WO2023048098A1 - Conductive paste, cured product, sintering accelerator and method for accelerating sintering - Google Patents
Conductive paste, cured product, sintering accelerator and method for accelerating sintering Download PDFInfo
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- WO2023048098A1 WO2023048098A1 PCT/JP2022/034825 JP2022034825W WO2023048098A1 WO 2023048098 A1 WO2023048098 A1 WO 2023048098A1 JP 2022034825 W JP2022034825 W JP 2022034825W WO 2023048098 A1 WO2023048098 A1 WO 2023048098A1
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- WIPO (PCT)
- Prior art keywords
- conductive paste
- sintering
- silver
- meth
- particles
- Prior art date
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- 238000005245 sintering Methods 0.000 title claims abstract description 121
- 238000000034 method Methods 0.000 title claims description 21
- 239000002245 particle Substances 0.000 claims abstract description 142
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- 229910052709 silver Inorganic materials 0.000 claims abstract description 125
- 239000004332 silver Substances 0.000 claims abstract description 125
- 150000001875 compounds Chemical class 0.000 claims abstract description 16
- 239000000178 monomer Substances 0.000 claims description 39
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 22
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- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 15
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 13
- 239000007870 radical polymerization initiator Substances 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- 230000001737 promoting effect Effects 0.000 claims description 7
- 239000012798 spherical particle Substances 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 4
- 239000004848 polyfunctional curative Substances 0.000 claims description 2
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- QJVXKWHHAMZTBY-GCPOEHJPSA-N syringin Chemical compound COC1=CC(\C=C\CO)=CC(OC)=C1O[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 QJVXKWHHAMZTBY-GCPOEHJPSA-N 0.000 description 1
- 229940116411 terpineol Drugs 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 description 1
- UWHCKJMYHZGTIT-UHFFFAOYSA-N tetraethylene glycol Chemical compound OCCOCCOCCOCCO UWHCKJMYHZGTIT-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 230000009974 thixotropic effect Effects 0.000 description 1
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 1
- 125000002889 tridecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- QJAVUVZBMMXBRO-UHFFFAOYSA-N tripentyl phosphate Chemical compound CCCCCOP(=O)(OCCCCC)OCCCCC QJAVUVZBMMXBRO-UHFFFAOYSA-N 0.000 description 1
- 125000002948 undecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 235000012431 wafers Nutrition 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Images
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/20—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the epoxy compounds used
-
- 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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/50—Assembly of semiconductor devices using processes or apparatus not provided for in a single one of the subgroups H01L21/06 - H01L21/326, e.g. sealing of a cap to a base of a container
- H01L21/52—Mounting semiconductor bodies in containers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
- H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L24/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
- H01L24/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
- H01L24/29—Structure, shape, material or disposition of the layer connectors prior to the connecting process of an individual layer connector
-
- 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
- C08K2003/0806—Silver
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
- H01L2224/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
- H01L2224/29—Structure, shape, material or disposition of the layer connectors prior to the connecting process of an individual layer connector
- H01L2224/29001—Core members of the layer connector
- H01L2224/29099—Material
- H01L2224/291—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron [B], silicon [Si], germanium [Ge], arsenic [As], antimony [Sb], tellurium [Te] and polonium [Po], and alloys thereof
- H01L2224/29138—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron [B], silicon [Si], germanium [Ge], arsenic [As], antimony [Sb], tellurium [Te] and polonium [Po], and alloys thereof the principal constituent melting at a temperature of greater than or equal to 950°C and less than 1550°C
- H01L2224/29139—Silver [Ag] as principal constituent
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
- H01L2224/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
- H01L2224/29—Structure, shape, material or disposition of the layer connectors prior to the connecting process of an individual layer connector
- H01L2224/29001—Core members of the layer connector
- H01L2224/29099—Material
- H01L2224/2919—Material with a principal constituent of the material being a polymer, e.g. polyester, phenolic based polymer, epoxy
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/80—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected
- H01L2224/83—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected using a layer connector
- H01L2224/838—Bonding techniques
- H01L2224/8384—Sintering
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Definitions
- the present invention relates to a conductive paste, a cured product, a sintering accelerator, and a sintering acceleration method.
- Electronic parts such as semiconductor elements are mounted on a substrate, for example, via an adhesive layer.
- an adhesive layer may be required to have conductivity, and in such a case, the conductive adhesive layer may be formed from a resin composition containing silver-containing particles, for example.
- a resin composition containing silver-containing particles may be used as a resin composition for producing a conductive paste.
- Techniques related to such resin compositions include, for example, those described in Patent Document 1.
- Patent Document 1 describes a thermosetting resin composition containing (A) plate-shaped fine silver particles, (B) silver powder having an average particle size of 0.5 to 30 ⁇ m, and (C) a thermosetting resin.
- thermosetting resin composition electrical conductivity is exhibited by the formation of contact points between silver particles.
- the following conductive paste, cured product, sintering accelerator, and sintering acceleration method are provided.
- m is an integer of 1 or more and 20 or less.
- n is an integer of 1 or more and 20 or less.
- a sintering accelerator that promotes sintering between silver-containing particles A sintering accelerator containing a compound represented by formula (1) or (2).
- m is an integer of 1 or more and 20 or less.
- n is an integer of 1 or more and 20 or less.
- a method for promoting sintering comprising promoting sintering of silver-containing particles using the sintering accelerator described in [14] above.
- a conductive paste with excellent conductivity is provided.
- FIG. 1 is a cross-sectional view showing a semiconductor device in which an adhesive layer is formed using the conductive paste of this embodiment;
- FIG. 4 is an SEM observation image of a cross section of a cured product formed from the conductive paste of Example 2.
- FIG. 4 is an SEM observation image of a cross section of a cured product formed from the conductive paste of Comparative Example 1.
- FIG. 4 is an SEM observation image of a cross section of a cured product formed from the conductive paste of Comparative Example 1.
- the conductive paste according to this embodiment is a sintering type conductive paste. First, an outline of the sintering technique will be explained.
- the sintering type conductive paste conductivity is ensured by sintering metal particles in the sintering process. That is, the interface between the metal particles disappears due to the action of heat, the metal particles are sintered with each other, and a sintering structure (metal particle connection structure) is formed.
- the sintered structure thus formed functions as a conductive path.
- the sintering type conductive paste usually contains a resin component as a binder.
- the full sintering type is one in which the resin component completely volatilizes in the sintering process and no resin component remains in the cured product.
- a half-sintering type when only a part of the resin component volatilizes in the sintering process and the resin component remains in the cured product, it is called a half-sintering type.
- the resin component remaining in the cured product acts to adhere the sintering structure (metal particle connecting structure) to the adherend.
- FIG. 1 is a cross-sectional view showing a semiconductor device 100 in which an adhesive layer is formed using the conductive paste of this embodiment.
- the adhesive layer 10 is formed by applying the conductive paste according to the present embodiment to the surface of the substrate 30 .
- the semiconductor element 20 is mounted on the surface of the substrate 30 with the adhesive layer 10 interposed therebetween.
- the silver-containing particles contained in the adhesive layer 10 are sintered by sintering.
- the semiconductor element 20 and the substrate 30 are electrically connected by bonding wires 40 and sealed with a mold resin 50. Then, a plurality of solders are applied to the back surface of the substrate 30 opposite to the surface on which the semiconductor element 20 is mounted.
- the semiconductor device 100 is formed by forming the balls 60 .
- the conductive paste according to this embodiment is silver-containing particles; a sintering accelerator that promotes sintering between the silver-containing particles;
- a conductive paste containing The sintering accelerator contains a compound represented by Formula (1) or Formula (2).
- m is an integer of 1 or more and 20 or less.
- n is an integer of 1 or more and 20 or less.
- the adhesive layer formed from the conductive paste of this embodiment has good conductivity.
- sintering accelerator is an agent that accelerates sintering of metal particles.
- the conductive paste of the present embodiment contains a sintering accelerator, sintering of silver-containing particles is promoted compared to a conductive paste that does not contain a sintering accelerator. It is considered that the promotion of sintering in this manner improves electrical conductivity and thermal conductivity.
- the sintering accelerator of the present embodiment promotes sintering
- the dispersibility of the silver-containing particles is enhanced by the sintering accelerator of the present embodiment acting on the surface of the silver-containing particles.
- fusion and mass transfer at the contact interface between the silver-containing particles are promoted, and sintering is promoted.
- the sintering accelerator according to this embodiment can contain one or more compounds represented by formula (1) or formula (2).
- m is an integer of 1 or more and 20 or less.
- n is an integer of 1 or more and 20 or less.
- the sintering accelerator according to this embodiment is characterized by having an ethylene glycol structure or a propylene glycol structure.
- the inventors speculate that these structures interact with the surfaces of the silver-containing fine particles to improve the dispersibility of the silver-containing fine particles.
- m is an integer of 1 or more, preferably 2 or more, more preferably 3 or more, still more preferably 4 or more, and 20 or less, preferably 11 or less, more preferably is an integer of 10 or less, more preferably 9 or less.
- n is an integer of 1 or more, preferably 2 or more, more preferably 3 or more, still more preferably 4 or more, and 20 or less, preferably 13 or less, more preferably is 12 or less, more preferably 11 or less.
- the sintering accelerator according to the present embodiment include: Kyoeisha Chemical Co., Ltd. Epolite 40E (ethylene glycol diglycidyl ether), Epolite 100E (diethylene glycol diglycidyl ether), Epolite 400E (polyethylene glycol diglycidyl ether), Epolite 70P (polypropylene glycol diglycidyl ether), Epolite 200P (tripropylene) glycol diglycidyl ether), Epolite 400P (polypropylene glycol diglycidyl ether); Nagase ChemteX Co., Ltd.
- Denacol EX-810 (ethylene glycol diglycidyl ether), Denacol EX-821 (polyethylene glycol diglycidyl ether), Denacol EX-830 (polyethylene glycol diglycidyl ether), Denacol EX-920 (polypropylene glycol) diglycidyl ether), Denacol EX-931 (polypropylene glycol diglycidyl ether), and the like.
- the conductive paste of the present embodiment may contain only one type of sintering accelerator, or may contain two or more types.
- the content of the sintering accelerator in the conductive paste of the present embodiment is preferably 0.5 parts by mass or more, more preferably 0.7 parts by mass or more when the conductive paste is 100 parts by mass. and more preferably 1.0 parts by mass or more. This further promotes sintering of the silver-containing particles.
- the content of the sintering accelerator in the conductive paste of the present embodiment is preferably 50 parts by mass or less, more preferably 20 parts by mass or less, when the conductive paste is 100 parts by mass. It is preferably 10 parts by mass or less. As a result, the balance of properties such as heat cycle resistance and adhesion to adherends is improved.
- the conductive paste according to this embodiment contains silver-containing particles.
- the silver-containing particles undergo sintering (sintering) by an appropriate heat treatment in the sintering process to form a particle connecting structure (sintering structure).
- the shape of the silver-containing particles according to this embodiment is not particularly limited.
- the silver-containing particles according to this embodiment preferably contain one or more selected from the group consisting of spherical particles, scale-like particles, aggregated particles, and polyhedral particles.
- the contact ratio between the silver-containing particles is further improved, so that a network is easily formed after sintering the conductive paste, and thermal conductivity and electrical conductivity are further improved.
- the term “spherical” is not limited to a perfect sphere, and includes a shape with some irregularities on the surface. Its circularity is, for example, 0.90 or more, preferably 0.92 or more, and more preferably 0.94 or more.
