4 and 6 and the first conductive particles 5 or the second conductive particles 7 in a solvent.
- a solvent for example, a solvent having a boiling point of 50 to 150 ° C. at normal pressure is used.
- the adhesive film 1A according to the first embodiment can be used as an adhesive for adhering the same kind of adherends to each other, and different kinds of adherends (for example, adherends having different thermal expansion coefficients). ) It can also be used as an adhesive for bonding together.
- the adhesive film 1A is suitably used for connection between electronic members.
- FIG. 2 is a cross-sectional view of an essential part schematically showing an example of connection between electronic members.
- a first electronic member 10 including a first substrate 8 and a first electrode 9 formed on, for example, substantially the entire main surface of the first substrate 8;
- the adhesive film 1A is disposed between the second substrate 11 and the second electronic member 13 including the second electrode 12 formed on, for example, substantially the entire surface of the main surface of the second substrate 11.
- connection structure 16A is, for example, 50 to 190 ° C.
- the pressure at the time of pressurization is, for example, 0.1 to 30 MPa. These heating and pressurization are performed in a range of 0.5 to 120 seconds, for example.
- the first substrate 8 and the second substrate 11 may each be a substrate formed of glass, ceramic, polyimide, polycarbonate, polyester, polyethersulfone, or the like.
- the first electrode 9 and the second electrode 12 are each formed of gold, silver, copper, tin, aluminum, ruthenium, rhodium, palladium, osmium, iridium, platinum, indium tin oxide (ITO), or the like. It may be.
- the circuit connection material 15A includes the first conductive particles 5, the second conductive particles 7, and the cured product 17A of the adhesive components 4 and 6. That is, the circuit connection material 15 is obtained by curing the above-described adhesive film 1A.
- the adhesive film 1A according to the first embodiment has the electronic members 10 and 13 even when the first electrode 9 is formed of a material that easily forms an oxide film on the surface (for example, copper or aluminum). It becomes possible to connect each other suitably. This is considered to be due to the fact that the first conductive particles 5 and the second conductive particles 7 are used in combination in the adhesive film 1A. That is, as shown in FIG. 2B, the second conductive particles 7 form a main conduction path for conducting the first electrode 9 and the second electrode 12 to each other, while the first conductive particles 5. However, it is considered that a suitable connection is realized by assisting the electrical connection between the second conductive particles 7 and the first electrode 9.
- the first conductive particles 5 are dendritic conductive particles, the first conductive particles 5 are oxidized even when an oxide film is formed on the surface of the first electrode 9.
- the inventor says that the first electrode 9 can be contacted through the coating, thus allowing a suitable connection between the second conductive particles 7 and the first electrode 9. I guess. Therefore, the adhesive film 1A according to the first embodiment is excellent in reliability as compared with an adhesive film using only one of the first conductive particles and the second conductive particles, that is, a change in environmental temperature. It is considered that the desired conductivity can be maintained.
- the adhesive film 1A according to the first embodiment includes a first adhesive layer 2 containing the first conductive particles 5, a second adhesive layer 3 containing the second conductive particles 7, It becomes possible to connect the electronic members 10 and 13 more suitably. Specifically, when the electronic members 10 and 13 are connected to each other, the first adhesive layer 2 containing the first conductive particles 5 is adhered to the first electrode 9 in the first electronic member 10. Thus, the first conductive particles 5 in the first adhesive layer 2 are in contact with the first electrode 9, and in this state, the second conductive particles 7 in the second adhesive layer 3 are the first conductive particles 5. Contact with. As a result, even when an oxide film is formed on the surface of the first electrode 9, the first conductive particles 5 can come into stronger contact with the first electrode 9, thereby achieving a more stable connection. I think it can be done.
- the reliability is further improved as compared with, for example, a single-layer adhesive film containing both the first conductive particles 5 and the second conductive particles 7. It is thought to do.
- a single-layer adhesive film containing both the first conductive particles 5 and the second conductive particles 7.
- 1 A of adhesive films which concern on 1st Embodiment, containing both the 1st conductive particle 5 and the 2nd conductive particle 7, for example, ensuring the suitable connection of electronic members 10 and 13 mutually.
- the content of the first conductive particles 5 can be reduced.
- the adhesive film may further include a third adhesive layer.
- FIG. 3 is a schematic cross-sectional view showing another embodiment (second embodiment) of the adhesive film.
- the adhesive film 1 ⁇ / b> B according to the second embodiment includes a first adhesive layer 2, a second adhesive layer 3, and a third adhesive layer 18 in this order.
