WO2012118061A1 - Electrically conductive composition - Google Patents
Electrically conductive composition Download PDFInfo
- Publication number
- WO2012118061A1 WO2012118061A1 PCT/JP2012/054882 JP2012054882W WO2012118061A1 WO 2012118061 A1 WO2012118061 A1 WO 2012118061A1 JP 2012054882 W JP2012054882 W JP 2012054882W WO 2012118061 A1 WO2012118061 A1 WO 2012118061A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- silver
- conductive composition
- component
- particles
- coated
- Prior art date
Links
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- XFUOBHWPTSIEOV-UHFFFAOYSA-N bis(oxiran-2-ylmethyl) cyclohexane-1,2-dicarboxylate Chemical compound C1CCCC(C(=O)OCC2OC2)C1C(=O)OCC1CO1 XFUOBHWPTSIEOV-UHFFFAOYSA-N 0.000 description 1
- HGXHJQLDZPXEOG-UHFFFAOYSA-N bis(oxiran-2-ylmethyl) cyclohexane-1,4-dicarboxylate Chemical compound C1CC(C(=O)OCC2OC2)CCC1C(=O)OCC1CO1 HGXHJQLDZPXEOG-UHFFFAOYSA-N 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
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- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
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- OZEHOHQZIRILDX-UHFFFAOYSA-N ctk1b7797 Chemical compound O=C1OC(=O)C2C1C1(C)CC2CC1 OZEHOHQZIRILDX-UHFFFAOYSA-N 0.000 description 1
- SPTHWAJJMLCAQF-UHFFFAOYSA-M ctk4f8481 Chemical compound [O-]O.CC(C)C1=CC=CC=C1C(C)C SPTHWAJJMLCAQF-UHFFFAOYSA-M 0.000 description 1
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 1
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 description 1
- 150000005690 diesters Chemical class 0.000 description 1
- XXJWXESWEXIICW-UHFFFAOYSA-N diethylene glycol monoethyl ether Chemical compound CCOCCOCCO XXJWXESWEXIICW-UHFFFAOYSA-N 0.000 description 1
- 229940075557 diethylene glycol monoethyl ether Drugs 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- XHWQYYPUYFYELO-UHFFFAOYSA-N ditridecyl phosphite Chemical compound CCCCCCCCCCCCCOP([O-])OCCCCCCCCCCCCC XHWQYYPUYFYELO-UHFFFAOYSA-N 0.000 description 1
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- 239000003063 flame retardant Substances 0.000 description 1
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- VANNPISTIUFMLH-UHFFFAOYSA-N glutaric anhydride Chemical compound O=C1CCCC(=O)O1 VANNPISTIUFMLH-UHFFFAOYSA-N 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
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- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
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- 239000010410 layer Substances 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 229930007744 linalool Natural products 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
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- 239000011777 magnesium Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
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- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 description 1
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- 238000000465 moulding Methods 0.000 description 1
- JAYXSROKFZAHRQ-UHFFFAOYSA-N n,n-bis(oxiran-2-ylmethyl)aniline Chemical compound C1OC1CN(C=1C=CC=CC=1)CC1CO1 JAYXSROKFZAHRQ-UHFFFAOYSA-N 0.000 description 1
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
- NPFIXJIFUHTLRP-UHFFFAOYSA-N n-cyclohexyl-2-methylpropanamide Chemical compound CC(C)C(=O)NC1CCCCC1 NPFIXJIFUHTLRP-UHFFFAOYSA-N 0.000 description 1
- 125000001624 naphthyl group Chemical group 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- 239000004843 novolac epoxy resin Substances 0.000 description 1
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- 239000003208 petroleum Substances 0.000 description 1
- NAKOELLGRBLZOF-UHFFFAOYSA-N phenoxybenzene;pyrrole-2,5-dione Chemical compound O=C1NC(=O)C=C1.O=C1NC(=O)C=C1.C=1C=CC=CC=1OC1=CC=CC=C1 NAKOELLGRBLZOF-UHFFFAOYSA-N 0.000 description 1
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- 238000003756 stirring Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- RINCXYDBBGOEEQ-UHFFFAOYSA-N succinic anhydride Chemical group O=C1CCC(=O)O1 RINCXYDBBGOEEQ-UHFFFAOYSA-N 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
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- NMOALOSNPWTWRH-UHFFFAOYSA-N tert-butyl 7,7-dimethyloctaneperoxoate Chemical compound CC(C)(C)CCCCCC(=O)OOC(C)(C)C NMOALOSNPWTWRH-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
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- 239000011135 tin Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
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- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
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- 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
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L101/00—Compositions of unspecified macromolecular compounds
-
- 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
Definitions
- the present invention relates to a conductive composition useful as a circuit pattern formation or die bonding agent.
- conductive compositions are used as bonding materials for forming circuit patterns and bonding semiconductor elements such as ICs and LSIs to lead frames or substrates.
- the conductive circuit can be formed by applying a conductive composition on a substrate by screen printing or the like and then thermally curing the conductive composition.
- the bonding between the semiconductor element and the lead frame or the substrate can be performed by applying a conductive composition to a predetermined part of the lead frame or the substrate, mounting the semiconductor element, and thermally curing the semiconductor element.
- a conductive composition is one that develops conductivity by blending silver particles, but in recent years, while blending cheaper nickel particles and silver plating particles, it also has adhesiveness and conductivity.
- an electrically conductive composition that can provide a cured film.
- conductive compositions containing silver-coated particles have been proposed (see Patent Documents 1 to 3).
- the conductive composition of Patent Document 1 requires the use of an organometallic complex containing titanium and / or zirconium, and cannot sufficiently contribute to cost reduction.
- the conductive compositions of Patent Documents 2 and 3 use a thermoplastic resin such as a polyester resin having a molecular weight of 3000 or more and / or a modified polyester resin, and soften at a high temperature (260 ° C.). In addition, it becomes difficult to maintain reliability in reflow after moisture absorption.
- flake powder having an average particle size / thickness of 2 or more and a high degree of flaming when used for bonding a chip and a substrate, a plurality of flakes overlap to obtain vertical conduction, and consequently The contact resistance is high, and unlike silver, electricity passes through the periphery of the core material, so the conduction path is long, and the resistance value of vertical conduction is generally high. Furthermore, flake powder having a high average particle size / thickness of 2 or more and having a high degree of flaming has a large specific surface area. In order to uniformly coat with silver, it is necessary to increase the coating rate of silver, thus reducing the cost effectively. It will not be expected.
