WO2020241054A1 - 熱伝導性シリコーン組成物、半導体装置及びその製造方法 - Google Patents

熱伝導性シリコーン組成物、半導体装置及びその製造方法 Download PDF

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WO2020241054A1
WO2020241054A1 PCT/JP2020/015462 JP2020015462W WO2020241054A1 WO 2020241054 A1 WO2020241054 A1 WO 2020241054A1 JP 2020015462 W JP2020015462 W JP 2020015462W WO 2020241054 A1 WO2020241054 A1 WO 2020241054A1
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group
component
heat
conductive silicone
silicone composition
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翔太 秋場
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Shin Etsu Chemical Co Ltd
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Shin Etsu Chemical Co Ltd
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Priority to CN202080037748.2A priority Critical patent/CN113853676A/zh
Priority to KR1020217037727A priority patent/KR20220012850A/ko
Priority to EP20813307.4A priority patent/EP3979314A4/en
Priority to US17/607,133 priority patent/US12060517B2/en
Publication of WO2020241054A1 publication Critical patent/WO2020241054A1/ja
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Definitions

  • the present invention relates to a thermally conductive silicone composition, a semiconductor device, and a method for producing the same.
  • Patent Document 1 describes a silicone grease composition obtained by blending a specific organopolysiloxane with a spherical hexagonal aluminum nitride powder having a certain particle size range
  • Patent Document 2 describes a fine-grained aluminum nitride powder and a particle size.
  • Patent Document 3 describes a thermally conductive silicone grease combining aluminum nitride powder and zinc oxide powder
  • Patent Document 4 provides surface treatment with organosilane.
  • a heat conductive grease composition using the aluminum nitride powder is disclosed.
  • Patent Document 5 discloses a thermally conductive silicone composition using diamond, zinc oxide, and a dispersant as the silicone resin.
  • Patent Document 6 and Patent Document 7 disclose a thermally conductive grease composition in which a metal aluminum powder is mixed with a base oil such as silicone oil. Further, Patent Documents 8 to 12 and the like also disclose that silver powder having high thermal conductivity is used as a filler. Some of the above show high thermal conductivity, but the minimum thickness (BLT) at the time of compression is thick and the thermal resistance is high. On the other hand, those with low thermal resistance have high hardness after heat curing, and when applied to electronic components, they are easily peeled off and lack reliability. Therefore, any of the thermally conductive materials and the thermally conductive grease has become insufficient for the amount of heat generated by the recent integrated circuit elements such as CPUs.
  • BLT minimum thickness
  • the present invention has been made to solve the above problems, and an object of the present invention is to use a thermally conductive silicone composition that gives a cured product having good heat dissipation characteristics and a cured product of the composition.
  • the purpose is to provide a semiconductor device and a method for manufacturing the same.
  • the present invention provides a thermally conductive silicone composition containing the following components (A), (B), (C), (D) and (E).
  • (A) Organopolysiloxane containing at least two alkenyl groups bonded to silicon atoms in one molecule: 100 parts by mass
  • (B) Organohydrogenpolysiloxane containing at least two hydrogen atoms bonded to a silicon atom in one molecule: A hydrogen atom bonded to a silicon atom in the component (B) per mole of an alkenyl group in the entire composition.
  • This thermally conductive silicone composition provides a cured product having excellent thermal conductivity, that is, low thermal resistance, and is therefore useful for semiconductor devices that require a good heat dissipation effect.
  • the semiconductor device includes a heat-generating electronic component and a heat radiating body, and a cured product of the heat conductive silicone composition is interposed between the heat-generating electronic component and the heat radiating body.
  • a heat-generating electronic component and a heat radiating body
  • a cured product of the heat conductive silicone composition is interposed between the heat-generating electronic component and the heat radiating body.
  • a method for manufacturing a semiconductor device comprising a step of heating the thermally conductive silicone composition to 80 ° C. or higher in a state where a pressure of 0.01 MPa or higher is applied between a heat-generating electronic component and a radiator.
