WO2024070068A1 - 熱伝導性グリース組成物 - Google Patents

熱伝導性グリース組成物 Download PDF

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WO2024070068A1
WO2024070068A1 PCT/JP2023/021843 JP2023021843W WO2024070068A1 WO 2024070068 A1 WO2024070068 A1 WO 2024070068A1 JP 2023021843 W JP2023021843 W JP 2023021843W WO 2024070068 A1 WO2024070068 A1 WO 2024070068A1
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Prior art keywords
thermally conductive
mass
parts
grease composition
conductive grease
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PCT/JP2023/021843
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English (en)
French (fr)
Japanese (ja)
Inventor
片石拓海
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Fuji Polymer Industries Co Ltd
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Fuji Polymer Industries Co Ltd
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Application filed by Fuji Polymer Industries Co Ltd filed Critical Fuji Polymer Industries Co Ltd
Priority to CN202380066884.8A priority Critical patent/CN119894983A/zh
Priority to US19/114,715 priority patent/US20260103656A1/en
Priority to EP23871313.5A priority patent/EP4578915A4/en
Priority to KR1020257009255A priority patent/KR20250073129A/ko
Priority to JP2023558855A priority patent/JP7500884B1/ja
Publication of WO2024070068A1 publication Critical patent/WO2024070068A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/08—Materials not undergoing a change of physical state when used
    • C09K5/14—Solid materials, e.g. powdery or granular
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/04—Mixtures of base-materials and additives
    • 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
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • 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
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • 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
    • C08K3/28—Nitrogen-containing compounds
    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/54—Silicon-containing compounds
    • C08K5/541—Silicon-containing compounds containing oxygen
    • C08K5/5415—Silicon-containing compounds containing oxygen containing at least one Si—O bond
    • C08K5/5419—Silicon-containing compounds containing oxygen containing at least one Si—O bond containing at least one Si—C bond
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/16—Ethylene-propylene or ethylene-propylene-diene copolymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M107/00—Lubricating compositions characterised by the base-material being a macromolecular compound
    • C10M107/02—Hydrocarbon polymers; Hydrocarbon polymers modified by oxidation
    • C10M107/06—Hydrocarbon polymers; Hydrocarbon polymers modified by oxidation containing propene
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M107/00—Lubricating compositions characterised by the base-material being a macromolecular compound
    • C10M107/50—Lubricating compositions characterised by the base-material being a macromolecular compound containing silicon
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/10—Metal oxides, hydroxides, carbonates or bicarbonates
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/20—Compounds containing nitrogen
    • 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
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • 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
    • C08K3/28—Nitrogen-containing compounds
    • C08K2003/282—Binary compounds of nitrogen with aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/001—Conductive additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/005—Additives being defined by their particle size in general
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06—Metal compounds
    • C10M2201/061—Carbides; Hydrides; Nitrides
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06—Metal compounds
    • C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/024—Propene
    • C10M2205/0245—Propene used as base material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
    • C10M2229/04—Siloxanes with specific structure
    • C10M2229/041—Siloxanes with specific structure containing aliphatic substituents
    • C10M2229/0415—Siloxanes with specific structure containing aliphatic substituents used as base material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2290/00—Mixtures of base materials or thickeners or additives
    • C10M2290/04—Synthetic base oils
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10—Form in which the lubricant is applied to the material being lubricated semi-solid; greasy

Definitions

  • the present invention relates to a thermally conductive grease composition suitable for placement between a heat generating body, such as an electric or electronic component, and a heat dissipating body.
  • thermally conductive grease is used to improve the adhesion between the heat sink and the heat sink, for example, the semiconductor.
  • thermally conductive grease is required to have high thermal conductivity as well as the property of not dripping easily from between the heat sink and the heat sink (known as "drop resistance").
  • Patent Document 1 proposes a composition containing a thermally conductive filler, a polyorganosiloxane resin containing at least one polysiloxane having one curable functional group in the molecule, and a siloxane compound having an alkoxysilyl group and a linear siloxane structure.