- the median diameter D50 of the silver-containing particles is, for example, 0.01 ⁇ m or more and 50 ⁇ m or less, preferably 0.1 ⁇ m or more and 20 ⁇ m or less, more preferably 0.5 ⁇ m or more and 10 ⁇ m or less.
- the particle size distribution (horizontal axis: particle size, vertical axis: frequency) of the silver-containing particles may be unimodal or multimodal.
- the silver-containing particles include spherical silver-containing particles b1 and scale-like silver-containing particles b2-1. These silver-containing particles are more preferably silver particles consisting essentially of silver.
- the median diameter D 50 of the spherical silver-containing particles b1 is, for example, 0.1 to 20 ⁇ m, preferably 0.5 to 10 ⁇ m, more preferably 0.5 to 5.0 ⁇ m.
- the specific surface area of the spherical silver-containing particles b1 is, for example, 0.1 to 2.5 m 2 /g, preferably 0.5 to 2.3 m 2 /g, more preferably 0.8 to 2.0 m 2 /g. be.
- the tap density of the spherical silver-containing particles b1 is, for example, 1.5 to 6.0 g/cm 3 , preferably 2.5 to 5.8 g/cm 3 , more preferably 4.5 to 5.5 g/cm 3 . be.
- the circularity of the spherical silver-containing particles b1 is, for example, 0.90 or more, preferably 0.92 or more, and more preferably 0.94 or more. Satisfying each of these properties provides an excellent balance of thermal conductivity, sinterability, resistance to heat cycles, and the like.
- the median diameter D50 of the scale-like silver-containing particles b2-1 is, for example, 0.1 to 20 ⁇ m, preferably 1.0 to 15 ⁇ m, more preferably 2.0 to 10 ⁇ m.
- the specific surface area of the scale-like silver-containing particles b2-1 is, for example, 0.1 to 2.5 m 2 /g, preferably 0.2 to 2.0 m 2 /g, more preferably 0.25 to 1.2 m 2 /g.
- the tap density of the scale-like silver-containing particles b2-1 is, for example, 1.5 to 6.0 g/cm 3 , preferably 2.5 to 5.9 g/cm 3 , more preferably 4.0 to 5.8 g/cm 3 . cm3 . Satisfying each of these properties provides an excellent balance of thermal conductivity, sinterability, resistance to heat cycles, and the like.
- thermo conductivity and electrical conductivity especially improved.
- the ratio of the content of the spherical silver-containing particles b1 to the content of the scale-like silver-containing particles b2-1 (b1/b2-1) is preferably 0.1 or more and 10 or less, more preferably 0.3 or more and 5 or less. , particularly preferably 0.5 or more and 3 or less.
- the contact ratio between the silver-containing particles is particularly improved, so that a network is easily formed after sintering the conductive paste, and the thermal conductivity and electrical conductivity are particularly improved.
- the ratio (b1/b2-1) of the median diameter D50 of the spherical silver-containing particles b1 to the median diameter D50 of the scale-like silver-containing particles b2-1 is preferably 0.01 or more and 0.8 or less, more preferably It is 0.05 or more and 0.6 or less.
- the ratio of the tap density of the spherical silver-containing particles b1 to the tap density of the scale-like silver-containing particles b2-1 (b1/b2-1) is preferably 0.5 or more and 2.0 or less, more preferably 0.7 or more. 1.2 or less.
- the filling rate of the silver-containing particles is improved, and the contact rate between the silver-containing particles is particularly improved, so that after sintering the conductive paste, a network is easily formed and thermal conductivity and electrical conductivity are improved. especially improve.
- the median diameter D50 of the silver-containing particles can be obtained by, for example, particle image measurement using a flow type particle image analyzer FPIA (registered trademark)-3000 manufactured by Sysmex Corporation. More specifically, the particle diameter of the silver-containing particles can be determined by measuring the volume-based median diameter in a wet manner using this device.
- FPIA flow type particle image analyzer
- the content of the silver-containing particles in the conductive paste according to the present embodiment is preferably 40 parts by mass or more, more preferably 60 parts by mass or more, when the total non-volatile components of the conductive paste are 100 parts by mass. and more preferably 80 parts by mass or more. Thereby, electrical conductivity and thermal conductivity can be further improved.
- the content of the silver-containing particles in the conductive paste according to the present embodiment is preferably 98 parts by mass or less, more preferably 97 parts by mass, when the total non-volatile components of the conductive paste are 100 parts by mass. parts or less, more preferably 96 parts by mass or less. This results in an excellent balance of thermal conductivity, sinterability, adhesion to adherends, resistance to heat cycles, and the like.
- the silver-containing particles may be (i) particles consisting essentially of silver, or (ii) particles consisting of silver and components other than silver. Moreover, (i) and (ii) may be used together as the metal-containing particles.
- Examples of the particles consisting essentially of silver include silver particles.
- Examples of particles composed of silver and components other than silver include silver-coated resin particles.
- Silver-coated resin particles are particles in which the surfaces of resin particles are coated with silver.
- Silver-coated resin particles whose surfaces are coated with silver have good thermal conductivity and are softer than particles made only of silver. It becomes easier to design the rate to an appropriate value.
- the silver-coated resin particles it is sufficient that at least a part of the surface of the resin particles is covered with a silver layer. Of course, the entire surface of the resin particles may be covered with silver.
- the silver layer preferably covers 50% or more, more preferably 75% or more, and still more preferably 90% or more of the surface of the resin particles.
- the silver layer covers substantially the entire surface of the resin particles. From another point of view, when the silver-coated resin particles are cut along a certain cross section, it is preferable that the silver layer is observed all around the cross section.
- the mass ratio of resin/silver in the silver-coated resin particles is, for example, 90/10 to 10/90, preferably 80/20 to 20/80, more preferably 70/30 to 30/70. be.
- the "resin" in the silver-coated resin particles examples include silicone resins, (meth)acrylic resins, phenol resins, polystyrene resins, melamine resins, polyamide resins, polytetrafluoroethylene resins, and the like. Of course, resins other than these may be used. Moreover, only one resin may be used, or two or more resins may be used in combination. From the viewpoint of elastic properties and heat resistance, the resin is preferably a silicone resin or a (meth)acrylic resin.
- Particles consisting essentially of silver can be obtained from, for example, DOWA Hi-Tech Co., Ltd., Fukuda Metal Foil & Powder Co., Ltd., and the like.
- silver-coated resin particles among particles composed of silver and components other than silver can be obtained, for example, from Mitsubishi Materials Corporation, Sekisui Chemical Co., Ltd., Sanno Co., Ltd., and the like.
- the conductive paste according to this embodiment may contain components other than the sintering accelerator and the silver-containing particles.
- the conductive paste according to the present embodiment preferably contains an epoxy monomer.
- the epoxy monomer according to this embodiment has an epoxy group in its structure.
- the epoxy monomer according to the present embodiment may be a monofunctional epoxy monomer having only one epoxy group in its structure, or a polyfunctional epoxy monomer having two or more epoxy groups in its structure. good.
- Examples of monofunctional epoxy monomers include 4-tert-butylphenyl glycidyl ether, m,p-cresyl glycidyl ether, phenyl glycidyl ether, and cresyl glycidyl ether.
- polyfunctional epoxy monomers include bisphenol compounds such as bisphenol A, bisphenol F and biphenol, or derivatives thereof; hydrogenated bisphenol A, hydrogenated bisphenol F, hydrogenated biphenol, cyclohexanediol, cyclohexanedimethanol, cyclohexanediethanol Diols having an alicyclic structure or derivatives thereof; aliphatic diols such as butanediol, hexanediol, octanediol, nonanediol, decanediol, or difunctional epoxidized derivatives thereof; trimethylolpropane skeleton, tri trifunctional ones having a hydroxyphenylmethane skeleton and aminophenol skeleton; polyfunctional ones obtained by epoxidizing phenol novolak resins, cresol novolak resins, phenol aralkyl resins, biphenyl aralkyl resins, naphthol aralkyl
- the content of the epoxy monomer in the conductive paste of the present embodiment is preferably 0.5 parts by mass or more, more preferably 0.7 parts by mass or more, when the conductive paste is 100 parts by mass. It is preferably 1.0 parts by mass or more. As a result, the balance of properties such as heat cycle resistance and adhesion to adherends is improved.
- the content of the epoxy monomer in the conductive paste of the present embodiment is preferably 50 parts by mass or less, more preferably 20 parts by mass or less, and even more preferably 100 parts by mass of the conductive paste. is 10 parts by mass or less.
- the conductive paste according to the present embodiment preferably contains a (meth)acrylic monomer.
- the acrylic monomer according to this embodiment is a monomer having a (meth)acrylic group in its structure.
- the acrylic monomer according to the present embodiment may be a monofunctional acrylic monomer having only one (meth)acrylic group in its structure, or a polyfunctional acrylic monomer having two or more (meth)acrylic groups in its structure. It may be an acrylic monomer.
- the (meth)acrylic group is a concept including a (meth)acrylate group. Further, in the present embodiment, the (meth)acryl group is a concept representing an acryl group and a methacryl group, and the (meth)acryloyl group is a concept representing an acryloyl group and a methacryloyl group.
- monofunctional acrylic monomers include methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, isopropyl (meth) acrylate, butyl (meth) acrylate, isobutyl (meth) acrylate, s-butyl (meth) acrylate, and s-butyl (meth) acrylate.
- acrylate t-butyl (meth)acrylate, butoxyethyl (meth)acrylate, pentyl (meth)acrylate, hexyl (meth)acrylate, 2-ethylhexyl (meth)acrylate, heptyl (meth)acrylate, octylheptyl (meth)acrylate , nonyl (meth)acrylate, decyl (meth)acrylate, undecyl (meth)acrylate, lauryl (meth)acrylate, tridecyl (meth)acrylate, tetradecyl (meth)acrylate, pentadecyl (meth)acrylate, hexadecyl (meth)acrylate, stearyl (meth)acrylate, behenyl (meth)acrylate, 2-hydroxyethyl (meth)acrylate, 2-hydroxypropyl (meth)acrylate, 3-chloro-2-hydroxypropyl
- bifunctional acrylic monomers include ethylene glycol di(meth)acrylate, diethylene glycol di(meth)acrylate, triethylene glycol di(meth)acrylate, tetraethylene glycol di(meth)acrylate, polyethylene glycol di(meth)acrylate, Propylene glycol di(meth)acrylate, dipropylene glycol di(meth)acrylate, tripropylene glycol di(meth)acrylate, tetrapropylene glycol di(meth)acrylate, polypropylene glycol di(meth)acrylate, 1,3-butanediol di (Meth)acrylates, 2-methyl-1,3-propanediol di(meth)acrylate, 1,4-butanediol di(meth)acrylate, neopentyl glycol di(meth)acrylate, 3-methyl-1,5- Pentanediol di(meth)acrylate, 1,6-hexanediol di(meth)
- the content of the (meth)acrylic monomer in the conductive paste of the present embodiment is preferably 0.3 parts by mass or more, more preferably 0.5 parts by mass, when the conductive paste is 100 parts by mass. Above, more preferably 0.6 parts by mass or more. As a result, the balance of properties such as heat cycle resistance and adhesion to adherends is improved.
- the content of the (meth)acrylic monomer in the conductive paste of the present embodiment is preferably 50 parts by mass or less, more preferably 20 parts by mass or less, when the conductive paste is 100 parts by mass. More preferably, it is 10 parts by mass or less.