- the first adhesive layer 2 contains a first adhesive component 4 and first conductive particles 5 dispersed in the first adhesive component 4.
- the second adhesive layer 3 contains a second adhesive component 6 and second conductive particles 7 dispersed in the second adhesive component 6.
- the third adhesive layer 18 contains a third adhesive component 19 and third conductive particles 20 dispersed in the third adhesive component 19.
- the first adhesive component 4, the second adhesive component 6 and the third adhesive component 19 may be the same or different from each other, and have a stable adhesive force against changes in environmental temperature. From the viewpoint of being obtained, they are preferably the same as each other.
- the third adhesive component 19 may be the adhesive component described above.
- the content of the third adhesive component 19 in the third adhesive layer 18 is the whole of the third adhesive layer 18. On a product basis, it may be 75% by volume or more or 85% by volume or more, or 98% by volume or less or 92% by volume or less.
- the third adhesive layer 18 contains third conductive particles 20 that are dendritic conductive particles.
- the details of the third conductive particles 20 are the same as those of the first conductive particles 5 described above, and redundant description is omitted here.
- the third conductive particles 20 may be the same type or different from the first conductive particles 5, and are preferably the same type from the viewpoint of obtaining a stable adhesive force against changes in environmental temperature.
- the content of the third conductive particles 20 in the third adhesive layer 18 is based on the total volume of the third adhesive layer 18 2 volume% or more or 8 volume% or more, and may be 25 volume% or less or 15 volume% or less.
- the thickness of the third adhesive layer 18 may be, for example, 5 ⁇ m or more, 7 ⁇ m or more, or 10 ⁇ m or more, and may be 30 ⁇ m or less, 25 ⁇ m or less, or 20 ⁇ m or less.
- the third adhesive layer 18 contains only the third conductive particles 20 as the conductive particles.
- the third adhesive layer includes other conductive materials such as the second conductive particles 7. It may further contain particles.
- the volume ratio of the second conductive particles 7 in the third adhesive layer is a viewpoint of obtaining an adhesive film with further excellent reliability. Accordingly, the volume ratio of the second conductive particles 7 in the second adhesive layer is preferably smaller than the volume ratio.
- the content of the second conductive particles 7 in the third adhesive layer is, for example, 10% by volume or less, 5% by volume or less, or 2% by volume or less based on the total volume of the third adhesive layer. Good. From the same viewpoint, the third adhesive layer preferably does not contain the second conductive particles 7 as in the second embodiment.
- the first adhesive layer 2, the second adhesive layer 3, and the third adhesive layer 18 are separately formed and then laminated. Can be obtained.
- the 3rd adhesive bond layer 18 is obtained by the method similar to the formation method of the 1st adhesive bond layer 2 and the 2nd adhesive bond layer 3 mentioned above.
- the adhesive film 1B according to the second embodiment can also be used as an adhesive for bonding the same kind of adherends to each other, and different kinds of adherends (for example, adherends having different thermal expansion coefficients). ) Can also be used as an adhesive for adhering each other, and is preferably used for connecting electronic members.
- FIG. 4 is a cross-sectional view of an essential part schematically showing another example of connection between electronic members.
- the description which overlaps with the example of the connection of the electronic members shown in FIG. 2 is omitted.
- the adhesive film 1B which concerns on 2nd Embodiment is arrange
- positioned between the 1st electronic member 10 and the 2nd electronic member 13, and laminated body 14B is used.
- the circuit connection material 15B includes the first conductive particles 5, the second conductive particles 7, the third conductive particles 20, and the cured product 17B of the adhesive component. That is, the circuit connection material 15B is formed by curing the adhesive film 1B described above.
- the second electrode 12 in addition to the first electrode 9, the second electrode 12 is formed of a material that easily forms an oxide film on its surface (for example, copper or aluminum). Even if it exists, it becomes possible to connect electronic members 10 and 13 suitably. This is because the third conductive particle 20 is a dendrite-like conductive particle, so that even when an oxide film is formed on the surface of the second electrode 12, the third conductive particle 20 penetrates the oxide film. This is because the second electrode 12 can be contacted. Therefore, the adhesive film 1B according to the second embodiment is superior in reliability as compared with an adhesive film using only one of the first conductive particles and the second conductive particles, that is, a change in environmental temperature. It is considered that the desired conductivity can be maintained.