  • Patent Document 2 proposes a thermally conductive silicone composition containing liquid silicone, a thermally conductive filler, and specific hydrophobic spherical silica microparticles, and having improved heat dissipation properties.
  • Patent Document 3 discloses a thermally conductive fluorine-containing adhesive composition containing alumina with different particle sizes and shapes.
  • Patent Documents 4 and 5 the present inventor proposes a thermally conductive grease composition containing an ethylene- ⁇ -olefin copolymer.
  • thermally conductive silicone greases of Patent Documents 1 to 3 have the problem that, for example, when interposed between a heating element and a heat sink and sandwiched vertically between the heating element and the heat sink, they drip from between the heating element and the heat sink.
  • thermally conductive grease compositions of Patent Documents 4 and 5 have the problem of being more viscous than thermally conductive silicone grease.
  • the present invention provides a thermally conductive grease composition that has low viscosity, is less likely to drip, and has high thermal conductivity.
  • the thermally conductive grease composition of the present invention comprises: A thermally conductive grease composition comprising a matrix resin and a thermally conductive filler, the matrix resin comprises a liquid dimethylpolysiloxane (A) having a kinetic viscosity at 40° C. of 100 to 10,000 mm 2 /s and an ethylene-propylene copolymer (B) having a kinetic viscosity at 40° C.
  • a thermally conductive grease composition comprising a matrix resin and a thermally conductive filler, the matrix resin comprises a liquid dimethylpolysiloxane (A) having a kinetic viscosity at 40° C. of 100 to 10,000 mm 2 /s and an ethylene-propylene copolymer (B) having a kinetic viscosity at 40° C.
  • the matrix resin contains 50 parts by mass or more and 97 parts by mass or less of the liquid dimethylpolysiloxane (A) and 3 parts by mass or more and 50 parts by mass or less of the ethylene-propylene copolymer (B);
  • the thermally conductive filler is contained in an amount of 400 to 2500 parts by mass per 100 parts by mass of the total amount of the liquid dimethylpolysiloxane (A) and the ethylene-propylene copolymer (B).
  • the present invention relates to a thermally conductive grease composition
  • a thermally conductive grease composition comprising a matrix resin and a thermally conductive filler, the matrix resin being composed of a liquid dimethylpolysiloxane (A) having a kinetic viscosity at 40° C. of 100 to 10,000 mm 2 /s and a thermally conductive filler (B) having a kinetic viscosity at 40° C. of 1 to 10,000 mm 2 / s.
  • A liquid dimethylpolysiloxane
  • B thermally conductive filler
  • the matrix resin contains 50 parts by mass or more and 97 parts by mass or less of the liquid dimethylpolysiloxane (A) and 3 parts by mass or more and 50 parts by mass or less of the ethylene-propylene copolymer (B), and by containing 400 to 2500 parts by mass of the thermally conductive filler per 100 parts by mass of the total amount of the liquid dimethylpolysiloxane (A) and the ethylene-propylene copolymer (B), it is possible to provide a thermally conductive grease composition that is low in viscosity, does not drip easily, and has high thermal conductivity.
  • 1A and 1B are explanatory diagrams showing a method for measuring the thermal conductivity of a sample in one embodiment of the present invention.
  • 2A to 2D are schematic explanatory views illustrating a drop test used in one embodiment of the present invention.
  • the thermally conductive grease composition of the present invention (hereinafter sometimes abbreviated as "grease composition”) comprises a matrix resin and a thermally conductive filler, and the matrix resin comprises a liquid dimethylpolysiloxane (A) having a kinetic viscosity of 100 to 10,000 mm 2 /s at 40°C, and an ethylene-propylene copolymer (B) having a kinetic viscosity of 1 to 10,000 mm 2 /s at 40°C.
  • the liquid dimethylpolysiloxane (A) has high heat resistance, while the ethylene-propylene copolymer (B) tends to harden at high temperatures.