- the conductive paste according to the present embodiment contains an epoxy monomer or an epoxy resin
- the conductive paste according to the present embodiment preferably contains a curing agent. Thereby, the curing shrinkage of the epoxy monomer or the epoxy resin can be caused, and the silver-containing particles can be aggregated.
- the content of the curing agent in the conductive paste of the present embodiment is preferably 0.5 parts by mass or more, more preferably 1.0 parts by mass or more, when the conductive paste is 100 parts by mass. It is preferably 1.2 parts by mass or more. As a result, the balance of properties such as heat cycle resistance and adhesion to adherends is improved.
- the content of the curing agent in the conductive paste of the present embodiment is preferably 50 parts by mass or less, more preferably 20 parts by mass or less, even more preferably when the conductive paste is 100 parts by mass. is 10 parts by mass or less.
- the conductive paste according to this embodiment preferably contains a phenol-based curing agent.
- Phenolic curing agents include, for example, phenol novolak resins, cresol novolak resins, bisphenol novolak resins, phenol-biphenyl novolak resins and other novolak phenol resins; polyvinylphenol; polyfunctional phenol resins such as triphenylmethane phenol resins; modified phenol resins such as terpene-modified phenol resins and dicyclopentadiene-modified phenol resins; phenol aralkyl resins having a phenylene skeleton and/or biphenylene skeleton; phenol aralkyl-type phenol resins such as naphthol aralkyl resins having a phenylene and/or biphenylene skeleton; A, bisphenol compounds such as bisphenol F (dihydroxydiphenylmethane); and compounds having a biphenylene skeleton such as 4,4'-biphenol.
- bisphenol compounds such as bisphenol F (dihydroxydipheny
- the conductive paste according to the present embodiment may contain a curing accelerator that accelerates the reaction between the epoxy monomer or epoxy resin and the curing agent.
- Curing accelerators include, for example, imidazole-based curing accelerators; organic phosphines, tetrasubstituted phosphonium compounds, phosphobetaine compounds, adducts of phosphine compounds and quinone compounds, adducts of phosphonium compounds and silane compounds containing phosphorus atoms, etc.
- Compounds; amidines and tertiary amines such as dicyandiamide, 1,8-diazabicyclo[5.4.0]undecene-7, and benzyldimethylamine; nitrogen atom-containing compounds such as quaternary ammonium salts of the above amidines or the above tertiary amines; can be mentioned.
- the content of the curing accelerator in the conductive paste of the present embodiment is preferably 0.01 parts by mass or more, more preferably 0.05 parts by mass or more, when the conductive paste is 100 parts by mass. More preferably, it is 0.07 parts by mass or more. As a result, the balance of properties such as heat cycle resistance and adhesion to adherends is improved.
- the content of the curing accelerator in the conductive paste of the present embodiment is preferably 10 parts by mass or less, more preferably 5 parts by mass or less when the conductive paste is 100 parts by mass.
- the conductive paste according to this embodiment preferably contains an imidazole curing accelerator.
- imidazole curing accelerators examples include 2-phenyl-1H-imidazole-4,5-dimethanol, 2-phenyl-4-methyl-5-hydroxymethylimidazole, 2-methylimidazole, 2-phenylimidazole, 2 , 4-diamino-6-[2-methylimidazolyl-(1)]-ethyl-s-triazine, 2-undecylimidazole, 2-heptadecylimidazole, 2,4-diamino-6-[2-methylimidazolyl- (1)]-ethyl-s-triazine isocyanurate, 2-phenylimidazole isocyanurate, 2-methylimidazole isocyanurate, 1-cyanoethyl-2-phenylimidazolium trimellitate, 1-cyanoethyl- 2-undecylimidazolium trimellitate and the like can be mentioned.
- the conductive paste according to the present embodiment contains a (meth)acrylic monomer
- the conductive paste according to the present embodiment preferably contains a radical polymerization initiator.
- the (meth)acrylic monomer can be caused to cure and shrink, and the silver-containing particles can be aggregated.
- azo compounds, peroxides, and the like can be used as radical polymerization initiators.
- peroxide examples include organic peroxides such as diacyl peroxide, dialkyl peroxide, and peroxyketal, and more specifically, ketone peroxides such as methyl ethyl ketone peroxide and cyclohexanone peroxide.
- peroxyketals such as 1,1-di(t-butylperoxy)cyclohexane and 2,2-di(4,4-di(t-butylperoxy)cyclohexyl)propane;
- Hydroperoxides such as p-menthane hydroperoxide, diisopropylbenzene hydroperoxide, 1,1,3,3-tetramethylbutyl hydroperoxide, cumene hydroperoxide, t-butyl hydroperoxide; di(2-t-butylperoxyisopropyl)benzene, dicumyl peroxide, 2,5-dimethyl-2,5-di(t-butylperoxy)hexane, t-butylcumyl peroxide, di-t- Dialkyl peroxides such as xyl peroxide, 2,5-dimethyl-2,5-di(t-butylperoxy)hexyne-3, di-t-butyl peroxide
- the content of the radical polymerization initiator in the conductive paste of the present embodiment is preferably 0.01 parts by mass or more, more preferably 0.03 parts by mass or more when the conductive paste is 100 parts by mass. and more preferably 0.04 parts by mass or more. As a result, the balance of properties such as heat cycle resistance and adhesion to adherends is improved.
- the content of the radical polymerization initiator in the conductive paste of the present embodiment is preferably 10 parts by mass or less, more preferably 5 parts by mass or less when the conductive paste is 100 parts by mass. .
- the conductive paste according to the present embodiment preferably contains a solvent. This can improve the fluidity of the conductive paste and contribute to the improvement of workability.
- Examples of the solvent according to the present embodiment include methyl carbitol, ethyl carbitol, butyl carbitol, methyl carbitol acetate, ethyl carbitol acetate, butyl carbitol acetate, acetylacetone, methyl isobutyl ketone (MIBK), anone, di Acetone alcohol, ethyl cellosolve, methyl cellosolve, butyl cellosolve, ethyl cellosolve acetate, methyl cellosolve acetate, butyl cellosolve acetate, ethyl alcohol, propyl alcohol, butyl alcohol, pentyl alcohol, hexyl alcohol, heptyl alcohol, octyl alcohol, nonyl alcohol, decyl alcohol, ethylene Glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monopropyl ether, ethylene glycol monobuty
- the content of the solvent in the conductive paste of the present embodiment is preferably 1 part by mass or more, more preferably 2 parts by mass or more, and even more preferably 3 parts by mass when the conductive paste is 100 parts by mass. Department or above.
- the content of the solvent in the conductive paste of the present embodiment is preferably 50 parts by mass or less, more preferably 20 parts by mass or less, further preferably when the conductive paste is 100 parts by mass. It is 10 parts by mass or less.
- polymer components such as epoxy resin, (meth)acrylic resin, silicone resin, butadiene rubber; inorganic fillers such as silica and alumina; thixotropic adjustment such as fine silica Coupling agents: antioxidants; dispersing agents; antifoaming agents; leveling agents and other components may also be added.
- the content ratio of these components can be appropriately set according to the application of the conductive paste.
- the conductive paste of the present embodiment contains, for example, butadiene rubber among the above components, it preferably has an epoxy group from the viewpoint of the reactivity of other components.
- the content of the butadiene rubber having an epoxy group (hereinafter referred to as epoxy group-containing butadiene rubber) in the conductive paste of the present embodiment reduces the storage elastic modulus of the effect obtained from the paste and improves the adhesion to the substrate or the like.
- the conductive paste when it is 100 parts by mass, it is preferably 0.1 parts by mass or more, more preferably 0.5 parts by mass or more, and still more preferably 1.0 parts by mass or more, and It is preferably 50 parts by mass or less, more preferably 40 parts by mass or less, and even more preferably 30 parts by mass or less.
- a specific example of the epoxy group-containing butadiene rubber is NISSO-PB JP-200 (epoxy-modified polybutadiene) manufactured by Nippon Soda Co., Ltd.
- the conductive paste according to the present embodiment can be obtained by mixing the components described above and, if necessary, other components by a conventionally known method.
- the conductive paste according to this embodiment is preferably pasty at 20°C. That is, the conductive paste according to the present embodiment can be preferably applied to a substrate or the like like glue at 20°C. As a result, the conductive paste of the present embodiment can be preferably used as an adhesive for semiconductor elements or the like. Of course, depending on the applied process, the conductive paste of the present embodiment may be in the form of a relatively low viscosity varnish.
- the conductive paste according to this embodiment is applied to a glass plate so that the thickness after sintering is 0.05 mm, and the temperature is raised from 30 ° C. to 200 ° C. over 60 minutes in a nitrogen atmosphere.
- the volume resistivity of the cured product is preferably 9.5 ⁇ cm or less, more preferably 9.2 ⁇ cm or less. be.
- the conductivity of the cured product obtained from the conductive paste of the present embodiment can be improved.
- the volume resistivity of the cured product is usually 4.0 ⁇ cm or more, preferably 4.5 ⁇ cm or more.
- a semiconductor device can be manufactured using the conductive paste of the present embodiment.
- a semiconductor device can be manufactured by using the conductive paste of the present embodiment as an "adhesive" between a substrate and a semiconductor element.
- the semiconductor device of the present embodiment includes, for example, a base material and a semiconductor element mounted on the base material via an adhesive layer obtained by sintering the conductive paste described above.
- Examples of semiconductor elements include ICs, LSIs, power semiconductor elements (power semiconductors), and various other elements.
- substrates include various semiconductor wafers, lead frames, BGA substrates, mounting substrates, heat spreaders, and heat sinks.
- FIG. 1 is a cross-sectional view showing an example of a semiconductor device.
- the adhesive layer 10 is formed by applying the conductive paste according to the present embodiment to the surface of the substrate 30 .
- the semiconductor element 20 is mounted on the surface of the substrate 30 with the adhesive layer 10 interposed therebetween.
- the thickness of the adhesive layer 10 is preferably 5 ⁇ m or more, more preferably 10 ⁇ m or more, and even more preferably 20 ⁇ m or more. Thereby, the conductive reliability of the adhesive layer is improved. Also, the thickness of the adhesive layer 10 is preferably 100 ⁇ m or less, more preferably 50 ⁇ m or less.
- the method of applying the conductive paste is not particularly limited. Specifically, a dispensing method, a printing method, an inkjet method, and the like can be mentioned.
- the silver-containing particles contained in the adhesive layer 10 are sintered by sintering.
- the semiconductor element 20 and the substrate 30 are electrically connected by bonding wires 40 and sealed with a mold resin 50. Then, a plurality of solders are applied to the back surface of the substrate 30 opposite to the surface on which the semiconductor element 20 is mounted.
- the semiconductor device 100 is formed by forming the balls 60 .
- the cured product according to this embodiment is obtained by sintering the conductive paste.
- the sintering temperature is preferably 150°C or higher, more preferably 180°C or higher, and even more preferably 200°C or higher. This can further promote sintering between the silver-containing particles.
- the sintering temperature is preferably 300°C or lower, more preferably 280°C or lower, and even more preferably 250°C or lower. This makes it easier to adjust the volatilization of the monomer components and the like during sintering, making it easier to adjust the physical properties of the cured product.
- the volume resistivity of the cured product according to this embodiment is preferably 10.0 ⁇ cm or less, more preferably 9.5 ⁇ cm or less, and even more preferably 9.2 ⁇ cm or less. Thereby, the electroconductivity of hardened
- the storage elastic modulus (E') of the cured product according to this embodiment is preferably 20 GPa or less, more preferably 17 GPa or less, and even more preferably 15 GPa or less. Thereby, the adhesion between the cured product and the adherend can be improved.