- the adhesive film 1B according to the second embodiment includes a first adhesive layer 2 containing the first conductive particles 5, a second adhesive layer 3 containing the second conductive particles 7,
- the third adhesive layer 18 containing the third conductive particles 20 in this order, the electronic members 10 and 13 can be more suitably connected. Specifically, even when an oxide film is formed on the surface of the second electrode 12 in addition to the first electrode 9, the first adhesive layer 2 is used when the electronic members 10 and 13 are connected to each other.
- the first conductive particles 5 in the second adhesive layer 3 can be brought into contact with the first electrode 9 preferentially over the second conductive particles 7 in the second adhesive layer 3, and the third conductive layer 18 in the third adhesive layer 18 can be contacted.
- the conductive particles 20 can be brought into contact with the second electrode 12 preferentially over the second conductive particles 7 in the second adhesive layer 3.
- the adhesive film 1B according to the second embodiment for example, compared to an adhesive film made of a single layer containing the first conductive particles 5 (third conductive particles 20) and the second conductive particles 7, for example. It is considered that the reliability is further improved. Further, according to the adhesive film 1B according to the second embodiment, for example, the first conductive particles 5 (third conductive particles 20) and the second conductive particles 5 are secured while ensuring a suitable connection between the electronic members 10 and 13. Compared to a single-layer adhesive film containing the conductive particles 7, the content of the first conductive particles 5 (third conductive particles 20) can be reduced.
- urethane acrylate manufactured by Negami Kogyo Co., Ltd., product name: UN7700
- phosphoric acid ester dimethacrylate manufactured by Kyoeisha Chemical Co., Ltd., product name: Light Ester P-2M
- 1,1-bis (t-hexylperoxy) -3,3,5-trimethylcyclohexane manufactured by NOF Corporation, product name: Perhexa TMH
- conductive particles B1 first conductive particles
- dendritic conductive particles silver-coated copper particles, manufactured by Mitsui Kinzoku Mine Co., Ltd., product name: ACBY-2
- Benzoyl peroxide was added as a polymerization initiator to a mixed solution of divinylbenzene, styrene monomer, and butyl methacrylate, and the polymerization reaction was carried out by heating with uniform stirring at high speed to obtain a fine particle dispersion.
- the fine particle dispersion was filtered and dried under reduced pressure to obtain a block body which is an aggregate of fine particles.
- the block body was pulverized to prepare core bodies (resin particles) having an average particle diameter of 20 ⁇ m, each having a different crosslinking density.
- a palladium catalyst (manufactured by Muromachi Technos Co., Ltd., product name: MK-2605) is supported on the surface of the above-mentioned nuclei, and a nuclei using an accelerator (Muromachi Technos Co., Ltd., product name: MK-370). was activated.
- This nucleus was put into a mixed solution of nickel sulfate aqueous solution, sodium hypophosphite aqueous solution and sodium tartrate aqueous solution heated to 60 ° C., and a pre-electroless plating step was performed. The mixture was stirred for 20 minutes to confirm that hydrogen bubbling stopped.
- Example 1 ⁇ Filming adhesive composition> To 100 parts by volume of solution A1, 45 parts by volume of conductive particles B1 were dispersed to obtain a mixed solution. The obtained mixed solution was applied onto a fluororesin film having a thickness of 80 ⁇ m, and the solvent was removed by drying with hot air at 70 ° C. for 10 minutes to form a 10 ⁇ m-thick film adhesive formed on the fluororesin film. A composition (first adhesive layer) was obtained.
- conductive particles C1 were dispersed in 100 volume parts of the solution A1 to obtain a mixed solution.
- the obtained mixed solution was applied onto a fluororesin film having a thickness of 80 ⁇ m, and the solvent was removed by drying with hot air at 70 ° C. for 10 minutes to form an adhesive on the film having a thickness of 20 ⁇ m formed on the fluororesin film.
- a composition (second adhesive layer) was obtained.
- the first adhesive layer was laminated on the second adhesive layer, and the fluororesin film was peeled off to obtain an adhesive film with a thickness of 30 ⁇ m.
- Example 2 In the same manner as in Example 1, a first adhesive layer and a second adhesive layer were produced. Moreover, the same adhesive bond layer as the 1st adhesive bond layer was produced as a 3rd adhesive bond layer. In the same manner as in Example 1, after laminating the first adhesive layer on the second adhesive layer, the fluororesin film on the second adhesive layer was peeled off, and then the second adhesive layer A third adhesive layer was laminated on the surface opposite to the adhesive layer 1 and the fluororesin film was peeled off to obtain an adhesive film having a thickness of 40 ⁇ m.