  • the liquid dimethylpolysiloxane (A) preferably has a kinetic viscosity at 40° C. of 100 to 5000 mm 2 /s, more preferably 100 to 3000 mm 2 /s, even more preferably 100 to 1000 mm 2 /s, still more preferably 100 to 400 mm 2 /s, and even more preferably 100 to 200 mm 2 /s.
  • the ethylene-propylene copolymer (B) preferably has a kinetic viscosity at 40° C.
  • the grease composition of the present invention has excellent heat resistance and low viscosity, yet is less likely to drip when clamped vertically.
  • the ethylene-propylene copolymer (B) is a hydrocarbon-based synthetic oil that does not contain polar groups, and examples of commercially available products include the "Lucant" series manufactured by Mitsui Chemicals, Inc.
  • the density of the ethylene-propylene copolymer is preferably 0.83 to 0.85 g/ cm3 , which has the advantage of allowing the specific gravity of the grease composition to be reduced.
  • the arrangement of the ethylene-derived units and the propylene-derived units in the ethylene-propylene copolymer (B) may be either block or random.
  • the content of the thermally conductive filler is 400 to 2500 parts by mass, preferably 600 to 2400 parts by mass, more preferably 800 to 2400 parts by mass, and even more preferably 1000 to 2400 parts by mass. This allows the grease composition to have a low viscosity, yet is less likely to drip, and has a high thermal conductivity.
  • the content of liquid dimethylpolysiloxane (A) is 50 parts by mass or more and 97 parts by mass or less, and the content of ethylene-propylene copolymer (B) is 3 parts by mass or more and 50 parts by mass or less, preferably the content of liquid dimethylpolysiloxane (A) is 55 parts by mass or more and 95 parts by mass or less, and the content of ethylene-propylene copolymer (B) is 5 parts by mass or more and 45 parts by mass or less, more preferably the content of liquid dimethylpolysiloxane (A) is 60 parts by mass or more and 94 parts by mass or less, and the content of ethylene-propylene copolymer (B) is 6 parts by mass or more and 40 parts by mass or less, and even more preferably the content of liquid dimethylpolysiloxane (
  • the thermally conductive filler preferably contains 20 to 2000 parts by mass of alumina having a median particle size of 1 ⁇ m or more and 5 ⁇ m or less, more preferably 100 to 600 parts by mass, and even more preferably 200 to 500 parts by mass.
  • the thermally conductive filler preferably contains 20 to 1500 parts by mass of spherical alumina having a median particle size of more than 100 ⁇ m, 20 to 500 parts by mass of aluminum nitride having a median particle size of 5 ⁇ m or more and 50 ⁇ m or less, 20 to 1000 parts by mass of irregularly pulverized alumina having a median particle size of 1 ⁇ m or more and 5 ⁇ m or less, and 20 to 500 parts by mass of irregularly pulverized alumina having a median particle size of 0.1 ⁇ m or more and less than 1 ⁇ m.
  • the thermally conductive filler contains 500 to 1200 parts by mass of spherical alumina having a median particle size of more than 100 ⁇ m, 50 to 400 parts by mass of aluminum nitride having a median particle size of 5 ⁇ m or more and 50 ⁇ m or less, 100 to 600 parts by mass of irregularly ground alumina having a median particle size of 1 ⁇ m or more and 5 ⁇ m or less, and 50 to 400 parts by mass of irregularly ground alumina having a median particle size of 0.1 ⁇ m or more and less than 1 ⁇ m, and the thermally conductive filler contains 700 to 1200 parts by mass of spherical alumina having a median particle size of more than 100 ⁇ m, 100 to 400 parts by mass of aluminum nitride having
  • the thermally conductive filler contains 150 to 500 parts by mass of amorphous crushed alumina having a particle size of 1 ⁇ m or more and 5 ⁇ m or less, and 100 to 400 parts by mass of amorphous crushed alumina having a central particle size of 0.1 ⁇ m or more and less than 1 ⁇ m.