- the storage elastic modulus (E') of the cured product according to this embodiment is preferably 1.0 GPa or higher, more preferably 3.0 GPa or higher, and even more preferably 5.0 GPa or higher. Thereby, the strength of the cured product can be improved.
- the cured product according to the present embodiment is obtained by sintering a conductive paste containing a sintering accelerator. is promoted.
- the sintering accelerator promotes sintering between silver-containing particles, and includes a compound represented by formula (1) or formula (2).
- m is an integer of 1 or more and 20 or less.
- n is an integer of 1 or more and 20 or less.
- the sintering accelerator of the present embodiment promotes sintering
- the dispersibility of the silver-containing particles is enhanced by the sintering accelerator of the present embodiment acting on the surface of the silver-containing particles.
- fusion and mass transfer at the contact interface between the silver-containing particles are promoted, and sintering is promoted.
- the sintering accelerator according to this embodiment can be blended in various resin compositions including conductive paste.
- composition of the resin composition containing the sintering accelerator according to the present embodiment is not particularly limited.
- the content of the sintering accelerator in the resin composition is not particularly limited. Above, more preferably 1.0 parts by mass or more. This further promotes sintering of the silver-containing particles.
- the content of the sintering accelerator in the resin composition is preferably 50 parts by mass or less, more preferably 20 parts by mass or less, and even more preferably 100 parts by mass of the resin composition. It is 10 parts by mass or less. As a result, the balance of properties such as heat cycle resistance and adhesion to adherends is improved.
- the method for promoting sintering according to this embodiment is a method for promoting sintering of silver-containing particles using the sintering accelerator described above.
- the sintering of the silver-containing particles can be promoted by adding the sintering accelerator described above to various resin compositions including conductive pastes.
- Varnishes 1 to 11 and A1 to A7 to be blended in the conductive paste for jet dispensing were prepared by uniformly mixing each component according to the formulations shown in Tables 1 and 3.
- the unit of content of each component in Tables 1 and 3 is parts by mass.
- Sintering accelerator 5 polyethylene glycol diglycidyl ether
- Epoxy monomer 1 trimethylolpropane polyglycidyl ether (product name: Denacol EX-321L, manufactured by Nagase ChemteX Corporation)
- Epoxy monomer 2 Bisphenol F type epoxy monomer (product name: RE-303S, manufactured by Nippon Kayaku Co., Ltd.)
- Epoxy group-containing butadiene rubber epoxy-modified polybutadiene (product name: NISSO-PB JP-200, manufactured by Nippon Soda Co., Ltd.)
- ((meth)acrylic monomer) ⁇ (Meth) acrylic monomer 1: 1,4-cyclohexanedimethanol monoacrylate (product name: CHDMMA, manufactured by Nippon Kasei Co., Ltd.) ⁇ (Meth) acrylic monomer 2: ethylene glycol dimethacrylate (product name: Light Ester EG, manufactured by Kyoeisha Chemical Co., Ltd.)
- Curing agent 1 Bisphenol F type phenolic resin (product name: DIC-BPF, manufactured by DIC Corporation)
- Curing accelerator 1 2-phenyl-1H-imidazole-4,5-dimethanol (product name: 2PHZ-PW, manufactured by Shikoku Kasei Co., Ltd.)
- Radical polymerization initiator ⁇ Radical polymerization initiator 1: dicumyl peroxide (product name: Perkadox BC, manufactured by Kayaku Noorion Co., Ltd.)
- each component was uniformly mixed according to the formulations shown in Tables 2 and 4 to obtain a conductive paste.
- the unit of content of each component in Tables 2 and 4 is parts by mass.
- volume resistivity of the surface of the obtained cured product was measured by a DC four-electrode method using a milliohmmeter (manufactured by Hioki) using electrodes with an electrode spacing of 40 mm.
- Example 2 The SEM observation image of Example 2 is shown in FIG. 2, and the SEM observation image of Comparative Example 1 is shown in FIG. In each SEM image, white portions are silver-containing particles. In the SEM observation image of Example 2, as compared with the SEM observation image of Comparative Example 1, it can be seen that the silver-containing particles are more fused together and sintering is promoted.
- adhesive layer 20 semiconductor element 30 substrate 40 bonding wire 50 mold resin 60 solder ball 100 semiconductor device
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Abstract
Description
[1]
銀含有粒子と、
前記銀含有粒子同士がシンタリングすることを促進するシンタリング促進剤と、
を含有する導電性ペーストであって、
前記シンタリング促進剤が式(1)または式(2)で示される化合物を含む、導電性ペースト。
[2]
上記[1]に記載の導電性ペーストであって、
前記シンタリング促進剤が式(1)で示される化合物を含み、式(1)中、mは1以上11以下の整数である、導電性ペースト。
[3]
上記[1]または[2]に記載の導電性ペーストであって、
前記シンタリング促進剤が式(2)で示される化合物を含み、式(2)中、nは2以上13以下の整数である、導電性ペースト。
[4]
上記[1]~[3]のいずれかに記載の導電性ペーストであって、
前記銀含有粒子が球状粒子、鱗片状粒子、凝集状粒子、および多面体形状の粒子からなる群から選択される1種または2種以上を含む、導電性ペースト。
[5]
上記[4]に記載の導電性ペーストであって、
前記銀含有粒子が球状粒子、鱗片状粒子、凝集状粒子、および多面体形状の粒子からなる群から選択される2種以上を含む、導電性ペースト。
[6]
上記[1]~[5]のいずれかに記載の導電性ペーストであって、
エポキシモノマーをさらに含む、導電性ペースト。
[7]
上記[6]に記載の導電性ペーストであって、
フェノール系硬化剤をさらに含む、導電性ペースト。
[8]
上記[6]または[7]に記載の導電性ペーストであって、
イミダゾール系硬化促進剤をさらに含む、導電性ペースト。
[9]
上記[1]~[8]のいずれかに記載の導電性ペーストであって、
(メタ)アクリルモノマーをさらに含む、導電性ペースト。
[10]
上記[9]に記載の導電性ペーストであって、
ラジカル重合開始剤をさらに含む、導電性ペースト。
[11]
上記[1]~[10]のいずれかに記載の導電性ペーストであって、
溶剤をさらに含む、導電性ペースト。
[12]
上記[1]~[11]のいずれかに記載の導電性ペーストであって、
当該導電性ペーストを、焼結処理後の厚みが0.05mmになるようにガラス板上に塗布し、窒素雰囲気下で、30℃から200℃まで60分間かけて昇温し、続けて200℃で120分間焼結処理し、硬化物を得た場合の、当該硬化物の体積抵抗率が4.0μΩ・cm以上9.5μΩ・cm以下である、導電性ペースト。
[13]
上記[1]~[12]のいずれかに記載の導電性ペーストを焼結して得られる硬化物。
[14]
銀含有粒子同士がシンタリングすることを促進するシンタリング促進剤であって、
式(1)または式(2)で示される化合物を含む、シンタリング促進剤。
[15]
上記[14]に記載のシンタリング促進剤を用いて銀含有粒子のシンタリングを促進する、シンタリング促進方法。 According to the present invention, the following conductive paste, cured product, sintering accelerator, and sintering acceleration method are provided.
[1]
silver-containing particles;
a sintering accelerator that promotes sintering between the silver-containing particles;
A conductive paste containing
A conductive paste, wherein the sintering accelerator contains a compound represented by formula (1) or (2).
[2]
The conductive paste according to [1] above,
A conductive paste, wherein the sintering accelerator contains a compound represented by formula (1), wherein m is an integer of 1 or more and 11 or less.
[3]
The conductive paste according to [1] or [2] above,
A conductive paste, wherein the sintering accelerator contains a compound represented by formula (2), wherein n is an integer of 2 or more and 13 or less.
[4]
The conductive paste according to any one of [1] to [3] above,
A conductive paste, wherein the silver-containing particles include one or more selected from the group consisting of spherical particles, scale-like particles, aggregated particles, and polyhedral particles.
[5]
The conductive paste according to [4] above,
A conductive paste, wherein the silver-containing particles include two or more selected from the group consisting of spherical particles, scale-like particles, aggregated particles, and polyhedral particles.
[6]
The conductive paste according to any one of [1] to [5] above,
A conductive paste further comprising an epoxy monomer.
[7]
The conductive paste according to [6] above,
A conductive paste further comprising a phenolic hardener.
[8]
The conductive paste according to [6] or [7] above,
An electrically conductive paste, further comprising an imidazole curing accelerator.
[9]
The conductive paste according to any one of [1] to [8] above,
An electrically conductive paste further comprising a (meth)acrylic monomer.
[10]
The conductive paste according to [9] above,
A conductive paste, further comprising a radical polymerization initiator.
[11]
The conductive paste according to any one of [1] to [10] above,
A conductive paste further comprising a solvent.
[12]
The conductive paste according to any one of [1] to [11] above,
The conductive paste was applied to a glass plate so that the thickness after sintering was 0.05 mm, and the temperature was raised from 30°C to 200°C over 60 minutes in a nitrogen atmosphere, and then to 200°C. is sintered for 120 minutes to obtain a cured product having a volume resistivity of 4.0 μΩ·cm or more and 9.5 μΩ·cm or less.
[13]
A cured product obtained by sintering the conductive paste according to any one of [1] to [12] above.
[14]
A sintering accelerator that promotes sintering between silver-containing particles,
A sintering accelerator containing a compound represented by formula (1) or (2).
[15]
A method for promoting sintering, comprising promoting sintering of silver-containing particles using the sintering accelerator described in [14] above.
<シンタリング技術の概要>
本実施形態にかかる導電性ペーストは、シンタリングタイプの導電性ペーストである。まず、シンタリング技術の概要について説明する。 [Conductive paste]
<Overview of sintering technology>
The conductive paste according to this embodiment is a sintering type conductive paste. First, an outline of the sintering technique will be explained.
半導体装置100においては、基板30の表面に本実施形態にかかる導電性ペーストが塗布されることにより接着層10が形成される。次いで、上記基板30の表面に上記接着層10を介して半導体素子20が搭載される。 FIG. 1 is a cross-sectional view showing a
In the
本実施形態にかかる導電性ペーストは、
銀含有粒子と、
上記銀含有粒子同士がシンタリングすることを促進するシンタリング促進剤と、
を含有する導電性ペーストであって、
上記シンタリング促進剤が式(1)または式(2)で示される化合物を含む。
The conductive paste according to this embodiment is
silver-containing particles;
a sintering accelerator that promotes sintering between the silver-containing particles;
A conductive paste containing
The sintering accelerator contains a compound represented by Formula (1) or Formula (2).
以下、本実施形態の導電性ペーストが含有する各成分について説明する。 <Each component>
Each component contained in the conductive paste of the present embodiment will be described below.
シンタリング促進剤とは、金属粒子のシンタリングを促進する剤である。 (sintering accelerator)
A sintering accelerator is an agent that accelerates sintering of metal particles.
mが上記範囲であることにより、銀含有粒子の分散性がより向上し、導電性ペーストから形成された接着層の導電性および熱伝導性がより向上する。
上記式(2)中、nは、1以上、好適には2以上、より好適には3以上、さらに好適には4以上の整数であり、そして、20以下、好適には13以下、より好適には12以下、さらに好適には11以下である。
nが上記範囲であることにより、銀含有粒子の分散性がより向上し、導電性ペーストから形成された接着層の導電性および熱伝導性がより向上する。 In the above formula (1), m is an integer of 1 or more, preferably 2 or more, more preferably 3 or more, still more preferably 4 or more, and 20 or less, preferably 11 or less, more preferably is an integer of 10 or less, more preferably 9 or less.