- This invention is made
- the conductive composition is a flaky silver having a specific shape selected from the group consisting of silver-coated ceramic particles, silver-coated glass particles, and silver-coated aluminum particles. It has been discovered that blending the coated particles results in a cured film that is sufficient in terms of adhesion and conductivity, thus completing the present invention. In the present invention, since relatively inexpensive silver-coated particles are used, the cost can be reduced at the same time.
- a volume average particle diameter D50 selected from the group consisting of silver-coated ceramic particles, silver-coated glass particles, and silver-coated aluminum particles and measured by a laser light scattering method is 1 to 10 ⁇ m, and a scanning electron microscope Flaky silver-coated particles having an average thickness T measured by observation of 0.3 to 10 ⁇ m and an aspect ratio T / D50 of 0.3 to 1.0
- B thermosetting resin
- C It relates to a conductive composition containing a curing agent.
- a conductive composition that satisfies both cost reduction and good adhesion and expression of conductivity.
- the conductive composition of the present invention is selected from the group consisting of (A) silver-coated ceramic particles, silver-coated glass particles, and silver-coated aluminum particles, and has a volume average particle diameter D50 measured by a laser light scattering method of 1 Including flaky silver-coated particles having an average thickness T measured by observation with a scanning electron microscope of 0.3 to 10 ⁇ m and an aspect ratio T / D50 of 0.3 to 1.0 .
- the flaky silver-coated particles of the component (A) may be used alone or in combination of two or more.
- the core of the flaky silver-coated particles of component (A) is made of ceramic, glass or aluminum.
- ceramics include alumina, silicon carbide, silicon nitride, barium titanate, boron nitride, ferrite, steatite, zinc oxide, and zirconia. Freedom to obtain, freedom to control particle size and shape, and cost In particular, alumina is preferable.
- the flaky silver-coated particles of the component have a volume average particle diameter D50 of 1 to 10 ⁇ m as measured by a laser light scattering method.
- D50 volume average particle diameter
- the workability of the conductive composition is good.
- the film thickness of the conductive composition is often set to 20 to 30 ⁇ m, but the film thickness increases due to the presence of the component (A) and the chip is tilted. This can also be avoided.
- D50 is a glass-coated particle with 2 cups of microspatella, taken in a 300 ml beaker, put 50 ml of 0.5% sodium sulfosuccinate dioctyl ester solution, and dispersed with an ultrasonic homogenizer for 10 minutes. (A Coulter LS230 (manufactured by Beckman Coulter)) The average value of 50% cumulative diameter is D50.
- D50 of the flaky silver-coated particles of the component (A) is 1 to 10 ⁇ m, preferably 3 to 8 ⁇ m.
- the flaky silver-coated particles of the component (A) have an average thickness T measured by observation with a scanning electron microscope of 0.3 to 10 ⁇ m.
- T is in this range, the workability of the conductive composition is good, and it is also possible to avoid the inconvenience that the chip is inclined due to the component (A) in joining the semiconductor chip and the substrate.
- the average thickness is 2 g of silver-coated particles, 5 g of epoxy resin (Epoxy Resin 20-8130-032 (manufactured by BUEHLER)) and 1 g of epoxy resin curing agent (EPOXY HARDENER 20-8132-008 (manufactured by BUEHLER)) in a 25 mm diameter clear cup.
- T of the flaky silver-coated particles of the component (A) is 0.3 to 10 ⁇ m, preferably 1 to 8 ⁇ m.
- the flaky silver-coated particles of the component have an aspect ratio T / D50 of 0.3 to 1.0.
- T / D50 aspect ratio of 0.3 to 1.0.
- the semiconductor chip and the substrate are more conductive than the one having a higher degree of fragmentation (that is, the T / D50 is less than 0.3).
- the number of silver-coated particles can be reduced, thereby making it possible to reduce the contact resistance between the silver-coated particles.
- the one with a high degree of fragmentation has a long conduction path because electricity passes around the core material, whereas the silver-coated fine particles of the present invention require a short conduction path, thereby reducing the resistance value of vertical conduction. Is possible.
- T / D50 is preferably 0.3 to 1.0, and more preferably 0.4 to 1.0.
- the flaky silver-coated particles of component (A) have a maximum particle size of 40 ⁇ m from the viewpoint of workability (especially suppression of nozzle clogging during dispensing) and prevention of tip tilting in bonding between the semiconductor chip and the substrate.
- the maximum particle size is a value measured with a light scattering analysis type particle size distribution measuring device.
- the maximum particle size is more preferably 35 ⁇ m or less, and further preferably 30 ⁇ m or less.
- the silver coating layer is preferably 10 to 60% by mass of the total weight of the silver-coated particles, more preferably, from the viewpoint of silver coverage on the core material and conductivity. Is 20 to 50% by mass, more preferably 20 to 40% by mass.
- the weight of the silver coating layer can be calculated from the weight of the silver coating particles and the core material measured by dissolving the silver coating layer in nitric acid and removing silver.
- the flaky silver-coated particles of the component (A) are preferably provided with a uniform silver coating layer, the silver coating layer is thick, and the specific gravity of the entire particle, and hence the specific gravity of the conductive composition, is increased.
- the thickness of the silver coating layer is preferably 50 to 300 nm from the viewpoint of avoiding a decrease in efficiency by reducing the volume when the conductive composition is applied with the same weight and obtaining stable conductivity. is there.
- the thickness of the silver coating layer is more preferably 50 to 200 nm, still more preferably 80 to 200 nm, and particularly preferably 80 to 150 nm.
- the thickness of the silver coating layer can be measured by preparing a sample having the same thickness as the average thickness T, and using a field emission scanning electron microscope (JSM-7500F manufactured by JEOL) at a magnification of 10,000 to 30,000 times.
- the flaky silver-coated particles of the component can be obtained by coating the ceramic, glass, and aluminum particles serving as the core with silver by a method such as electroless plating, sputtering, or vapor deposition.
- the flaky silver-coated particles of the component (A) are preferably those that have been surface-treated with a fatty acid, a salt thereof, or a coupling agent from the viewpoint of stability when formed into a paste.
- fatty acids examples include propionic acid, caprylic acid, lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, acrylic acid, oleic acid, linoleic acid, arachidonic acid, epoxy resin, phenolic resin, acrylate resin, From the viewpoint of compatibility with isocyanate resin and maleimide resin, wettability, and reactivity to resin, oleic acid and stearic acid are preferred.
- fatty acid salts include metal salts of the above fatty acids such as lithium, sodium, potassium, barium, magnesium, calcium, aluminum, iron, cobalt, manganese, lead, zinc, tin, strontium, zirconium, silver, copper, and epoxy. From the viewpoint of compatibility with resins, phenolic resins, acrylate resins, isocyanate resins, and maleimide resins, wettability, and reactivity to resins, sodium salts are preferred.