  • the thermally conductive filler contains 800 to 1100 parts by mass of spherical alumina having a central particle size of more than 100 ⁇ m, 150 to 400 parts by mass of aluminum nitride having a central particle size of 5 ⁇ m or more and 50 ⁇ m or less, 200 to 500 parts by mass of amorphous crushed alumina having a central particle size of 1 ⁇ m or more and 5 ⁇ m or less, and 100 to 400 parts by mass of amorphous crushed alumina having a central particle size of 0.1 ⁇ m or more and less than 1 ⁇ m.
  • the spherical alumina having a median particle size exceeding 100 ⁇ m is preferably spherical alumina having a median particle size exceeding 100 ⁇ m and not exceeding 200 ⁇ m, more preferably having a median particle size exceeding 100 ⁇ m and not exceeding 150 ⁇ m.
  • the shape of the aluminum nitride having a median grain size of 5 ⁇ m to 50 ⁇ m is preferably irregular.
  • the aluminum nitride having a median grain size of 5 ⁇ m to 50 ⁇ m is preferably aluminum nitride having a median grain size of 5 ⁇ m to 30 ⁇ m.
  • the median particle size is the D50 (median diameter) of the cumulative particle size distribution based on volume measured by a laser diffraction light scattering method.
  • An example of this measuring device is the LA-950S2 laser diffraction/scattering type particle size distribution measuring device manufactured by Horiba, Ltd.
  • the grease composition of the present invention preferably further contains, as a viscosity modifier, 0.1 to 10 parts by mass of an alkoxysilane compound represented by R a Si(OR') 4-a (wherein R is an unsubstituted or substituted organic group having 8 to 12 carbon atoms, R' is an alkyl group having 1 to 4 carbon atoms, and a is 0 or 1) or a partial hydrolyzate thereof, per 100 parts by mass of the total amount of the liquid dimethylpolysiloxane (A) and the ethylene-propylene copolymer (B).
  • R alkoxysilane compound represented by R a Si(OR') 4-a
  • R is an unsubstituted or substituted organic group having 8 to 12 carbon atoms
  • R' is an alkyl group having 1 to 4 carbon atoms
  • a is 0 or 1
  • the thermally conductive filler is preferably surface-pretreated with an alkoxysilane compound represented by R a Si(OR') 4-a (wherein R is an unsubstituted or substituted organic group having 8 to 12 carbon atoms, R' is an alkyl group having 1 to 4 carbon atoms, and a is 0 or 1) or a partial hydrolyzate thereof.
  • R is an unsubstituted or substituted organic group having 8 to 12 carbon atoms
  • R' is an alkyl group having 1 to 4 carbon atoms
  • a is 0 or 1
  • small particle size fillers having a median particle size of 0.1 ⁇ m or more and 5 ⁇ m or less are surface-pretreated.
  • alkoxysilane compounds include octyltrimethoxysilane, octyltriethoxysilane, decyltrimethoxysilane, decyltriethoxysilane, dodecyltrimethoxysilane, and dodecyltriethoxysilane.
  • the alkoxysilane compounds can be used alone or in combination of two or more.
  • a surface treatment agent an alkoxysilane compound and a siloxane having a silanol end may be used in combination. Surface treatment here includes adsorption as well as covalent bonding. If the surface is treated, the thermally conductive filler will have good mixability with the matrix resin.
  • the alkoxysilane compound is preferably mixed with the thermally conductive filler in advance, and the thermally conductive filler is preferably pretreated with the alkoxysilane compound. It is preferable to add 0.01 to 10 parts by mass of the alkoxysilane compound per 100 parts by mass of the thermally conductive filler. By surface treating the thermally conductive filler with the alkoxysilane compound, it becomes easier to fill the matrix resin.
  • the thermal conductivity of the thermally conductive grease composition is preferably 1.0 W/m ⁇ K or more and 10.0 W/m ⁇ K or less, more preferably 1.5 W/m ⁇ K or more and 10.0 W/m ⁇ K or less, and even more preferably 2.0 W/m ⁇ K or more and 10.0 W/m ⁇ K or less.