  • a pressure of 0.01 MPa or higher is applied between a heat-generating electronic component and a radiator.
  • the thermally conductive silicone composition of the present invention provides a cured product having excellent thermal conductivity, that is, low thermal resistance, and is therefore useful for semiconductor devices that require a good heat dissipation effect.
  • the present inventors have obtained silver powder having a specific tap density, specific surface area, and aspect ratio, and graphite powder having a specific average particle size into a specific organopolysiloxane.
  • the present invention has been completed by finding that the thermal conductivity of the cured product of the composition is dramatically improved by mixing the mixture therein.
  • the present invention is a thermally conductive silicone composition containing the following components (A), (B), (C), (D) and (E).
  • (A) Organopolysiloxane containing at least two alkenyl groups bonded to silicon atoms in one molecule: 100 parts by mass
  • (B) Organohydrogenpolysiloxane containing at least two hydrogen atoms bonded to a silicon atom in one molecule: A hydrogen atom bonded to a silicon atom in the component (B) per mole of an alkenyl group in the entire composition.
  • the organopolysiloxane of the component (A) is the base polymer of the composition of the present invention, and contains at least two alkenyl groups bonded to a silicon atom in one molecule.
  • Examples of the molecular structure of the component (A) include a linear structure and a cyclic structure, and these structures may have branches, but the main chain is basically repeated from the diorganosiloxane unit. Therefore, a linear diorganopolysiloxane having both ends of the molecular chain sealed with a triorganosyloxy group is preferably used as the component (A).
  • the kinematic viscosity of the component (A) at 25 ° C. is 10 mm 2 / s or more, oil bleeding is unlikely to occur in the composition, and if it is 100,000 mm 2 / s or less, the kinematic viscosity of the composition does not increase, so handleability Is good. Therefore, the kinematic viscosity of the component (A) at 25 ° C. is preferably 10 to 100,000 mm 2 / s, and more preferably 100 to 50,000 mm 2 / s.
  • the kinematic viscosity of the organopolysiloxane of the component (A) described in the present specification is a value of 25 ° C. measured by an Ostwald viscometer.
  • the alkenyl group bonded to the silicon atom in the component (A) for example, the number of carbon atoms such as vinyl group, allyl group, butenyl group, pentenyl group, hexenyl group and heptenyl group is preferably 2 to 8, more preferably. 2 to 4 are mentioned, and a vinyl group is more preferable.
  • the organopolysiloxane of the component (A) has a linear structure, the alkenyl group is silicon at either the molecular chain end or the non-molecular chain end portion, even if it is bonded to the silicon atom. It may be bonded to an atom.
  • Examples of the organic group bonded to the silicon atom other than the alkenyl group in the component (A) include an alkyl group, particularly a methyl group, an ethyl group, a bropyl group, a butyl group, a pentyl group, a hexyl group, a cyclohexyl group and a heptyl group.
  • Aralkyl groups with 7 to 14 atoms alkyl halide groups, especially alkyl halides with 1 to 3 carbon atoms such as chloromethyl group, 3-chloropropyl group, 3,3,3-trifluoropropyl group, etc. Examples thereof include an unsubstituted or halogen-substituted monovalent hydrocarbon group, and a methyl group and a phenyl group are particularly preferable.
  • component (A) examples include a trimethylsiloxy group-blocking dimethylsiloxane / methylvinylsiloxane copolymer at both ends of the molecular chain, a trimethylsiloxy group-blocking methylvinylpolysiloxane at both ends of the molecular chain, and a trimethylsiloxy group-blocking dimethyl at both ends of the molecular chain.
  • R 1 is an unsubstituted or substituted monovalent hydrocarbon groups other than alkenyl groups hereinafter the same) siloxane units of the formula: R 1 2 R 2 SiO 0.5 (R 2 is It is an alkenyl group.