- Examples of the surface treatment method using a fatty acid or a fatty acid salt include a method in which the fatty acid or the fatty acid salt is dissolved in an optionally heated alcohol, and silver-coated particles are added thereto, followed by stirring for a certain time.
- Examples of coupling agents include silane coupling agents, titanate coupling agents, aluminum coupling agents, etc., compatibility with epoxy resins, phenol resins, acrylate resins, isocyanate resins, maleimide resins, wettability, resins From the viewpoint of reactivity to silane, a silane coupling agent and a titanate coupling agent are preferable.
- a surface treatment method using a coupling agent a method in which silver-coated particles are sprayed onto an agitator where the particles are being agitated, the coupling agent is dissolved in alcohol, and silver-coated particles are added thereto and stirred. There is a method of performing and processing.
- the conductive composition of the present invention contains (B) a thermosetting resin.
- a thermosetting resin of a component is not specifically limited, For example, an epoxy resin, an acrylic resin, a silicone resin, a urethane resin, a maleimide resin etc. are mentioned.
- a thermosetting resin may be individual or may use multiple types together.
- the thermosetting resin of component (B) is preferably an epoxy resin from the viewpoints of adhesiveness, curability and heat resistance required for the die bonding agent.
- the epoxy resin is preferably liquid at normal temperature, but even if it is solid at normal temperature, it can be diluted with another liquid epoxy resin or diluent and used in liquid form.
- Specific examples of epoxy resins include bisphenol A type epoxy resins, brominated bisphenol A type epoxy resins, bisphenol F type epoxy resins, biphenyl type epoxy resins, novolac type epoxy resins, alicyclic epoxy resins, and naphthalene type epoxy resins.
- Ether-based or polyether-based epoxy resins for example, polyoxypropylene-modified epoxy resins such as polyoxypropylene bisphenol A diglycidyl ether), oxirane ring-containing polybutadiene, diglycidyl esterified modified products of dimer acid with epichlorohydrin, epoxy groups A polybutadiene compound having a molecular weight, a silicone epoxy copolymer resin, an aminophenol type epoxy resin (for example, N, N-bis (2,3-epoxypropyl) -4- (2,3-epoxypropylene) Piruokishi) aniline), and the like.
- polyoxypropylene-modified epoxy resins such as polyoxypropylene bisphenol A diglycidyl ether
- oxirane ring-containing polybutadiene diglycidyl esterified modified products of dimer acid with epichlorohydrin
- epoxy groups A polybutadiene compound having a molecular weight a silicone epoxy copolymer resin
- the liquid epoxy resin includes a bisphenol A type epoxy resin having an average molecular weight of about 400 or less; a branched polyfunctional bisphenol A type epoxy resin such as p-glycidyloxyphenyldimethyltrisbisphenol A diglycidyl ether; Bisphenol F type epoxy resin; phenol novolak type epoxy resin having an average molecular weight of about 570 or less; vinyl (3,4-cyclohexene) dioxide, 3,4-epoxycyclohexylcarboxylic acid (3,4-epoxycyclohexyl) methyl, adipine Cycloaliphatic epoxies such as bis (3,4-epoxy-6-methylcyclohexylmethyl) acid, 2- (3,4-epoxycyclohexyl) 5,1-spiro (3,4-epoxycyclohexyl) -m-dioxane Resin; 3,3 ' Biphenyl type epoxy resin such as 5,5′-tetra
- An epoxy resin having a silicone skeleton such as 1,3-bis (3-glycidoxypropyl) -1,1,3,3-tetramethyldisiloxane can also be used.
- the epoxy resin can be used in combination with a solid or ultra-high viscosity epoxy resin at room temperature, and as such an epoxy resin, a high molecular weight bisphenol A type epoxy resin, a novolac epoxy resin, a tetrabromobisphenol A type epoxy resin. And dicyclopentadiene type epoxy resin, isocyanate-modified epoxy resin, fluorene type epoxy resin, biphenyl aralkyl epoxy resin and the like. These can be used in combination with an epoxy resin and / or a diluent that is liquid at room temperature to adjust fluidity.
- low-viscosity epoxy resins such as (poly) ethylene glycol diglycidyl ether, (poly) propylene glycol diglycidyl ether, butanediol glycidyl ether, neopentyl glycol diester Glycidyl ether, 1,4-cyclohexanedimethanol diglycidyl ether, 1,6-hexanediol diglycidyl ether, p-tert-butylphenylglycidyl ether, dicyclopentadiene dimethanol diglycidyl ether, glycidyl ether of trimethylolpropane Diglycidyl ether of polytetramethylene ether glycol, diglycidyl ether of dimer acid and diglycidyl ether of polypropylene glycol, glycerine jig Glycidyl ether,
- acrylic resins examples include neopentyl glycol dimethacrylate, 1,6-hexanediol dimethacrylate, 1,9-nonanediol dimethacrylate, 1,10-decanediol dimethacrylate, dimethylol-tricyclodecane dimethacrylate, and trimethylolpropane triacrylate.
- silicone resins include epoxy-modified polysiloxane, alicyclic epoxy-modified polysiloxane, carbinol-modified polysiloxane, carboxyl-modified polysiloxane, monoamine-modified polysiloxane, diamine-modified polysiloxane, hydrogen-modified polysiloxane, mercapto-modified polysiloxane, Examples include methacryl-modified polysiloxane and diol-modified polysiloxane.
- urethane resin examples include isocyanate resins, isocyanate resins whose isocyanate groups are blocked with ⁇ -caprolactam, epoxy-modified urethane resins, methacrylate-modified urethane resins, and acrylate-modified urethane resins.
- maleimide resins include bismaleimide resins (4,4′-diphenylmethane bismaleimide, m-phenylene bismaleimide, bisphenol A type diphenyl ether bismaleimide, 3,3′-dimethyl-5,5′-diethyl 4,4′-diphenylmethane).
- Bismaleimide 4-methyl-1,3-phenylenebismaleimide, 1,6-bismaleimide- (2,2,4-trimethyl) hexane), monomaleimide resin (N-phenylmaleimide, N-cyclohexylmaleimide, o- Methylphenylmaleimide, p-hydroxyphenylmaleimide, p-carboxyphenylmaleimide, N-dodecylmaleimide).
- the conductive composition of the present invention contains (C) a curing agent.
- curing agent can be suitably selected with a combination with a thermosetting resin, for example, a phenol resin, an amine compound, an acid anhydride, a peroxide, a metal complex, an azo compound etc. are mentioned.
- curing agent may be individual or may use multiple types together.