When m is within the above range, the dispersibility of the silver-containing particles is further improved, and the electrical conductivity and thermal conductivity of the adhesive layer formed from the conductive paste are further improved.
In the above formula (2), n is an integer of 1 or more, preferably 2 or more, more preferably 3 or more, still more preferably 4 or more, and 20 or less, preferably 13 or less, more preferably is 12 or less, more preferably 11 or less.
When n is within the above range, the dispersibility of the silver-containing particles is further improved, and the electrical conductivity and thermal conductivity of the adhesive layer formed from the conductive paste are further improved.
共栄社化学株式会社製のエポライト40E(エチレングリコールジグリシジルエーテル)、エポライト100E(ジエチレングリコールジグリシジルエーテル)、エポライト400E(ポリエチレングリコールジグリシジルエーテル)、エポライト70P(ポリプロピレングリコールジグリシジルエーテル)、エポライト200P(トリプロピレングリコールジグリシジルエーテル)、エポライト400P(ポリプロピレングリコールジグリシジルエーテル);
ナガセケムテックス株式会社製のデナコールEX-810(エチレングリコールジグリシジルエーテル)、デナコールEX-821(ポリエチレングリコールジグリシジルエーテル)、デナコールEX-830(ポリエチレングリコールジグリシジルエーテル)、デナコールEX-920(ポリプロピレングリコールジグリシジルエーテル)、デナコールEX-931(ポリプロピレングリコールジグリシジルエーテル)等を挙げることができる。 Specific examples of the sintering accelerator according to the present embodiment include:
Kyoeisha Chemical Co., Ltd. Epolite 40E (ethylene glycol diglycidyl ether), Epolite 100E (diethylene glycol diglycidyl ether), Epolite 400E (polyethylene glycol diglycidyl ether), Epolite 70P (polypropylene glycol diglycidyl ether), Epolite 200P (tripropylene) glycol diglycidyl ether), Epolite 400P (polypropylene glycol diglycidyl ether);
Nagase ChemteX Co., Ltd. Denacol EX-810 (ethylene glycol diglycidyl ether), Denacol EX-821 (polyethylene glycol diglycidyl ether), Denacol EX-830 (polyethylene glycol diglycidyl ether), Denacol EX-920 (polypropylene glycol) diglycidyl ether), Denacol EX-931 (polypropylene glycol diglycidyl ether), and the like.
本実施形態にかかる導電性ペーストは、銀含有粒子を含有する。 (Silver-containing particles)
The conductive paste according to this embodiment contains silver-containing particles.
なお、本実施形態において、「球状」とは、完全な真球に限られず、表面に若干の凹凸がある形状等も包含する。その円形度は、例えば0.90以上、好ましくは0.92以上、より好ましくは0.94以上である。 By including the silver-containing particles b2 in the silver-containing particles, it is possible to suppress resin cracks in the molded product obtained from the conductive paste and to suppress an increase in the coefficient of linear expansion.
In the present embodiment, the term “spherical” is not limited to a perfect sphere, and includes a shape with some irregularities on the surface. Its circularity is, for example, 0.90 or more, preferably 0.92 or more, and more preferably 0.94 or more.
銀含有粒子の粒度分布(横軸:粒子径、縦軸:頻度)は、単峰性であっても多峰性であってもよい。 The median diameter D50 of the silver-containing particles is, for example, 0.01 μm or more and 50 μm or less, preferably 0.1 μm or more and 20 μm or less, more preferably 0.5 μm or more and 10 μm or less. By setting the median diameter D50 to an appropriate value, it is easy to balance thermal conductivity, sinterability, resistance to heat cycles, and the like. Also, by setting the D50 to an appropriate value, it may be possible to improve the workability of application/adhesion.
The particle size distribution (horizontal axis: particle size, vertical axis: frequency) of the silver-containing particles may be unimodal or multimodal.
球状の銀含有粒子b1の比表面積は、例えば0.1~2.5m2/g、好ましくは0.5~2.3m2/g、より好ましくは0.8~2.0m2/gである。
球状の銀含有粒子b1のタップ密度は、例えば1.5~6.0g/cm3、好ましくは2.5~5.8g/cm3、より好ましくは4.5~5.5g/cm3である。
球状の銀含有粒子b1の円形度は、例えば0.90以上、好ましくは0.92以上、より好ましくは0.94以上である。
これらの各特性を満たすことにより、熱伝導性、焼結性、ヒートサイクルに対する耐性などのバランスに優れる。 The median diameter D 50 of the spherical silver-containing particles b1 is, for example, 0.1 to 20 μm, preferably 0.5 to 10 μm, more preferably 0.5 to 5.0 μm.
The specific surface area of the spherical silver-containing particles b1 is, for example, 0.1 to 2.5 m 2 /g, preferably 0.5 to 2.3 m 2 /g, more preferably 0.8 to 2.0 m 2 /g. be.
The tap density of the spherical silver-containing particles b1 is, for example, 1.5 to 6.0 g/cm 3 , preferably 2.5 to 5.8 g/cm 3 , more preferably 4.5 to 5.5 g/cm 3 . be.
The circularity of the spherical silver-containing particles b1 is, for example, 0.90 or more, preferably 0.92 or more, and more preferably 0.94 or more.
Satisfying each of these properties provides an excellent balance of thermal conductivity, sinterability, resistance to heat cycles, and the like.
鱗片状の銀含有粒子b2-1の比表面積は、例えば0.1~2.5m2/g、好ましくは0.2~2.0m2/g、より好ましくは0.25~1.2m2/gである。
鱗片状の銀含有粒子b2-1のタップ密度は、例えば1.5~6.0g/cm3、好ましくは2.5~5.9g/cm3、より好ましくは4.0~5.8g/cm3である。
これらの各特性を満たすことにより、熱伝導性、焼結性、ヒートサイクルに対する耐性などのバランスに優れる。 The median diameter D50 of the scale-like silver-containing particles b2-1 is, for example, 0.1 to 20 μm, preferably 1.0 to 15 μm, more preferably 2.0 to 10 μm.
The specific surface area of the scale-like silver-containing particles b2-1 is, for example, 0.1 to 2.5 m 2 /g, preferably 0.2 to 2.0 m 2 /g, more preferably 0.25 to 1.2 m 2 /g.
The tap density of the scale-like silver-containing particles b2-1 is, for example, 1.5 to 6.0 g/cm 3 , preferably 2.5 to 5.9 g/cm 3 , more preferably 4.0 to 5.8 g/cm 3 . cm3 .
Satisfying each of these properties provides an excellent balance of thermal conductivity, sinterability, resistance to heat cycles, and the like.
これにより、鱗片状の銀含有粒子間の空隙に、球状の銀含有粒子が効率的に充填され、銀含有粒子同士の接触率が特に向上することから、当該導電性ペーストの焼結後においてネットワークが容易に形成され熱伝導性および電気伝導性が特に向上する。 The ratio (b1/b2-1) of the median diameter D50 of the spherical silver-containing particles b1 to the median diameter D50 of the scale-like silver-containing particles b2-1 is preferably 0.01 or more and 0.8 or less, more preferably It is 0.05 or more and 0.6 or less.
As a result, the voids between the scale-like silver-containing particles are efficiently filled with the spherical silver-containing particles, and the contact ratio between the silver-containing particles is particularly improved. Therefore, after sintering the conductive paste, the network is easily formed, and thermal conductivity and electrical conductivity are particularly improved.
これにより、銀含有粒子の充填率が向上し、銀含有粒子同士の接触率が特に向上することから、当該導電性ペーストの焼結後においてネットワークが容易に形成され熱伝導性および電気伝導性が特に向上する。 The ratio of the tap density of the spherical silver-containing particles b1 to the tap density of the scale-like silver-containing particles b2-1 (b1/b2-1) is preferably 0.5 or more and 2.0 or less, more preferably 0.7 or more. 1.2 or less.
As a result, the filling rate of the silver-containing particles is improved, and the contact rate between the silver-containing particles is particularly improved, so that after sintering the conductive paste, a network is easily formed and thermal conductivity and electrical conductivity are improved. especially improve.
別観点として、銀コート樹脂粒子をある断面で切断したときには、その断面の周囲全部に銀層が確認されることが好ましい。 Specifically, in the silver-coated resin particles, the silver layer preferably covers 50% or more, more preferably 75% or more, and still more preferably 90% or more of the surface of the resin particles. Particularly preferably, in silver-coated resin particles, the silver layer covers substantially the entire surface of the resin particles.
From another point of view, when the silver-coated resin particles are cut along a certain cross section, it is preferable that the silver layer is observed all around the cross section.
弾性特性や耐熱性の観点から、樹脂は、シリコーン樹脂または(メタ)アクリル樹脂が好ましい。 Examples of the "resin" in the silver-coated resin particles include silicone resins, (meth)acrylic resins, phenol resins, polystyrene resins, melamine resins, polyamide resins, polytetrafluoroethylene resins, and the like. Of course, resins other than these may be used. Moreover, only one resin may be used, or two or more resins may be used in combination.
From the viewpoint of elastic properties and heat resistance, the resin is preferably a silicone resin or a (meth)acrylic resin.
本実施形態にかかる導電性ペーストは、シンタリング促進剤と銀含有粒子以外の成分を含有していてもよい。 (other ingredients)
The conductive paste according to this embodiment may contain components other than the sintering accelerator and the silver-containing particles.
本実施形態にかかる導電性ペーストは、好適にはエポキシモノマーを含有する。 - Epoxy monomer The conductive paste according to the present embodiment preferably contains an epoxy monomer.
本実施形態にかかる導電性ペーストは、好適には(メタ)アクリルモノマーを含有する。 - (Meth)acrylic monomer The conductive paste according to the present embodiment preferably contains a (meth)acrylic monomer.