- FIGS. 5A and 5B an adhesive film 21 cut out to 6 mm ⁇ 6 mm is disposed at the approximate center of a 6 mm ⁇ 50 mm copper foil 22 and BD-07 manufactured by Ohashi Manufacturing Co., Ltd. is used. Then, heating and pressurization (50 ° C., 0.5 MPa, 2 seconds) was performed for pasting. Subsequently, as shown in FIGS. 5C and 5D, a 50 mm ⁇ 6 mm aluminum foil 23 is prepared, and the adhesive film 21 is covered with the laminate of the copper foil 22 and the adhesive film 21.
- connection resistance (initial) was measured by a four-terminal method. Also, using TSA-43EL manufactured by ESPEC CORP., Hold at ⁇ 20 ° C. for 30 minutes, increase to 100 ° C. over 10 minutes, hold at 100 ° C. for 30 minutes, decrease to ⁇ 20 ° C. over 10 minutes. After performing a heat cycle test for repeating the heat cycle 500 times on the mounting body, the connection resistance (after the heat cycle test) was measured in the same manner as described above.
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Abstract
Description
フェノキシ樹脂(ユニオンカーバイド株式会社製、製品名:PKHC、重量平均分子量:45000)50gを、トルエン(沸点:110.6℃)と酢酸エチル(沸点:77.1℃)との混合溶剤(質量比でトルエン:酢酸エチル=1:1)に溶解して、固形分40質量%のフェノキシ樹脂溶液を得た。このフェノキシ樹脂溶液に、ラジカル重合性物質として、ウレタンアクリレート(根上工業株式会社製、製品名:UN7700)及びリン酸エステルジメタクリレート(共栄社化学株式会社製、製品名:ライトエステルP-2M)と、硬化剤として1,1-ビス(t-ヘキシルパーオキシ)-3,3,5-トリメチルシクロヘキサン(日本油脂株式会社製、製品名:パーヘキサTMH)とを、フェノキシ樹脂:ウレタンアクリレート:リン酸エステルジメタクリレート:硬化剤=10:10:3:2の固形質量比で配合し溶液A1を得た。
ジビニルベンゼン、スチレンモノマー及びブチルメタクリレートの混合溶液に、重合開始剤としてベンゾイルパーオキサイドを投入して、高速で均一撹拌しながら加熱して重合反応を行うことで微粒子分散液を得た。この微粒子分散液を濾過し減圧乾燥することで、微粒子の凝集体であるブロック体を得た。さらに、このブロック体を粉砕することで、それぞれ架橋密度の異なる平均粒子径20μmの核体(樹脂粒子)を作製した。
上記の核体の表面に、パラジウム触媒(ムロマチテクノス株式会社製、製品名:MK-2605)を担持させて、促進剤(ムロマチテクノス株式会社製、製品名:MK-370)を用いて核体を活性化させた。この核体を、60℃に加温された、硫酸ニッケル水溶液、次亜燐酸ナトリウム水溶液及び酒石酸ナトリウム水溶液の混合液中に投入して、無電解メッキ前工程を行った。この混合物を20分間撹拌し、水素の発泡が停止するのを確認した。次に、硫酸ニッケル、次亜リン酸ナトリウム、クエン酸ナトリウム及びメッキ安定剤の混合溶液を添加し、pHが安定するまで撹拌し、水素の発泡が停止するまで無電解メッキ後工程を行った。続いて、メッキ液を濾過し、濾過物を水で洗浄した後、80℃の真空乾燥機で乾燥してニッケルメッキされた導電粒子C1(第2の導電粒子)を作製した。
<接着剤組成物のフィルム化>
100体積部の溶液A1に対して、45体積部の導電粒子B1を分散させて、混合溶液を得た。得られた混合溶液を、厚み80μmのフッ素樹脂フィルム上に塗布し、70℃で10分間熱風乾燥することにより溶剤を除去して、フッ素樹脂フィルム上に形成された厚み10μmのフィルム状の接着剤組成物(第1の接着剤層)を得た。
実施例1と同様にして、第1の接着剤層及び第2の接着剤層を作製した。また、第3の接着剤層として、第1の接着剤層と同一の接着剤層を作製した。実施例1と同様にして、第2の接着剤層に第1の接着剤層をラミネートした後、第2の接着剤層上のフッ素樹脂フィルムを剥がしてから、第2の接着剤層の第1の接着剤層とは反対側の面上に第3の接着剤層をラミネートし、フッ素樹脂フィルムを剥がして、厚み40μmの接着剤フィルムを得た。