- phenol resin examples include bisphenol F type phenol resin, allyl phenol resin, phenol novolac resin, cresol novolac resin, naphthol modified phenol resin, dicyclopentadiene modified phenol resin, p-xylene modified phenol resin and the like.
- amine compounds include aliphatic polyamines, aromatic amines, modified polyamines (eg, polyaminoamides, polyaminoimides, polyaminoesters, polyaminoureas, polyether-modified amines), tertiary amine compounds, and imidazole compounds (eg, 2 -Methylimidazole, 2-phenylimidazole, 2-phenyl-4-methylimidazole, 2-phenyl-4-methyl-5-hydroxymethylimidazole, 2-undecylimidazole, 2-heptadecylimidazole, 2,2-diamino- 6- [2′-methylimidazolyl- (1 ′)]-ethyl-s-triazine, etc.), hydrazide compounds, dicyanamide compounds, melamine compounds and the like.
- modified polyamines eg, polyaminoamides, polyaminoimides, polyaminoesters, polyaminoureas, poly
- acid anhydrides include methyltetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, alkylated tetrahydrophthalic anhydride, hexahydrophthalic anhydride, methylheimic acid anhydride, and alkenyl-substituted succinic acid.
- acid anhydride methyl nadic acid anhydride, glutaric acid anhydride and the like.
- 2,4-diethylpentanedioic anhydride 3,4-dimethyl-6- (2-methyl-1-propenyl) -1,2,3,6-tetrahydrophthalic anhydride
- Peroxides include 1,1,3,3-tetramethylbutylperoxy 2-ethylhexanate, t-butylperoxybenzoate, t-butylperoxyneodecanoate, cumylperoxyneodecanoate, 1,1,3,3-tetramethylbutylperoxyneodecanoate, t-butylperoxybenzoate, dicumyl peroxide, di-t-butyl peroxide, di-t-hexyl peroxide, di (2- t-butylperoxyisopropyl) benzene, 2,2-di (4,4-di- (butylperoxy) cyclohexyl) propane, p-menthane hydroperoxide, diisopropylbenzene hydroperoxide, 1,1,3,3 -Tetramethylbutyl hydroperoxide, cumene hydroperoxide, Examples include 1,1-di (t-butylperoxy) cycl
- metal complex examples include alkyl acetoacetate aluminum diisopropylate, aluminum tris (acetylacetonate), aluminum acrylate, aluminum bisethylacetoacetate diisopropylate, and magnesium 2-ethylhexanoate.
- conductive particles other than the component (A) may be blended.
- the total amount of the conductive particles other than the component (A) is preferably 50% by mass or less, more preferably 30% in total in all the conductive particles (the silver-coated particles of the component (A) and the conductive particles other than the component (A)). Most preferably, only the silver-coated particles of component (A) are used as the conductive particles.
- spherical silver-coated ceramic particles, silver-coated glass particles, and silver-coated aluminum particles can be used as the conductive particles.
- the core of the spherical silver-coated particles is preferably made of ceramic, glass or aluminum.
- Ceramics include alumina, silicon carbide, silicon nitride, barium titanate, boron nitride, ferrite, steatite, zinc oxide, and zirconia. Freedom to obtain, freedom to control particle size and shape, and cost From this point, alumina is particularly preferable.
- the spherical silver-coated particles preferably have a volume average particle diameter D50 measured by a laser light scattering method of 1 to 20 ⁇ m, more preferably 2 to 15 ⁇ m.
- the spherical silver-coated particles are preferably 10 to 50% by mass, more preferably, of the total weight of the silver-coated particles having a spherical silver coating layer, from the viewpoint of silver coverage on the core material and conductivity.
- Spherical silver-coated particles preferably have a uniform silver coating layer, and the thickness of the silver coating layer increases, and the specific gravity of the entire particle, and hence the specific gravity of the conductive composition, increases.
- the thickness is preferably 50 to 300 nm from the viewpoint of avoiding a decrease in efficiency due to a decrease in volume when an object is coated with the same weight and obtaining stable conductivity.
- the thickness of the silver coating layer is more preferably 50 to 200 nm, still more preferably 70 to 150 nm.
- conductive particles other than the component (A) silver particles, copper particles, nickel particles, palladium particles, indium particles, tin particles, zinc particles, bismuth particles, or alloys thereof can also be used.
- the shape is not particularly limited.
- a solvent may be added to the conductive composition of the present invention.
- the solvent is not particularly limited, and examples thereof include alcohol solvents such as ethylene glycol, propylene glycol, dihydroterpineol; toluene, xylene, ethylbenzene, diethylbenzene, isopropylbenzene, amylbenzene, p-cymene, tetralin, and petroleum aromatic hydrocarbons.
- Aromatic hydrocarbon solvents such as mixtures; terpene alcohols such as terpineol, linalool, geraniol, citronellol; ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, propylene glycol monomethyl ether, propylene glycol monoethyl ether, propylene glycol mono-n- Butyl ether, propylene glycol mono-tert-butyl ether, diethylene glycol monoethyl ether, die Ether alcohol solvents such as ethylene glycol monobutyl ether, dipropylene glycol monomethyl ether, dipropylene glycol monobutyl ether, tripropylene glycol monomethyl ether; ketone solvents such as methyl isobutyl ketone; and ethylene glycol monomethyl ether acetate, ethylene glycol monoethyl ether Examples thereof include ester solvents such as acetate, ethylene glycol monobutyl ether a
- the conductive composition of the present invention includes an inorganic filler (for example, fumed silica, calcium carbonate, talc, etc.) and a coupling agent (for example, ⁇ -glycol) within the range that does not impair the predetermined effects of the present invention.
- an inorganic filler for example, fumed silica, calcium carbonate, talc, etc.
- a coupling agent for example, ⁇ -glycol
- Silane coupling agents such as Sidoxypropyltrimethoxysilane, Titanate coupling agents such as Tetraoctylbis (ditridecylphosphite) titanate), Silane monomers (eg, tris (3- (trimethoxysilyl) propyl) isocyanurate ), Plasticizer (for example, copolymer such as carboxyl group-terminated polybutadiene-acrylonitrile, silicone rubber, silicone rubber powder, silicone resin powder, resin powder such as acrylic resin powder), flame retardant, antioxidant, antifoaming agent, etc. can do.
- Plasticizer for example, copolymer such as carboxyl group-terminated polybutadiene-acrylonitrile, silicone rubber, silicone rubber powder, silicone resin powder, resin powder such as acrylic resin powder
- flame retardant antioxidant, antifoaming agent, etc.
- the conductive composition of the present invention is composed of (A) component, (B) component and (C) component, and optionally optional components such as a solvent, for example, using a three roll, planetary mixer, or likai machine.