  • Such thermally conductive grease is suitable as a TIM (Thermal Interface Material).
  • the thermally conductive grease composition preferably has an absolute viscosity at 23°C measured with a B-type viscometer at a rotation speed of 5 rpm using a T-E spindle of 1,000 Pa ⁇ s or more and 20,000 Pa ⁇ s or less, more preferably 1,000 Pa ⁇ s or more and 18,000 Pa ⁇ s or less, even more preferably 1,000 Pa ⁇ s or more and 15,000 Pa ⁇ s or less, and even more preferably 1,000 Pa ⁇ s or more and 10,000 Pa ⁇ s or less.
  • This results in a thermally conductive grease composition that is easy to work with and can be easily injected or applied between a heating element and a heat sink.
  • the plates are held in a heat shock tester so that the main surfaces of the plates are perpendicular to the ground, and then the plate is held at -40°C for 30 minutes, heated to 125°C, held at 125°C for 30 minutes, and cooled to -40°C, this cycle is repeated 500 times.
  • the thermally conductive grease composition falls within 5 mm from the start of the test. This allows high drop resistance to be maintained.
  • the thermally conductive grease composition of the present invention may contain, as necessary, a heat resistance improver such as red iron oxide, titanium oxide, or cerium oxide, a flame retardant, or a flame retardant assistant.
  • the thermally conductive grease composition of the present invention may also contain, as necessary, an organic or inorganic particle pigment for the purpose of coloring or color matching.
  • the thermally conductive grease composition of the present invention may also contain, as necessary, an alkoxy group-containing silicone for the purpose of surface treatment of the thermally conductive filler.
  • the thermally conductive grease composition of the present invention does not particularly require a curing catalyst, and it is preferable that the thermally conductive grease composition of the present invention is a non-curing type grease.
  • the thermally conductive grease composition of the present invention can be filled into containers, bottles, cans, tubes, etc. to produce a product.
  • the present invention relates to the use of the thermally conductive grease of the present invention, in which the thermally conductive grease composition of the present invention is interposed between a heating element and a heat dissipation element.
  • the present invention relates to the use of the thermally conductive grease of the present invention, in which the thermally conductive grease composition of the present invention is interposed between a heating element and a heat dissipation element, and the thermally conductive grease is sandwiched vertically between the heating element and the heat dissipation element.
  • heating elements include electrical components, or electronic components such as semiconductor elements.
  • heat dissipation elements include heat sinks, etc.
  • the thermal conductivity of the thermally conductive grease composition was measured by a hot disk (ISO/CD 22007-2 compliant). As shown in FIG. 1A, this thermal conductivity measuring device 1 sandwiches a polyimide film sensor 2 between two samples 3a and 3b, applies a constant power to the sensor 2, and generates a constant amount of heat, and analyzes the thermal characteristics from the temperature rise value of the sensor 2.
  • the sensor 2 has a tip 4 with a diameter of 7 mm, and as shown in FIG. 1B, has a double spiral electrode structure, with an applied current electrode 5 and a resistance value electrode (temperature measurement electrode) 6 arranged at the bottom.
  • the thermal conductivity is calculated by the following formula (Math. 1).
  • the absolute viscosity of the thermally conductive grease composition was measured using a Brookfield HBDV2T viscometer.
  • the spindle used was a T-E spindle, and the absolute viscosity was measured at a rotation speed of 5 rpm (except for Comparative Examples 3 and 4, which were rotated at 0.5 rpm) at 23°C.
  • thermally conductive grease composition ⁇ Drop test of thermally conductive grease composition> The drop test of the thermally conductive grease composition will be described with reference to FIGS. 2A to 2D.
  • 0.4 g of the thermally conductive grease composition 14 was applied to an aluminum plate 12 having a length of 40 mm, a width of 100 mm, and a thickness of 5 mm (FIG. 2A), and the aluminum plate and a glass plate 11 having a length of 40 mm, a width of 100 mm, and a thickness of 5 mm were sandwiched between them with a spacer 13 so that the thickness of the thermally conductive grease composition was 0.5 mm (FIG. 2B).