シクロペンチル(メタ)アクリレート、シクロヘキシル(メタ)アクリレート、1,4-シクロヘキサンジメタノールモノ(メタ)アクリレート、シクロペンチル(メタ)アクリレート、ジシクロペンタニル(メタ)アクリレート、ジシクロペンテニル(メタ)アクリレート、イソボルニル(メタ)アクリレート、3-メチル-3-オキセタニルメチル(メタ)アクリレート、1-アダマンチル(メタ)アクリレートのような脂環式(メタ)アクリレート;
フェニル(メタ)アクリレート、ノニルフェニル(メタ)アクリレート、p-クミルフェニル(メタ)アクリレート、o-ビフェニル(メタ)アクリレート、1-ナフチル(メタ)アクリレート、2-ナフチル(メタ)アクリレート、ベンジル(メタ)アクリレート、2-ヒドロキシ-3-フェノキシプロピル(メタ)アクリレート、2-ヒドロキシ-3-(o-フェニルフェノキシ)プロピル(メタ)アクリレート、2-ヒドロキシ-3-(1-ナフトキシ)プロピル(メタ)アクリレート、2-ヒドロキシ-3-(2-ナフトキシ)プロピル(メタ)アクリレートのような芳香族(メタ)アクリレート;
2-テトラヒドロフルフリル(メタ)アクリレート、N-(メタ)アクリロイルオキシエチルヘキサヒドロフタルイミド、2-(メタ)アクリロイルオキシエチル-N-カルバゾールのような複素環式(メタ)アクリレート
などを挙げることができる。 Examples of monofunctional acrylic monomers include methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, isopropyl (meth) acrylate, butyl (meth) acrylate, isobutyl (meth) acrylate, s-butyl (meth) acrylate, and s-butyl (meth) acrylate. ) acrylate, t-butyl (meth)acrylate, butoxyethyl (meth)acrylate, pentyl (meth)acrylate, hexyl (meth)acrylate, 2-ethylhexyl (meth)acrylate, heptyl (meth)acrylate, octylheptyl (meth)acrylate , nonyl (meth)acrylate, decyl (meth)acrylate, undecyl (meth)acrylate, lauryl (meth)acrylate, tridecyl (meth)acrylate, tetradecyl (meth)acrylate, pentadecyl (meth)acrylate, hexadecyl (meth)acrylate, stearyl (meth)acrylate, behenyl (meth)acrylate, 2-hydroxyethyl (meth)acrylate, 2-hydroxypropyl (meth)acrylate, 3-chloro-2-hydroxypropyl (meth)acrylate, 2-hydroxybutyl (meth)acrylate , aliphatic (meth)acrylates such as phenoxy polyethylene glycol (meth)acrylates;
Cyclopentyl (meth)acrylate, cyclohexyl (meth)acrylate, 1,4-cyclohexanedimethanol mono (meth)acrylate, cyclopentyl (meth)acrylate, dicyclopentanyl (meth)acrylate, dicyclopentenyl (meth)acrylate, isobornyl ( Alicyclic (meth)acrylates such as meth)acrylate, 3-methyl-3-oxetanylmethyl (meth)acrylate, 1-adamantyl (meth)acrylate;
Phenyl (meth)acrylate, nonylphenyl (meth)acrylate, p-cumylphenyl (meth)acrylate, o-biphenyl (meth)acrylate, 1-naphthyl (meth)acrylate, 2-naphthyl (meth)acrylate, benzyl (meth)acrylate , 2-hydroxy-3-phenoxypropyl (meth)acrylate, 2-hydroxy-3-(o-phenylphenoxy)propyl (meth)acrylate, 2-hydroxy-3-(1-naphthoxy)propyl (meth)acrylate, 2 - aromatic (meth)acrylates such as hydroxy-3-(2-naphthoxy)propyl (meth)acrylate;
Heterocyclic (meth)acrylates such as 2-tetrahydrofurfuryl (meth)acrylate, N-(meth)acryloyloxyethylhexahydrophthalimide, 2-(meth)acryloyloxyethyl-N-carbazole, and the like can be mentioned. .
シクロヘキサンジメタノールジ(メタ)アクリレート、トリシクロデカンジメタノールジ(メタ)アクリレート、水添ビスフェノールAジ(メタ)アクリレート、水添ビスフェノールFジ(メタ)アクリレートのような脂環式ジ(メタ)アクリレート;
ビスフェノールAジ(メタ)アクリレート、ビスフェノールFジ(メタ)アクリレート、ビスフェノールAFジ(メタ)アクリレート、エトキシ化ビスフェノールAジ(メタ)アクリレート、フルオレン型ジ(メタ)アクリレートのような芳香族ジ(メタ)アクリレート;
イソシアヌル酸ジ(メタ)アクリレートのような複素環式ジ(メタ)アクリレート
などを挙げることができる。 Examples of bifunctional acrylic monomers include ethylene glycol di(meth)acrylate, diethylene glycol di(meth)acrylate, triethylene glycol di(meth)acrylate, tetraethylene glycol di(meth)acrylate, polyethylene glycol di(meth)acrylate, Propylene glycol di(meth)acrylate, dipropylene glycol di(meth)acrylate, tripropylene glycol di(meth)acrylate, tetrapropylene glycol di(meth)acrylate, polypropylene glycol di(meth)acrylate, 1,3-butanediol di (Meth)acrylates, 2-methyl-1,3-propanediol di(meth)acrylate, 1,4-butanediol di(meth)acrylate, neopentyl glycol di(meth)acrylate, 3-methyl-1,5- Pentanediol di(meth)acrylate, 1,6-hexanediol di(meth)acrylate, 2-butyl-2-ethyl-1,3-propanediol di(meth)acrylate, 1,9-nonanediol di(meth)acrylate aliphatic di(meth)acrylates such as acrylates, 1,10-decanediol di(meth)acrylates, glycerine di(meth)acrylates;
Alicyclic di(meth)acrylates such as cyclohexanedimethanol di(meth)acrylate, tricyclodecanedimethanol di(meth)acrylate, hydrogenated bisphenol A di(meth)acrylate, hydrogenated bisphenol F di(meth)acrylate ;
Aromatic di(meth)acrylates such as bisphenol A di(meth)acrylate, bisphenol F di(meth)acrylate, bisphenol AF di(meth)acrylate, ethoxylated bisphenol A di(meth)acrylate, fluorene type di(meth)acrylate acrylate;
Heterocyclic di(meth)acrylates such as isocyanuric acid di(meth)acrylate and the like can be mentioned.
イソシアヌル酸トリ(メタ)アクリレートのような複素環式(メタ)アクリレートなどを挙げることができる。 Trimethylolpropane tri(meth)acrylate, pentaerythritol tri(meth)acrylate, ditrimethylolpropane tetra(meth)acrylate, pentaerythritol tetra(meth)acrylate, dipentaerythritol penta( aliphatic (meth)acrylates such as meth)acrylates, dipentaerythritol hexa(meth)acrylate, ethoxylated glycerol tri(meth)acrylate;
Heterocyclic (meth)acrylates such as isocyanuric acid tri(meth)acrylate and the like can be mentioned.
本実施形態にかかる導電性ペーストがエポキシモノマーやエポキシ樹脂を含む場合、本実施形態にかかる導電性ペーストは硬化剤を含むことが好ましい。これにより、エポキシモノマーやエポキシ樹脂を硬化収縮させ、銀含有粒子を凝集させることができる。 - Curing Agent When the conductive paste according to the present embodiment contains an epoxy monomer or an epoxy resin, the conductive paste according to the present embodiment preferably contains a curing agent. Thereby, the curing shrinkage of the epoxy monomer or the epoxy resin can be caused, and the silver-containing particles can be aggregated.
本実施形態にかかる導電性ペーストは、エポキシモノマーまたはエポキシ樹脂と、硬化剤との反応を促進させる硬化促進剤を含んでもよい。 • Curing Accelerator The conductive paste according to the present embodiment may contain a curing accelerator that accelerates the reaction between the epoxy monomer or epoxy resin and the curing agent.
本実施形態にかかる導電性ペーストが(メタ)アクリルモノマーを含む場合、本実施形態にかかる導電性ペーストはラジカル重合開始剤を含むことが好ましい。これにより、(メタ)アクリルモノマーを硬化収縮させ、銀含有粒子を凝集させることができる。 - Radical polymerization initiator When the conductive paste according to the present embodiment contains a (meth)acrylic monomer, the conductive paste according to the present embodiment preferably contains a radical polymerization initiator. As a result, the (meth)acrylic monomer can be caused to cure and shrink, and the silver-containing particles can be aggregated.
p-メンタンハイドロパーオキサイド、ジイソプロピルベンゼンハイドロパーオキサイド、1,1,3,3-テトラメチルブチルハイドロパーオキサイド、クメンハイドロパーオキサイド、t-ブチルハイドロパーオキサイド等のハイドロパーオキサイド;
ジ(2-t-ブチルパーオキシイソプロピル)ベンゼン、ジクミルパーオキサイド、2,5-ジメチル-2,5-ジ(t-ブチルパーオキシ)ヘキサン、t-ブチルクミルパーオキサイド、ジ-t-へキシルパーオキサイド、2,5-ジメチル-2,5-ジ(t-ブチルパーオキシ)ヘキシン-3、ジ-t-ブチルパーオキサイド等のジアルキルパーオキサイド;
ジベンゾイルパーオキサイド、ジ(4-メチルベンゾイル)パーオキサイド等のジアシルパーオキサイド;
ジ-n-プロピルパーオキシジカーボネート、ジイソプロピルパーオキシジカーボネート等のパーオキシジカーボネート;
2,5-ジメチル-2,5-ジ(ベンゾイルパーオキシ)ヘキサン、t-へキシルパーオキシベンゾエート、t-ブチルパーオキシベンゾエート、t-ブチルパーオキシ2-エチルヘキサノエート等のパーオキシエステルなどを挙げることができる。 Examples of the peroxide include organic peroxides such as diacyl peroxide, dialkyl peroxide, and peroxyketal, and more specifically, ketone peroxides such as methyl ethyl ketone peroxide and cyclohexanone peroxide. peroxyketals such as 1,1-di(t-butylperoxy)cyclohexane and 2,2-di(4,4-di(t-butylperoxy)cyclohexyl)propane;
Hydroperoxides such as p-menthane hydroperoxide, diisopropylbenzene hydroperoxide, 1,1,3,3-tetramethylbutyl hydroperoxide, cumene hydroperoxide, t-butyl hydroperoxide;
di(2-t-butylperoxyisopropyl)benzene, dicumyl peroxide, 2,5-dimethyl-2,5-di(t-butylperoxy)hexane, t-butylcumyl peroxide, di-t- Dialkyl peroxides such as xyl peroxide, 2,5-dimethyl-2,5-di(t-butylperoxy)hexyne-3, di-t-butyl peroxide;
Diacyl peroxides such as dibenzoyl peroxide and di(4-methylbenzoyl) peroxide;
Peroxydicarbonates such as di-n-propyl peroxydicarbonate and diisopropyl peroxydicarbonate;
Peroxyesters such as 2,5-dimethyl-2,5-di(benzoylperoxy)hexane, t-hexylperoxybenzoate, t-butylperoxybenzoate, t-butylperoxy 2-ethylhexanoate, etc. can be mentioned.
本実施形態にかかる導電性ペーストは溶剤を含むことが好ましい。これにより、導電性ペーストの流動性を向上させ、作業性の向上に寄与することができる。 - Solvent The conductive paste according to the present embodiment preferably contains a solvent. This can improve the fluidity of the conductive paste and contribute to the improvement of workability.