  • R 1 in the above formula examples include alkyl groups such as methyl group, ethyl group, propyl group, butyl group, pentyl group, hexyl group and heptyl group; aryl groups such as phenyl group, tolyl group, xsilyl group and naphthyl group. Groups; Aralkyl groups such as benzyl group and phenethyl group; Alkyl halide groups such as chloromethyl group, 3-chloropropyl group and 3,3,3-trifluoropropyl group can be mentioned.
  • examples of R 2 in the above formula include a vinyl group, an allyl group, a butenyl group, a pentenyl group, a hexenyl group, and a heptenyl group.
  • the composition of the present invention preferably contains the component (A) in an amount of 4 to 25% by mass.
  • the organohydrogenpolysiloxane of the component (B) reacts with the component (A) and acts as a cross-linking agent.
  • the molecular structure of the component (B) is not particularly limited, and various conventionally known organohydrogenpolysiloxanes such as linear, cyclic, branched, and three-dimensional network structures (resin-like) can be used.
  • the number of organohydrogenpolysiloxane as the component (B) is 2 or more, preferably 3 or more (usually 3 to 500, preferably 3 to 200, more preferably about 3 to 100) in one molecule.
  • the organohydrogenpolysiloxane of the component (B) has a linear structure, these SiH groups are located at either the molecular chain end or the non-molecular chain end portion, even if they are located at both of them. May be.
  • the number of silicon atoms (degree of polymerization) in one molecule of the component (B) is preferably about 2 to 1,000, more preferably 3 to 300, and even more preferably about 4 to 150.
  • the viscosity of the component (B) at 25 ° C. is preferably 0.1 to 5,000 mPa ⁇ s, more preferably 0.5 to 1,000 mPa ⁇ s, still more preferably about 5 to 500 mPa ⁇ s.
  • the viscosity (absolute viscosity) of the organohydrogenpolysiloxane of the component (B) described in the present specification is, for example, a value of 25 ° C. measured by model number PC-1TL (10 rpm) manufactured by Malcolm Co., Ltd.
  • R 3 is a monovalent hydrocarbon group bonded to a silicon atom having an unsubstituted or substituted carbon atom number of preferably 1 to 14, more preferably 1 to 10, excluding an aliphatic unsaturated group.
  • a and b are preferably 0.7 ⁇ a ⁇ 2.1, 0.001 ⁇ b ⁇ 1.0, and 0.8 ⁇ a + b ⁇ 3.0, more preferably 0.9 ⁇ a ⁇ 2.
  • Organohydrogenpolysiloxane represented by is used.
  • R 3 include methyl group, ethyl group, propyl group, isopropyl group, butyl group, isobutyl group, tert-butyl group, pentyl group, neopentyl group, hexyl group, cyclohexyl group, octyl group, nonyl group and decyl.
  • Alkyl groups such as groups; aryl groups such as phenyl group, trill group, xsilyl group and naphthyl group; aralkyl groups such as benzyl group, phenylethyl group and phenylpropyl group; some of hydrogen atoms in these hydrocarbon groups or Examples thereof include a group entirely substituted with a halogen atom such as fluorine, bromine and chlorine, for example, a chloromethyl group, a 3-chloropropyl group, a bromoethyl group, a 3,3,3-trifluoropropyl group and the like, and an alkyl group is preferable.
  • An aryl group more preferably a methyl group or a phenyl group.
  • the component (B) can be obtained by a known production method.
  • a general production method for example, 1,3,5,7-tetramethyl-1,3,5,7-tetrahydrocyclotetrasiloxane (in some cases, the cyclotetrasiloxane and octamethylcyclotetrasiloxane) (Mixa) and a siloxane compound as a terminal source such as hexamethyldisiloxane, 1,3-dihydro-1,1,3,3-tetramethyldisiloxane, or octamethylcyclotetrasiloxane and 1,3.
  • a method of equilibrating -dihydro-1,1,3,3-tetramethyldisiloxane at a temperature of about -10 to + 40 ° C. in the presence of a catalyst such as sulfuric acid, trifluoromethanesulfonic acid, or methanesulfonic acid is mentioned. Be done.