  • FIG. 2A The drop test of the thermally conductive grease composition will be described with reference to FIGS. 2A to 2D.
  • 0.4 g of the thermally conductive grease composition 14 was applied to an aluminum plate 12 having a length of 40 mm, a width of 100 mm, and a thickness of 5 mm (FIG. 2
  • 15 denotes the thermally conductive grease composition sandwiched between the two plates 11 and 12 so that the thickness was 0.5 mm.
  • the aluminum plate 12 and the glass plate 11 were placed in a heat cycle tester so that the main surfaces of the plate 12 and the glass plate 11 were perpendicular to the ground (FIG. 2C).
  • 16 denotes the test piece before the test. In this state, the plate was held at -40°C for 30 minutes, then heated to 125°C, and then held at 125°C for 30 minutes, and then cooled to -40°C. This cycle was repeated 500 times. After 500 cycles, the test piece was removed and observed to see if the thermal conductive grease 15 had fallen. In Fig.
  • the kinematic viscosity is a kinematic viscosity at 40° C. measured with an Ubbelohde viscometer.
  • Examples 1 to 3, Comparative Examples 1 to 3 1.
  • Raw Material Component (1) Liquid Dimethylpolysiloxane As the liquid dimethylpolysiloxane (A), a dimethylsilicone oil having a kinetic viscosity of 110 mm 2 /s (catalog value) at 40° C. (manufactured by Dow-Toray, trade name "SH200CV 110CS", specific gravity 0.97 g/cm 3 ) was used.
  • Ethylene-Propylene Copolymer As the ethylene-propylene copolymer (B), an ethylene-propylene copolymer having a kinetic viscosity of 200 mm 2 /s (catalog value) at 40° C.
  • Viscosity modifier Decyltrimethoxysilane (specific gravity: 0.90 g/cm 3 ) was used.
  • Examples 1 to 3 were thermally conductive grease compositions that, while having low viscosity, were not prone to dripping when held vertically, could be highly filled with thermally conductive filler, and had high thermal conductivity.
  • the drop test results were poor in Comparative Example 1 because no ethylene-propylene copolymer was added as a matrix resin
  • the drop test results were poor in Comparative Example 2 because the content of the ethylene-propylene copolymer was low
  • the drop test results were poor in Comparative Examples 3 and 4 because the content of the ethylene-propylene copolymer was too high, resulting in a problem of high viscosity.
  • the thermally conductive grease composition of the present invention is suitable as a thermal interface material to be interposed between a heat generating body and a heat dissipating body, such as an electric or electronic component.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Combustion & Propulsion (AREA)
  • Thermal Sciences (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • Lubricants (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Cooling Or The Like Of Semiconductors Or Solid State Devices (AREA)
PCT/JP2023/021843 2022-09-26 2023-06-13 熱伝導性グリース組成物 Ceased WO2024070068A1 (ja)

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US19/114,715 US20260103656A1 (en) 2022-09-26 2023-06-13 Thermally conductive grease composition
EP23871313.5A EP4578915A4 (en) 2022-09-26 2023-06-13 THERMOCONDUCTIVE GREASE COMPOSITION
KR1020257009255A KR20250073129A (ko) 2022-09-26 2023-06-13 열전도성 그리스 조성물
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JP7690705B1 (ja) * 2024-08-06 2025-06-10 富士高分子工業株式会社 熱伝導性シート及びその製造方法

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WO2024224832A1 (ja) * 2023-04-27 2024-10-31 富士高分子工業株式会社 熱伝導性シリコーン樹脂組成物
JP7618897B1 (ja) * 2023-04-27 2025-01-21 富士高分子工業株式会社 熱伝導性シリコーン樹脂組成物
JP7690705B1 (ja) * 2024-08-06 2025-06-10 富士高分子工業株式会社 熱伝導性シート及びその製造方法

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JP7500884B1 (ja) 2024-06-17
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