アセトン、メチルエチルケトン、メチルイソブチルケトン、シクロヘキサノン、ジアセトンアルコール(4-ヒドロキシ-4-メチル-2-ペンタノン)、2-オクタノン、イソホロン(3,5,5-トリメチル-2-シクロヘキセン-1-オン)もしくはジイソブチルケトン(2,6-ジメチル-4-ヘプタノン)等のケトン類;
酢酸エチル、酢酸ブチル、ジエチルフタレート、ジブチルフタレート、アセトキシエタン、酪酸メチル、ヘキサン酸メチル、オクタン酸メチル、デカン酸メチル、メチルセロソルブアセテート、エチレングリコールモノブチルエーテルアセテート、プロピレングリコールモノメチルエーテルアセテート、1,2-ジアセトキシエタン、リン酸トリブチル、リン酸トリクレジルもしくはリン酸トリペンチル等のエステル類;
テトラヒドロフラン、ジプロピルエーテル、エチレングリコールジメチルエーテル、エチレングリコールジエチルエーテル、エチレングリコールジブチルエーテル、プロピレングリコールジメチルエーテル、エトキシエチルエーテル、1,2-ビス(2-ジエトキシ)エタンもしくは1,2-ビス(2-メトキシエトキシ)エタン等のエーテル類;
酢酸2-(2-ブトキシエトキシ)エタン等のエステルエーテル類;
2-(2-メトキシエトキシ)エタノール等のエーテルアルコール類、トルエン、キシレン、n-パラフィン、イソパラフィン、ドデシルベンゼン、テレピン油、ケロシンもしくは軽油等の炭化水素類;
アセトニトリルもしくはプロピオニトリル等のニトリル類;
アセトアミドもしくはN,N-ジメチルホルムアミド等のアミド類;
低分子量の揮発性シリコンオイル、または揮発性有機変成シリコンオイル等を挙げることができる。 Examples of the solvent according to the present embodiment include methyl carbitol, ethyl carbitol, butyl carbitol, methyl carbitol acetate, ethyl carbitol acetate, butyl carbitol acetate, acetylacetone, methyl isobutyl ketone (MIBK), anone, di Acetone alcohol, ethyl cellosolve, methyl cellosolve, butyl cellosolve, ethyl cellosolve acetate, methyl cellosolve acetate, butyl cellosolve acetate, ethyl alcohol, propyl alcohol, butyl alcohol, pentyl alcohol, hexyl alcohol, heptyl alcohol, octyl alcohol, nonyl alcohol, decyl alcohol, ethylene Glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monopropyl ether, ethylene glycol monobutyl ether, propylene glycol monomethyl ether, propylene glycol monoethyl ether, propylene glycol monopropyl ether, propylene glycol monobutyl ether, methylmethoxybutanol, α-terpineol , β-terpineol, γ-terpineol, terpineol (mixture of α, β, γ), dihydroterpineol, hexylene glycol, benzyl alcohol, 2-phenylethyl alcohol, isopalmityl alcohol, isostearyl alcohol, lauryl alcohol, ethylene glycol , alcohols such as propylene glycol or glycerin;
Acetone, methyl ethyl ketone, methyl isobutyl ketone, cyclohexanone, diacetone alcohol (4-hydroxy-4-methyl-2-pentanone), 2-octanone, isophorone (3,5,5-trimethyl-2-cyclohexen-1-one) or Ketones such as diisobutyl ketone (2,6-dimethyl-4-heptanone);
Ethyl acetate, butyl acetate, diethyl phthalate, dibutyl phthalate, acetoxyethane, methyl butyrate, methyl hexanoate, methyl octanoate, methyl decanoate, methyl cellosolve acetate, ethylene glycol monobutyl ether acetate, propylene glycol monomethyl ether acetate, 1,2- Esters such as diacetoxyethane, tributyl phosphate, tricresyl phosphate or tripentyl phosphate;
Tetrahydrofuran, dipropyl ether, ethylene glycol dimethyl ether, ethylene glycol diethyl ether, ethylene glycol dibutyl ether, propylene glycol dimethyl ether, ethoxyethyl ether, 1,2-bis(2-diethoxy)ethane or 1,2-bis(2-methoxyethoxy) ) ethers such as ethane;
ester ethers such as acetic acid 2-(2-butoxyethoxy)ethane;
Ether alcohols such as 2-(2-methoxyethoxy)ethanol, hydrocarbons such as toluene, xylene, n-paraffin, isoparaffin, dodecylbenzene, turpentine oil, kerosene or light oil;
Nitriles such as acetonitrile or propionitrile;
amides such as acetamide or N,N-dimethylformamide;
Examples include low-molecular-weight volatile silicone oils and volatile organically modified silicone oils.
これらの成分の含有割合は、導電性ペーストを適用する用途に合わせて適宜設定することができる。 In the conductive paste according to the present embodiment, if necessary, polymer components such as epoxy resin, (meth)acrylic resin, silicone resin, butadiene rubber; inorganic fillers such as silica and alumina; thixotropic adjustment such as fine silica Coupling agents: antioxidants; dispersing agents; antifoaming agents; leveling agents and other components may also be added.
The content ratio of these components can be appropriately set according to the application of the conductive paste.
本実施形態の導電性ペーストにおける、エポキシ基を有するブタジエンゴム(以下、エポキシ基含有ブタジエンゴムという)の含有量は、ペーストから得られる効果物の貯蔵弾性率を低減させ基板等との密着性を向上させる観点から、当該導電性ペーストを100質量部としたとき、好ましくは0.1質量部以上、より好ましくは0.5質量部以上、さらに好ましくは1.0質量部以上であり、そして、好ましくは50質量部以下、より好ましくは40質量部以下、さらに好ましくは30質量部以下である。
エポキシ基含有ブタジエンゴムの具体例としては、日本曹達株式会社製のNISSO-PB JP-200(エポキシ変性ポリブタジエン)を挙げることができる。 When the conductive paste of the present embodiment contains, for example, butadiene rubber among the above components, it preferably has an epoxy group from the viewpoint of the reactivity of other components.
The content of the butadiene rubber having an epoxy group (hereinafter referred to as epoxy group-containing butadiene rubber) in the conductive paste of the present embodiment reduces the storage elastic modulus of the effect obtained from the paste and improves the adhesion to the substrate or the like. From the viewpoint of improvement, when the conductive paste is 100 parts by mass, it is preferably 0.1 parts by mass or more, more preferably 0.5 parts by mass or more, and still more preferably 1.0 parts by mass or more, and It is preferably 50 parts by mass or less, more preferably 40 parts by mass or less, and even more preferably 30 parts by mass or less.
A specific example of the epoxy group-containing butadiene rubber is NISSO-PB JP-200 (epoxy-modified polybutadiene) manufactured by Nippon Soda Co., Ltd.
本実施形態にかかる導電性ペーストは、好適には、20℃でペースト状である。すなわち、本実施形態にかかる導電性ペーストは、好適には、20℃で、糊のようにして基板等に塗布することができる。このことにより、本実施形態の導電性ペーストを、半導体素子の接着剤などとして好ましく用いることができる。
もちろん、適用されるプロセスなどによっては、本実施形態の導電性ペーストは、比較的低粘度のワニス状などであってもよい。 <Physical properties>
The conductive paste according to this embodiment is preferably pasty at 20°C. That is, the conductive paste according to the present embodiment can be preferably applied to a substrate or the like like glue at 20°C. As a result, the conductive paste of the present embodiment can be preferably used as an adhesive for semiconductor elements or the like.
Of course, depending on the applied process, the conductive paste of the present embodiment may be in the form of a relatively low viscosity varnish.
本実施形態の導電性ペーストを用いて、半導体装置を製造することができる。例えば、本実施形態の導電性ペーストを、基材と半導体素子との「接着剤」として用いることで、半導体装置を製造することができる。 <Application>
A semiconductor device can be manufactured using the conductive paste of the present embodiment. For example, a semiconductor device can be manufactured by using the conductive paste of the present embodiment as an "adhesive" between a substrate and a semiconductor element.
図1は、半導体装置の一例を示す断面図である。 An example of a semiconductor device will be described below with reference to the drawings.
FIG. 1 is a cross-sectional view showing an example of a semiconductor device.
本実施形態にかかる硬化物は、上記の導電性ペーストを焼結して得られるものである。 [Cured product]
The cured product according to this embodiment is obtained by sintering the conductive paste.
また、本実施形態にかかる硬化物の体積抵抗率は、通常4.0μΩ・cm以上、好適には4.5μΩ・cm以上である。 The volume resistivity of the cured product according to this embodiment is preferably 10.0 μΩ·cm or less, more preferably 9.5 μΩ·cm or less, and even more preferably 9.2 μΩ·cm or less. Thereby, the electroconductivity of hardened|cured material can be improved.
Moreover, the volume resistivity of the cured product according to the present embodiment is usually 4.0 μΩ·cm or more, preferably 4.5 μΩ·cm or more.
また、本実施形態にかかる硬化物の貯蔵弾性率(E´)は、好適には1.0GPa以上、より好適には3.0GPa以上、さらに好適には5.0GPa以上である。これにより、硬化物の強度を向上させることができる。 The storage elastic modulus (E') of the cured product according to this embodiment is preferably 20 GPa or less, more preferably 17 GPa or less, and even more preferably 15 GPa or less. Thereby, the adhesion between the cured product and the adherend can be improved.
In addition, the storage elastic modulus (E') of the cured product according to this embodiment is preferably 1.0 GPa or higher, more preferably 3.0 GPa or higher, and even more preferably 5.0 GPa or higher. Thereby, the strength of the cured product can be improved.
本実施形態にかかるシンタリング促進剤は、銀含有粒子同士がシンタリングすることを促進するものであり、式(1)または式(2)で示される化合物を含む。
The sintering accelerator according to this embodiment promotes sintering between silver-containing particles, and includes a compound represented by formula (1) or formula (2).
本実施形態にかかるシンタリング促進方法は、上述のシンタリング促進剤を用いて銀含有粒子のシンタリングを促進する方法である。 [Method for Promoting Sintering]
The method for promoting sintering according to this embodiment is a method for promoting sintering of silver-containing particles using the sintering accelerator described above.
表1および3に示す配合に従い各成分を均一に混合することによりジェットディスペンス用導電性ペーストに配合するワニス1~11およびA1~A7を調製した。表1および3における各成分の含有量の単位は、質量部である。 [Preparation of conductive paste]
Varnishes 1 to 11 and A1 to A7 to be blended in the conductive paste for jet dispensing were prepared by uniformly mixing each component according to the formulations shown in Tables 1 and 3. The unit of content of each component in Tables 1 and 3 is parts by mass.
・シンタリング促進剤1:ポリエチレングリコールジグリシジルエーテル(製品名:エポライト400E、共栄社化学株式会社製、前述の式(1)に該当、m=9)
・シンタリング促進剤2:ポリエチレングリコールジグリシジルエーテル(製品名:デナコールEX-821、ナガセケムテックス株式会社製、前述の式(1)に該当、m=4)
・シンタリング促進剤3:ポリプロピレングリコールジグリシジルエーテル(製品名:デナコールEX-920、ナガセケムテックス株式会社製、前述の式(2)に該当、n=3)
・シンタリング促進剤4:ポリプロピレングリコールジグリシジルエーテル(製品名:デナコールEX-931、ナガセケムテックス株式会社製、前述の式(2)に該当、n=11)
・シンタリング促進剤5:ポリエチレングリコールジグリシジルエーテル(製品名:デナコールEX-830、ナガセケムテックス株式会社製、前述の式(1)に該当、n=9) (sintering accelerator)
Sintering accelerator 1: polyethylene glycol diglycidyl ether (product name: Epolite 400E, manufactured by Kyoeisha Chemical Co., Ltd., corresponding to the above formula (1), m = 9)
・ Sintering accelerator 2: polyethylene glycol diglycidyl ether (product name: Denacol EX-821, manufactured by Nagase ChemteX Corporation, corresponding to the above formula (1), m = 4)
・ Sintering accelerator 3: polypropylene glycol diglycidyl ether (product name: Denacol EX-920, manufactured by Nagase ChemteX Corporation, corresponds to the above formula (2), n = 3)
・ Sintering accelerator 4: polypropylene glycol diglycidyl ether (product name: Denacol EX-931, manufactured by Nagase ChemteX Corporation, corresponds to the above formula (2), n = 11)
・ Sintering accelerator 5: polyethylene glycol diglycidyl ether (product name: Denacol EX-830, manufactured by Nagase ChemteX Corporation, corresponds to the above formula (1), n = 9)
・エポキシモノマー1:トリメチロールプロパンポリグリシジルエーテル(製品名:デナコールEX-321L、ナガセケムテックス株式会社製)
・エポキシモノマー2:ビスフェノールF型エポキシモノマー(製品名:RE-303S、日本化薬株式会社製) (epoxy monomer)
・ Epoxy monomer 1: trimethylolpropane polyglycidyl ether (product name: Denacol EX-321L, manufactured by Nagase ChemteX Corporation)
・ Epoxy monomer 2: Bisphenol F type epoxy monomer (product name: RE-303S, manufactured by Nippon Kayaku Co., Ltd.)