100体積部の溶液A1に対して、15体積部の導電粒子C1を分散させて、混合溶液を得た。得られた混合溶液を、厚み80μmのフッ素樹脂フィルム上に塗布し、70℃で10分間熱風乾燥することにより溶剤を除去して、フッ素樹脂フィルム上に形成された厚み40μmのフィルム状の接着剤組成物を得た。
100体積部の溶液A1に対して、30体積部の導電粒子C1を分散させて、混合溶液を得た。得られた混合溶液を、厚み80μmのフッ素樹脂フィルム上に塗布し、70℃で10分間熱風乾燥することにより溶剤を除去して、フッ素樹脂フィルム上に形成された厚み40μmのフィルム状の接着剤組成物を得た。
100体積部の溶液A1に対して、45体積部の導電粒子B1と15体積部の導電粒子C1を分散させて、混合溶液を得た。得られた混合溶液を、厚み80μmのフッ素樹脂フィルム上に塗布し、70℃で10分間熱風乾燥することにより溶剤を除去して、フッ素樹脂フィルム上に形成された厚み30μmのフィルム状の接着剤組成物を得た。
図5(a),(b)に示すように、6mm×6mmに切り出した接着剤フィルム21を、6mm×50mmの銅箔22の略中央に配置し、株式会社大橋製作所製BD-07を用いて加熱加圧(50℃、0.5MPa、2秒間)を行って貼り付けた。続いて、図5(c),(d)に示すように、50mm×6mmのアルミ箔23を用意し、銅箔22と接着剤フィルム21との積層体に対して接着剤フィルム21を覆うように重ねて、株式会社大橋製作所製BD-07で加熱加圧(150℃、0.5MPa、10秒間)を行って、信頼性試験用の実装体を得た。
得られた実装体に対して、図6に示すように電流計、電圧計を接続し、4端子法で接続抵抗(初期)を測定した。また、エスペック株式会社製TSA-43ELを使用して、-20℃で30分間保持、10分間かけて100℃まで昇温、100℃で30分間保持、10分間かけて-20℃まで降温、というヒートサイクルを500回繰り返すヒートサイクル試験を実装体に対して行った後に、上記と同様にして接続抵抗(ヒートサイクル試験後)を測定した。
Claims (7)
- デンドライト状の導電粒子である第1の導電粒子を含有する第1の接着剤層と、
前記第1の導電粒子以外の導電粒子であって、非導電性の核体及び該核体上に設けられた導電層を有する導電粒子である第2の導電粒子を含有する第2の接着剤層と、を備える接着剤フィルム。 - 前記第1の接着剤層が前記第2の導電粒子を更に含有し、
前記第1の接着剤層に占める前記第2の導電粒子の体積割合が、前記第2の接着剤層に占める前記第2の導電粒子の体積割合より小さい、請求項1に記載の接着剤フィルム。 - 前記第1の接着剤層が前記第2の導電粒子を含有しない、請求項1に記載の接着剤フィルム。
- 前記第1の接着剤層と、前記第2の接着剤層と、第3の接着剤層と、をこの順に備え、
前記第3の接着剤層が、デンドライト状の導電粒子である第3の導電粒子を含有する、請求項1~3のいずれか一項に記載の接着剤フィルム。 - 前記第3の接着剤層が前記第2の導電粒子を更に含有し、
前記第3の接着剤層に占める前記第2の導電粒子の体積割合が、前記第2の接着剤層に占める前記第2の導電粒子の体積割合より小さい、請求項4に記載の接着剤フィルム。 - 前記第3の接着剤層が前記第2の導電粒子を含有しない、請求項4に記載の接着剤フィルム。
- 前記導電層が、金、ニッケル及びパラジウムからなる群より選ばれる少なくとも1種を含有する、請求項1~6のいずれか一項に記載の接着剤フィルム。
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US11217229B2 (en) | 2018-06-28 | 2022-01-04 | Tencent Technology (Shenzhen) Company Ltd | Method and apparatus for speech recognition, and electronic device |
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US11242472B2 (en) | 2022-02-08 |
JP2023029350A (ja) | 2023-03-03 |
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KR20190113956A (ko) | 2019-10-08 |
US20190367782A1 (en) | 2019-12-05 |
TW201833941A (zh) | 2018-09-16 |
CN110312770A (zh) | 2019-10-08 |
KR102457667B1 (ko) | 2022-10-20 |
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