- a paste-like conductive composition can be produced.
- the order which mixes said each component is arbitrary, may be mixed simultaneously and may be mixed sequentially.
- a cured film can be formed by heating and thermosetting.
- Application method is not particularly limited, and examples thereof include dispensing, jet dispensing, stencil printing, screen printing, pin transfer, and stamping.
- the heating temperature can be, for example, 120 to 200 ° C., more preferably 150 to 175 ° C., and the heating time can be, for example, 1 to 120 hours, preferably 30 to 60 hours. is there.
- a conductive circuit can be formed by applying the conductive composition of the present invention on a substrate (for example, a ceramic substrate such as LTCC or a glass / epoxy substrate) and then thermally curing it.
- the conductive composition of the present invention can also be used as a die bonding agent.
- a die bonding agent made of the conductive composition of the present invention to a predetermined part of a lead frame or a substrate (for example, Bare Cu lead frame, Ag plated Cu lead frame, PPF, Ag plated 42 alloy frame).
- the semiconductor element can be mounted and thermally cured to bond the lead frame or the substrate and the semiconductor element.
- the cured film thus obtained exhibits sufficient conductivity (for example, a specific resistance value of 1 ⁇ 10 ⁇ 2 ⁇ ⁇ cm or less). Moreover, the adhesiveness (adhesion strength, adhesion resistance value) between the substrates is also good.
- each conductive composition of the examples and comparative examples is made on an alumina substrate (120 mm ⁇ 20 mm, thickness 1.6 mm) using a stainless mask (200 mesh, resist 20 ⁇ m) so as to have a pattern as shown in FIG.
- the object was screen printed. Next, it heated for 30 minutes with the ventilation drying machine hold
- the resistance value X ( ⁇ ) at both ends of the cured film of the sample was measured using a 4261ALCR meter (manufactured by YHP).
- the thickness Z ( ⁇ m) of the cured film 2 of the conductive composition on the alumina substrate 1 was measured using a surface roughness profile measuring machine Surfcom 590A (surface roughness profile measuring machine manufactured by Tokyo Seimitsu Co., Ltd.) (FIG. 1 ⁇ 2).
- An AgPd electrode 3216 type capacitor component (capacitor electrode 6) is mounted so as to be in contact with the conductive composition 5 (FIG. 2-3), and a load of 1.0 ⁇ 0.5 N is applied evenly to the component.
- a sample was obtained.
- the conductive composition was cured under predetermined curing conditions (heated to 150 ° C. in 30 minutes and held at 150 ° C. for 30 minutes).
- the resistance value between the upper part of the capacitor electrode 6 of the sample and the conductor (substrate electrode) within 1 mm from the coated part of the conductive composition 5 was measured by a four-terminal method (see FIG. 2-4).
- the measured current value of the current source was 10 ⁇ 0.5 mA.
- the average value was calculated from the measured values of 8 samples and used as the value of contact resistance.
- Each conductive composition was screen-printed on a Bare Cu lead frame using a screen mask capable of forming 10 patterns of 1.5 mm ⁇ ⁇ 40 ⁇ mt.
- Ten 2 mm square silicon chips were mounted so that the silicon surface was in contact with the conductive composition.
- curing was performed under predetermined curing conditions (heating to 150 ° C. in 30 minutes and holding at 150 ° C. for 30 minutes).
- the obtained sample was struck from the side surface using a strength tester MODEL-1605HTP (manufactured by Aiko Engineering Co., Ltd.), and the numerical value when the silicon chip was peeled was read.
- the measurement was performed at a normal speed (25 ⁇ 5 ° C.) at a test speed of 12 ⁇ 1 mm / min when protruding from the side.
- Viscosity change rate (%) (V2 ⁇ V1) / V1 ⁇ 100
- D50 is 2 cups of silver-coated particles in a microspatella, taken in a 300 ml beaker, put 50 ml of a 0.5% sodium sulfosuccinate dioctyl ester solution, dispersed for 10 minutes with an ultrasonic homogenizer, and a light scattering analysis type particle size distribution analyzer. (A Coulter LS230 (manufactured by Beckman Coulter)) The average value of 50% cumulative diameter is D50.
- Weight of silver coating layer It is a value calculated from the weight of the silver-coated particles and the core material measured by dissolving the silver-coated layer in nitric acid and removing silver.
- Thickness of silver coating layer This is a value obtained by preparing a sample similar to the average thickness T and measuring it with a field emission scanning electron microscope (JEOL JSM-7500F) at a magnification of 10,000 to 30,000 times.
- Resin 1 Bisphenol F type epoxy resin Bisphenol F type epoxy resin (epoxy equivalent: 160 to 175)
- Resin 2 Aminophenol type epoxy resin N, N-bis (2,3-epoxypropyl) -4- (2,3-epoxypropyloxy) aniline resin 3: PO modified epoxy resin Polyoxypropylene bisphenol A diglycidyl ether ( Epoxy equivalent 250-270)
- Filler 1 Fumed silica Polydimethylsiloxane-treated fumed silica Volume-based average particle size: 0.25 ⁇ m
- FIG. 3-1 is a SEM photograph of the silver-coated particles 1 at a magnification of 5000 times
- FIG. 3-2 is a graph illustrating the measurement of the average thickness.
- the silver-coated particles 1 were mixed with a water-soluble epoxy resin and cured. It is a SEM photograph of the section of hardened material.
- Examples 1 to 6 using the flaky silver-coated particles of the present invention all had small specific resistance values and contact resistance values, and were excellent in adhesive strength.
- Examples 3 to 6 using silver particles treated with oleic acid had little change in viscosity and were excellent in the stability of the conductive composition.
- Comparative Example 1 using silver-coated particles having a small aspect ratio was inferior in specific resistance value and contact resistance value.
- Examples 7 to 9 in Table 2 even if the thermosetting resin system is changed, the flaky silver-coated particles of the present invention are effective, and even if the amount of silver-coated particles is changed, the flakes of the present invention are effective. It can be seen that the silver-coated particles are effective.
- the silver-coated particles of the (A) component are based on 100 parts by mass in total of the conductive composition ((A) component, (B) component and (C) component).
- the adhesive strength was slightly inferior.
- the specific resistance value and the contact resistance value are small even when the silver coating layer of the component (A) is 50 to 60% by mass of the total weight of the silver-coated particles.
- the adhesive strength was also excellent.
- Example 15 when spherical silver-coated particles having an aspect ratio T / D50 of 1.0 were used, a tendency to be slightly inferior in terms of contact resistance was observed.
- a conductive composition that satisfies both cost reduction and good adhesion and expression of conductivity.
- the conductive composition of the present invention is useful as a conductive circuit formation and die bonding agent.