・エポキシ基含有ブタジエンゴム1:エポキシ変性ポリブタジエン(製品名:NISSO-PB JP-200、日本曹達株式会社製) (epoxy group-containing butadiene rubber)
・ Epoxy group-containing butadiene rubber 1: epoxy-modified polybutadiene (product name: NISSO-PB JP-200, manufactured by Nippon Soda Co., Ltd.)
・(メタ)アクリルモノマー1:1,4-シクロヘキサンジメタノールモノアクリレート(製品名:CHDMMA、日本化成株式会社製)
・(メタ)アクリルモノマー2:エチレングリコールジメタクリレート(製品名:ライトエステルEG、共栄社化学株式会社製) ((meth)acrylic monomer)
・ (Meth) acrylic monomer 1: 1,4-cyclohexanedimethanol monoacrylate (product name: CHDMMA, manufactured by Nippon Kasei Co., Ltd.)
・ (Meth) acrylic monomer 2: ethylene glycol dimethacrylate (product name: Light Ester EG, manufactured by Kyoeisha Chemical Co., Ltd.)
・硬化剤1:ビスフェノールF型フェノール樹脂(製品名:DIC-BPF、DIC株式会社製) (curing agent)
・ Curing agent 1: Bisphenol F type phenolic resin (product name: DIC-BPF, manufactured by DIC Corporation)
・硬化促進剤1:2-フェニル-1H-イミダゾール-4,5-ジメタノール(製品名:2PHZ-PW、四国化成工業株式会社製) (Curing accelerator)
・ Curing accelerator 1: 2-phenyl-1H-imidazole-4,5-dimethanol (product name: 2PHZ-PW, manufactured by Shikoku Kasei Co., Ltd.)
・ラジカル重合開始剤1:ジクミルパーオキサイド(製品名:パーカドックスBC、化薬ヌーリオン株式会社製) (Radical polymerization initiator)
・ Radical polymerization initiator 1: dicumyl peroxide (product name: Perkadox BC, manufactured by Kayaku Noorion Co., Ltd.)
(銀含有粒子)
・銀フィラー1:銀粒子(製品名:AG-DSB-114、DOWAエレクトロニクス株式会社製、球状、D50:0.7μm、比表面積:1.05m2/g、タップ密度5.25g/cm3、円形度:0.953)
・銀フィラー2:銀粒子(製品名:HKD-12、福田金属箔粉工業株式会社製、鱗片状、D50:7.6μm、比表面積:0.315m2/g、タップ密度:5.5g/cm3)
(溶剤)
・溶剤1:トリプロピレングリコールモノn-ブチルエーテル(製品名:BFTG、日本乳化剤株式会社製) Details of the components shown in Tables 2 and 4 are as follows.
(Silver-containing particles)
・Silver filler 1: silver particles (product name: AG-DSB-114, manufactured by DOWA Electronics Co., Ltd., spherical, D 50 : 0.7 μm, specific surface area: 1.05 m 2 /g, tap density 5.25 g/cm 3 , Circularity: 0.953)
・Silver filler 2: Silver particles (product name: HKD-12, manufactured by Fukuda Metal Foil & Powder Co., Ltd., scale-like, D 50 : 7.6 μm, specific surface area: 0.315 m 2 /g, tap density: 5.5 g / cm3 )
(solvent)
・Solvent 1: Tripropylene glycol mono-n-butyl ether (product name: BFTG, manufactured by Nippon Nyukazai Co., Ltd.)
得られた導電性ペーストをガラス板上に塗布し、窒素雰囲気下で、30℃から200℃まで60分間かけて昇温し、続けて200℃で120分間焼結処理を行った。これにより、厚さ0.05mmの硬化物を得た。 [Preparation of cured product]
The resulting conductive paste was applied onto a glass plate, heated from 30° C. to 200° C. over 60 minutes in a nitrogen atmosphere, and then sintered at 200° C. for 120 minutes. Thereby, a cured product having a thickness of 0.05 mm was obtained.
ミリオームメータ(HIOKI社製)による直流四電極法により、電極間隔が40mmの電極を用い、得られた硬化物表面の体積抵抗率を測定した。 [Volume resistivity]
The volume resistivity of the surface of the obtained cured product was measured by a DC four-electrode method using a milliohmmeter (manufactured by Hioki) using electrodes with an electrode spacing of 40 mm.
得られた硬化物から約0.1mm×約10mm×約4mmの短冊状サンプルを切り出し、当該短冊状サンプルを用いて25℃における貯蔵弾性率(E’)を、DMA(動的粘弾性測定、引張モード)により昇温速度5℃/min、周波数10Hzの条件で測定した。 [Storage modulus]
A strip-shaped sample of about 0.1 mm x about 10 mm x about 4 mm was cut out from the obtained cured product, and the storage elastic modulus (E') at 25 ° C. was measured using the strip-shaped sample by DMA (dynamic viscoelasticity measurement, (tensile mode) at a temperature increase rate of 5° C./min and a frequency of 10 Hz.
得られた硬化物から約4mm×約10mm×約50μmのSEM観察用切片を切り出し、当該SEM観察用切片を走査電子顕微鏡(日立ハイテクノロジーズ社製、装置名:MiniscopeTM3030)により倍率:5000倍で観察した。 [SEM observation of cross section of cured product]
A section for SEM observation of about 4 mm×about 10 mm×about 50 μm is cut out from the obtained cured product, and the section for SEM observation is observed with a scanning electron microscope (manufactured by Hitachi High-Technologies Corporation, device name: MiniscopeTM3030) at a magnification of 5000. bottom.
20 半導体素子
30 基板
40 ボンディングワイヤ
50 モールド樹脂
60 半田ボール
100 半導体装置 10
Claims (15)
- 銀含有粒子と、
前記銀含有粒子同士がシンタリングすることを促進するシンタリング促進剤と、
を含有する導電性ペーストであって、
前記シンタリング促進剤が式(1)または式(2)で示される化合物を含む、導電性ペースト。
a sintering accelerator that promotes sintering between the silver-containing particles;
A conductive paste containing
A conductive paste, wherein the sintering accelerator contains a compound represented by formula (1) or (2).
- 請求項1に記載の導電性ペーストであって、
前記シンタリング促進剤が式(1)で示される化合物を含み、式(1)中、mは1以上11以下の整数である、導電性ペースト。 The conductive paste according to claim 1,
A conductive paste, wherein the sintering accelerator contains a compound represented by formula (1), wherein m is an integer of 1 or more and 11 or less. - 請求項1または2に記載の導電性ペーストであって、
前記シンタリング促進剤が式(2)で示される化合物を含み、式(2)中、nは2以上13以下の整数である、導電性ペースト。 The conductive paste according to claim 1 or 2,
A conductive paste, wherein the sintering accelerator contains a compound represented by formula (2), wherein n is an integer of 2 or more and 13 or less. - 請求項1~3のいずれかに記載の導電性ペーストであって、
前記銀含有粒子が球状粒子、鱗片状粒子、凝集状粒子、および多面体形状の粒子からなる群から選択される1種または2種以上を含む、導電性ペースト。 The conductive paste according to any one of claims 1 to 3,
A conductive paste, wherein the silver-containing particles include one or more selected from the group consisting of spherical particles, scale-like particles, aggregated particles, and polyhedral particles. - 請求項4に記載の導電性ペーストであって、
前記銀含有粒子が球状粒子、鱗片状粒子、凝集状粒子、および多面体形状の粒子からなる群から選択される2種以上を含む、導電性ペースト。 The conductive paste according to claim 4,
A conductive paste, wherein the silver-containing particles include two or more selected from the group consisting of spherical particles, scale-like particles, aggregated particles, and polyhedral particles. - 請求項1~5のいずれかに記載の導電性ペーストであって、
エポキシモノマーをさらに含む、導電性ペースト。 The conductive paste according to any one of claims 1 to 5,
A conductive paste further comprising an epoxy monomer. - 請求項6に記載の導電性ペーストであって、
フェノール系硬化剤をさらに含む、導電性ペースト。 The conductive paste according to claim 6,
A conductive paste further comprising a phenolic hardener. - 請求項6または7に記載の導電性ペーストであって、
イミダゾール系硬化促進剤をさらに含む、導電性ペースト。 The conductive paste according to claim 6 or 7,
An electrically conductive paste, further comprising an imidazole curing accelerator. - 請求項1~8のいずれかに記載の導電性ペーストであって、
(メタ)アクリルモノマーをさらに含む、導電性ペースト。 The conductive paste according to any one of claims 1 to 8,
An electrically conductive paste further comprising a (meth)acrylic monomer. - 請求項9に記載の導電性ペーストであって、
ラジカル重合開始剤をさらに含む、導電性ペースト。 The conductive paste according to claim 9,
A conductive paste, further comprising a radical polymerization initiator. - 請求項1~10のいずれかに記載の導電性ペーストであって、
溶剤をさらに含む、導電性ペースト。 The conductive paste according to any one of claims 1 to 10,
A conductive paste further comprising a solvent. - 請求項1~11のいずれかに記載の導電性ペーストであって、
当該導電性ペーストを、焼結処理後の厚みが0.05mmになるようにガラス板上に塗布し、窒素雰囲気下で、30℃から200℃まで60分間かけて昇温し、続けて200℃で120分間焼結処理し、硬化物を得た場合の、当該硬化物の体積抵抗率が4.0μΩ・cm以上9.5μΩ・cm以下である、導電性ペースト。 The conductive paste according to any one of claims 1 to 11,
The conductive paste was applied to a glass plate so that the thickness after sintering was 0.05 mm, and the temperature was raised from 30°C to 200°C over 60 minutes in a nitrogen atmosphere, and then to 200°C. is sintered for 120 minutes to obtain a cured product having a volume resistivity of 4.0 μΩ·cm or more and 9.5 μΩ·cm or less. - 請求項1~12のいずれかに記載の導電性ペーストを焼結して得られる硬化物。 A cured product obtained by sintering the conductive paste according to any one of claims 1 to 12.
- 銀含有粒子同士がシンタリングすることを促進するシンタリング促進剤であって、
式(1)または式(2)で示される化合物を含む、シンタリング促進剤。
A sintering accelerator containing a compound represented by formula (1) or (2).
- 請求項14に記載のシンタリング促進剤を用いて銀含有粒子のシンタリングを促進する、シンタリング促進方法。 A method for promoting sintering, comprising promoting sintering of silver-containing particles using the sintering accelerator according to claim 14.
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WO2012042780A1 (en) * | 2010-09-29 | 2012-04-05 | 横浜ゴム株式会社 | Electroconductive composition, solar battery cell, and method for producing solar battery cell |
JP2014146482A (en) * | 2013-01-28 | 2014-08-14 | Gunma Univ | Conductive paste |
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JPWO2023048098A1 (en) | 2023-03-30 |
KR20240058186A (en) | 2024-05-03 |
JP2023086762A (en) | 2023-06-22 |
JP7260079B1 (en) | 2023-04-18 |
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