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Abstract
Description
(A)銀被覆セラミック粒子、銀被覆ガラス粒子及び銀被覆アルミニウム粒子からなる群より選択され、かつ、レーザ光散乱法により測定した体積平均粒子径D50が、1~10μmであり、走査型電子顕微鏡観察により測定した平均厚みTが、0.3~10μmであり、アスペクト比T/D50が、0.3~1.0であるフレーク状の銀被覆粒子
(B)熱硬化性樹脂、並びに
(C)硬化剤
を含む、導電性組成物に関する。 That is, the present invention
(A) A volume average particle diameter D50 selected from the group consisting of silver-coated ceramic particles, silver-coated glass particles, and silver-coated aluminum particles and measured by a laser light scattering method is 1 to 10 μm, and a scanning electron microscope Flaky silver-coated particles having an average thickness T measured by observation of 0.3 to 10 μm and an aspect ratio T / D50 of 0.3 to 1.0 (B) thermosetting resin, and (C ) It relates to a conductive composition containing a curing agent.
マレイミド樹脂としては、ビスマレイミド樹脂(4,4’-ジフェニルメタンビスマレイミド、m-フェニレンビスマレイミド、ビスフェノールA型ジフェニルエーテルビスマレイミド、3,3’-ジメチル-5,5’-ジエチル4,4’-ジフェニルメタンビスマレイミド、4-メチル-1,3-フェニレンビスマレイミド、1,6-ビスマレイミド-(2,2,4-トリメチル)ヘキサン)、モノマレイミド樹脂(N-フェニルマレイミド、N-シクロヘキシルマレイミド、o-メチルフェニルマレイミド、p-ヒドロキシフェニルマレイミド、p-カルボキシフェニルマレイミド、N-ドデシルマレイミド)が挙げられる。 Examples of the urethane resin include isocyanate resins, isocyanate resins whose isocyanate groups are blocked with ε-caprolactam, epoxy-modified urethane resins, methacrylate-modified urethane resins, and acrylate-modified urethane resins.
Examples of maleimide resins include bismaleimide resins (4,4′-diphenylmethane bismaleimide, m-phenylene bismaleimide, bisphenol A type diphenyl ether bismaleimide, 3,3′-dimethyl-5,5′-
〔比抵抗の測定〕
アルミナ基板(120mm×20mm、厚み1.6mm)に、図1-1のようなパターンになるように、ステンレスマスク(200メッシュ、レジスト20μm)を用いて、実施例・比較例の各導電性組成物をスクリーン印刷した。次に、150℃±5℃に保持された送風乾燥機で30分間加熱して、硬化膜を形成した試料を得た。試料の硬化膜の両端の抵抗値X(Ω)を、4261ALCRメーター(YHP社製)を用いて測定した。
アルミナ基板1上の導電性組成物の硬化膜2の厚みZ(μm)を、表面粗さ形状測定機サーフコム590A(東京精密社製 表面粗さ形状測定機)を用いて測定した(図1-2参照)。
比抵抗値ρ(Ω・cm)を、次式により算出した。
ρ = (0.1/7.1)×X×Z×10-4 (Ω・cm)
試料2個の測定値から平均値を算出し、比抵抗の値とした。 The characteristics of each conductive composition of Examples and Comparative Examples were measured. The results are shown in Tables 1 and 2.
[Measurement of resistivity]
Each conductive composition of the examples and comparative examples is made on an alumina substrate (120 mm × 20 mm, thickness 1.6 mm) using a stainless mask (200 mesh, resist 20 μm) so as to have a pattern as shown in FIG. The object was screen printed. Next, it heated for 30 minutes with the ventilation drying machine hold | maintained at 150 degreeC +/- 5 degreeC, and the sample which formed the cured film was obtained. The resistance value X (Ω) at both ends of the cured film of the sample was measured using a 4261ALCR meter (manufactured by YHP).
The thickness Z (μm) of the cured
The specific resistance value ρ (Ω · cm) was calculated by the following equation.
ρ = (0.1 / 7.1) × X × Z × 10 −4 (Ω · cm)
The average value was calculated from the measured values of the two samples, and used as the specific resistance value.
メタルマスク(厚さ:70μm)を用いて、膜厚:7~15μmのAg厚膜電極3を備えた25.4±0.1mm□のアルミナ基板4上(図2-1参照)に、図2-2のようなパターンになるように、メタルマスク(厚さ70μm)を用いて、実施例・比較例の各導電性組成物5をスクリーン印刷した。スクリーン印刷は、メタルスキージ(スキージ圧力100kPa、スキージ20mm/s、基板-マスク間ギャップ0mm、スキージ角度60°、版離れ速度0.05mm/s)を使用して行った。
導電性組成物5に接触するようにして、AgPd電極の3216型コンデンサ部品(コンデンサ電極6)を搭載し(図2-3)、部品に均等に1.0±0.5Nの荷重を加えて、試料を得た。
恒温槽にて、所定の硬化条件(150℃へ30分で昇温させ、150℃で30分保持)で導電性組成物を硬化させた。
試料のコンデンサ電極6上部と導電性組成物5の塗布部より周囲1mm以内の導体(基板電極)間の抵抗値を4端子法にて測定した(図2-4参照)。電流源の測定電流値は10±0.5mAとした。
試料8個の測定値から平均値を算出し、接触抵抗の値とした。 [Contact resistance value]
Using a metal mask (thickness: 70 μm) on the 25.4 ± 0.1 mm square alumina substrate 4 (see FIG. 2-1) with the Ag
An AgPd electrode 3216 type capacitor component (capacitor electrode 6) is mounted so as to be in contact with the conductive composition 5 (FIG. 2-3), and a load of 1.0 ± 0.5 N is applied evenly to the component. A sample was obtained.
In a thermostatic bath, the conductive composition was cured under predetermined curing conditions (heated to 150 ° C. in 30 minutes and held at 150 ° C. for 30 minutes).
The resistance value between the upper part of the
The average value was calculated from the measured values of 8 samples and used as the value of contact resistance.
1.5mm□×40μmtとなるパターンを、10個形成できるスクリーンマスクを用いて、各導電性組成物をBare Cuリードフレームにスクリーン印刷した。
2mm□シリコンチップをシリコン面が導電性組成物に接触するようにして、10個マウントした。
恒温槽にて、所定の硬化条件(150℃へ30分で昇温させ、150℃で30分保持)で硬化させた。
得られた試料を、強度試験機 MODEL-1605HTP(アイコーエンジニアリング社製)を用いて側面から突き、シリコンチップが剥がれた時の数値を読み取った。測定は、側面から突く際のテストスピード12±1mm/分、常温(25±5℃)で行った。 (Measurement of adhesive strength)
Each conductive composition was screen-printed on a Bare Cu lead frame using a screen mask capable of forming 10 patterns of 1.5 mm □ × 40 μmt.
Ten 2 mm square silicon chips were mounted so that the silicon surface was in contact with the conductive composition.
In a thermostatic bath, curing was performed under predetermined curing conditions (heating to 150 ° C. in 30 minutes and holding at 150 ° C. for 30 minutes).
The obtained sample was struck from the side surface using a strength tester MODEL-1605HTP (manufactured by Aiko Engineering Co., Ltd.), and the numerical value when the silicon chip was peeled was read. The measurement was performed at a normal speed (25 ± 5 ° C.) at a test speed of 12 ± 1 mm / min when protruding from the side.
E型粘度計 TVE-22Hを用い、ローター 3°コーンR9.7 を用いた。
実施例・比較例の各導電性組成物を、テルモ社製シリンジを用いて0.3ml吸い上げ、粘度計のカップの中心部に塗布した。カップを粘度計に装着し、恒温槽を用いて25℃に保ち、10分間放置した。0.5rpmで3分後の粘度を測定した(V1)。
実施例・比較例の各導電性組成物をシリンジに充填後、25℃、湿度50%の環境下、24時間放置した。各導電性組成物をシリンジを用いて0.3ml吸い上げ、粘度計のカップの中心部に塗布した。カップを粘度計に装着し、恒温槽を用いて25℃に保ち、10分間放置した。0.5rpmで3分後の粘度を測定した(V2)。
粘度の変化率を、次式により算出した。
粘度変化率(%)=(V2-V1)/V1×100 [Viscosity change]
An E-type viscometer TVE-22H was used, and a
Each conductive composition of Examples and Comparative Examples was sucked up by 0.3 ml using a Terumo syringe and applied to the center of the cup of the viscometer. The cup was attached to a viscometer, kept at 25 ° C. using a thermostatic bath, and allowed to stand for 10 minutes. The viscosity after 3 minutes at 0.5 rpm was measured (V1).
Each conductive composition of Examples and Comparative Examples was filled in a syringe and then left for 24 hours in an environment of 25 ° C. and 50% humidity. 0.3 ml of each conductive composition was sucked up using a syringe and applied to the center of the viscometer cup. The cup was attached to a viscometer, kept at 25 ° C. using a thermostatic bath, and allowed to stand for 10 minutes. The viscosity after 3 minutes at 0.5 rpm was measured (V2).
The rate of change in viscosity was calculated by the following formula.
Viscosity change rate (%) = (V2−V1) / V1 × 100
D50は、銀被覆粒子をミクロスパテラで2杯、300mlビーカーに採り、0.5%スルホコハク酸ナトリウムのジオクチルエステル溶液を50ml入れ、超音波ホモジナイザーで10分間分散し、光散乱解析タイプ粒度分布測定装置(コールターLS230(ベックマンコールター製)で測定することができる。50%の累積径の平均値をD50とする。 [Measurement of D50]
D50 is 2 cups of silver-coated particles in a microspatella, taken in a 300 ml beaker, put 50 ml of a 0.5% sodium sulfosuccinate dioctyl ester solution, dispersed for 10 minutes with an ultrasonic homogenizer, and a light scattering analysis type particle size distribution analyzer. (A Coulter LS230 (manufactured by Beckman Coulter)) The average value of 50% cumulative diameter is D50.
平均厚みは、銀被覆粒子2gとエポキシ樹脂(Epoxy Resin20-8130-032(BUEHLER製))5gとエポキシ樹脂硬化剤(EPOXY HARDENER20-8132-008(BUEHLER製))1gを直径25mmのクリアカップに計り取り、ヘラを用いてよく混合し、室温で12時間静置後、硬化した樹脂を、クリアカップより取り出し、ミクロトームで面出し加工を行い、カーボン蒸着後、電界放射型走査型電子顕微鏡(JEOL製JSM-7500F)で1000倍又は2000倍の倍率で写真を撮影し、中心を通る最短辺を銀被覆の厚みとして測定し、測定個数50個の平均値を平均厚みTとする。 [Measurement of average thickness T]
The average thickness is 2 g of silver-coated particles, 5 g of epoxy resin (Epoxy Resin 20-8130-032 (manufactured by BUEHLER)) and 1 g of epoxy resin curing agent (EPOXY HARDENER 20-8132-008 (manufactured by BUEHLER)) in a 25 mm diameter clear cup. Take out and mix well using a spatula, let stand at room temperature for 12 hours, then remove the cured resin from the clear cup, perform surface processing with a microtome, and after carbon deposition, a field emission scanning electron microscope (manufactured by JEOL) JSM-7500F) is photographed at a magnification of 1000 times or 2000 times, the shortest side passing through the center is measured as the thickness of the silver coating, and the average value of 50 measured pieces is defined as the average thickness T.
銀被覆粒子の重量と、銀被覆層を硝酸に溶解させて、銀を除き、測定したコア材の重量から算出した値である。 [Weight of silver coating layer]
It is a value calculated from the weight of the silver-coated particles and the core material measured by dissolving the silver-coated layer in nitric acid and removing silver.
平均厚みTと同様なサンプルを作製し、電界放射型走査型電子顕微鏡(JEOL製JSM-7500F)で10000倍~30000倍の倍率で測定して求めた値である。 [Thickness of silver coating layer]
This is a value obtained by preparing a sample similar to the average thickness T and measuring it with a field emission scanning electron microscope (JEOL JSM-7500F) at a magnification of 10,000 to 30,000 times.
樹脂1:ビスフェノールF型エポキシ樹脂
ビスフェノールF型エポキシ樹脂(エポキシ当量:160~175)
樹脂2:アミノフェノール型エポキシ樹脂
N,N-ビス(2,3-エポキシプロピル)-4-(2,3-エポキシプロピルオキシ)アニリン
樹脂3:PO変性エポキシ樹脂
ポリオキシプロピレンビスフェノールAジグリシジルエーテル(エポキシ当量250~270)
樹脂4:ビスマレイミド樹脂
1,6-ビスマレイミド-(2,2,4-トリメチル)ヘキサン
硬化剤1:ポリオキシプロピレンジアミン
H2N-SH(CH3)CH2[OCH2CH(CH3)]xNH2
x=33.1、活性水素当量:514
フィラー1:ヒュームドシリカ
ポリジメチルシロキサン処理ヒュームドシリカ
体積基準平均粒径:0.25μm The resins, curing agents and other components in Tables 1 and 2 are as follows.
Resin 1: Bisphenol F type epoxy resin Bisphenol F type epoxy resin (epoxy equivalent: 160 to 175)
Resin 2: Aminophenol type epoxy resin N, N-bis (2,3-epoxypropyl) -4- (2,3-epoxypropyloxy) aniline resin 3: PO modified epoxy resin Polyoxypropylene bisphenol A diglycidyl ether ( Epoxy equivalent 250-270)
Resin 4:
x = 33.1, active hydrogen equivalent: 514
Filler 1: Fumed silica Polydimethylsiloxane-treated fumed silica Volume-based average particle size: 0.25 μm
一方、アスペクト比が小さい銀被覆粒子を使用した比較例1は、比抵抗値、接触抵抗値に劣っていた。
表2の実施例7~9より、熱硬化性樹脂系を変更しても、本発明のフレーク状の銀被覆粒子が有効であり、銀被覆粒子の量を変更しても、本発明のフレーク状の銀被覆粒子が有効であることがわかる。また、表2の実施例10及び11により、(A)成分の銀被覆粒子が、導電性組成物((A)成分、(B)成分及び(C)成分)の合計100質量部に対して、75質量部含まれると、若干接着強度が劣る傾向が見られた。また、表2の実施例14及び15により、(A)成分の銀被覆層が銀被覆粒子の全重量のうち、50~60質量%の場合においても、比抵抗値及び接触抵抗値が小さく、接着強度にも優れていた。実施例15により、アスペクト比T/D50が1.0の球状の銀被覆粒子を使用した場合には、接触抵抗の点で若干劣る傾向が見られた。 From Table 1, Examples 1 to 6 using the flaky silver-coated particles of the present invention all had small specific resistance values and contact resistance values, and were excellent in adhesive strength. In particular, Examples 3 to 6 using silver particles treated with oleic acid had little change in viscosity and were excellent in the stability of the conductive composition.
On the other hand, Comparative Example 1 using silver-coated particles having a small aspect ratio was inferior in specific resistance value and contact resistance value.
From Examples 7 to 9 in Table 2, even if the thermosetting resin system is changed, the flaky silver-coated particles of the present invention are effective, and even if the amount of silver-coated particles is changed, the flakes of the present invention are effective. It can be seen that the silver-coated particles are effective. Moreover, according to Examples 10 and 11 in Table 2, the silver-coated particles of the (A) component are based on 100 parts by mass in total of the conductive composition ((A) component, (B) component and (C) component). When 75 parts by mass was contained, the adhesive strength was slightly inferior. Further, according to Examples 14 and 15 in Table 2, the specific resistance value and the contact resistance value are small even when the silver coating layer of the component (A) is 50 to 60% by mass of the total weight of the silver-coated particles. The adhesive strength was also excellent. According to Example 15, when spherical silver-coated particles having an aspect ratio T / D50 of 1.0 were used, a tendency to be slightly inferior in terms of contact resistance was observed.
Claims (9)
- (A)銀被覆セラミック粒子、銀被覆ガラス粒子及び銀被覆アルミニウム粒子からなる群より選択され、かつ、レーザ光散乱法により測定した体積平均粒子径D50が、1~10μmであり、走査型電子顕微鏡観察により測定した平均厚みTが、0.3~10μmであり、アスペクト比T/D50が、0.3~1.0であるフレーク状の銀被覆粒子、
(B)熱硬化性樹脂、並びに
(C)硬化剤
を含む、導電性組成物。 (A) A volume average particle diameter D50 selected from the group consisting of silver-coated ceramic particles, silver-coated glass particles, and silver-coated aluminum particles and measured by a laser light scattering method is 1 to 10 μm, and a scanning electron microscope Flaky silver-coated particles having an average thickness T measured by observation of 0.3 to 10 μm and an aspect ratio T / D50 of 0.3 to 1.0;
(B) A thermosetting resin, and (C) a conductive composition containing a curing agent. - (A)成分中の銀被覆層の重量が10~60質量%である、請求項1記載の導電性組成物。 The conductive composition according to claim 1, wherein the weight of the silver coating layer in the component (A) is 10 to 60% by mass.
- (A)成分が、脂肪酸若しくはその塩、又はカップリング剤で表面処理された銀被覆粒子である、請求項1又は2記載の導電性組成物。 The conductive composition according to claim 1 or 2, wherein the component (A) is a silver-coated particle surface-treated with a fatty acid or a salt thereof, or a coupling agent.
- (A)成分が、オレイン酸、ステアリン酸及びシランカップリング剤からなる群より選択される1種以上で表面処理された銀被覆粒子である、請求項3記載の導電性組成物。 The conductive composition according to claim 3, wherein the component (A) is silver-coated particles surface-treated with one or more selected from the group consisting of oleic acid, stearic acid, and silane coupling agents.
- (A)成分、(B)成分及び(C)成分の合計を100質量部とした場合、(A)成分が40~80質量部であり、(B)成分が10~58質量部であり、(C)成分が2~10質量部である、請求項1~4のいずれか1項記載の導電性組成物。 When the total of component (A), component (B) and component (C) is 100 parts by mass, component (A) is 40 to 80 parts by mass, component (B) is 10 to 58 parts by mass, The conductive composition according to any one of claims 1 to 4, wherein the component (C) is 2 to 10 parts by mass.
- さらに、球状の銀被覆セラミック粒子、銀被覆ガラス粒子及び銀被覆アルミニウム粒子からなる群より選択される、球状の銀被覆粒子を含む、請求項1~5のいずれか1項記載の導電性組成物。 The conductive composition according to any one of claims 1 to 5, further comprising spherical silver-coated particles selected from the group consisting of spherical silver-coated ceramic particles, silver-coated glass particles, and silver-coated aluminum particles. .
- (B)成分が、エポキシ樹脂、アクリル樹脂、シリコーン樹脂、ウレタン樹脂及びマレイミド樹脂からなる群より選択される1種以上である、請求項1~6のいずれか1項記載の導電性組成物。 The conductive composition according to any one of claims 1 to 6, wherein the component (B) is at least one selected from the group consisting of epoxy resins, acrylic resins, silicone resins, urethane resins, and maleimide resins.
- (C)成分が、フェノール樹脂、アミン系化合物、酸無水物、過酸化物、金属錯体及びアゾ化合物からなる群より選択される1種以上である、請求項1~7のいずれか1項記載の導電性組成物。 The component (C) is one or more selected from the group consisting of a phenol resin, an amine compound, an acid anhydride, a peroxide, a metal complex, and an azo compound. Conductive composition.
- 請求項1~8のいずれか1項記載の導電性組成物からなるダイボンディング剤。 A die bonding agent comprising the conductive composition according to any one of claims 1 to 8.
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