  • component (B) examples include 1,1,3,3-tetramethyldisiloxane, 1,3,5,7-tetramethylcyclotetrasiloxane, tris (dimethylhydrogensiloxy) methylsilane, and tris (dimethylhydro).
  • These components (B) can be used alone or in combination of two or more.
  • the amount of the component (B) to be blended is such that the amount of hydrogen atoms (SiH groups) bonded to the silicon atom in the component (B) is 0.2 to 10 mol, preferably 1 per mol of the alkenyl group in the total composition.
  • the amount is in the range of 0.0 to 8.0 mol.
  • the ratio of the alkenyl group bonded to the silicon atom in the component (A) to the alkenyl group present in the entire composition is preferably 50 to 100 mol%, more preferably 80 to 100 mol%.
  • the amount of SiH group in the component (B) is increased per mole of the alkenyl group bonded to the silicon atom in the component (A).
  • the amount is in the range of 0.2 to 10 mol, preferably 1.0 to 5.0 mol. If the amount of the component (B) is too small, the composition may not be sufficiently cured, and if it is too large, the heat resistance of the obtained cured product (silicone rubber) may be extremely inferior.
  • catalyst for the hydrosilylation reaction of the component (C) any catalyst may be used as long as it promotes the addition reaction between the alkenyl group in the component (A) and the SiH group in the component (B). ..
  • platinum-based catalysts such as rhodium chloride, alcohol-modified rhodium chloride, coordination compounds of rhodium chloride with olefins, vinyl siloxane or acetylene compounds; palladium catalysts such as tetrakis (triphenylphosphine) palladium; chlorotris (chlorotris ( A rhodium-based catalyst such as triphenylphosphine) rhodium is used as the component (C), but a platinum-based catalyst such as a platinum-divinyltetramethyldisiloxane complex is preferable.
  • the blending amount of the component (C) is in the range of 0.1 to 2,000 ppm, preferably 1 to 1,500 ppm on a mass basis in terms of the catalytic metal element with respect to the total amount of the components (A) and (B). Is. If the blending amount is too small, the addition reaction is not sufficiently promoted and curing is insufficient, and if the blending amount is too large, it is economically disadvantageous.
  • the type of metal catalyst is not particularly limited as long as it is a metal having an effective activity as a catalyst for a hydrosilylation reaction, but platinum or the like having an activity of dividing hydrogen gas into atoms is useful.
  • the component (D) is a silver powder having a tap density of 3.0 g / cm 3 or more, a specific surface area of 2.0 m 2 / g or less, and an aspect ratio of 1 to 30. If the tap density of the silver powder of the component (D) is less than 3.0 g / cm 3 , the filling rate of the component (D) into the composition cannot be increased, the viscosity of the composition increases, and the workability is poor.
  • the range of 3.0 g / cm 3 to 8.0 g / cm 3 is preferable, and the range of 4.5 g / cm 3 to 8.0 g / cm 3 is more preferable, and the range of 5.5 g / cm 3 to 8.0 g is more preferable.
  • a range of / cm 3 is even more preferred.
  • the specific surface area of the silver powder of the component (D) is larger than 2.0 m 2 / g, the filling rate of the component (D) into the composition cannot be increased, the viscosity of the composition increases, and the workability is deteriorated.
  • the filling rate of the component (D) into the composition cannot be increased, the viscosity of the composition increases, and the workability is deteriorated.
  • the range of 0.08m 2 /g ⁇ 2.0m 2 / g to become, more preferably in the range of 0.08m 2 /g ⁇ 1.5m 2 / g, 0.08m 2 /g ⁇ 1.0m 2
  • the / g range is even more preferred.
  • the tap density described in the present specification is such that 100 g of silver powder is weighed, the silver powder is gently dropped into a 100 ml graduated cylinder with a funnel, and then the cylinder is placed on a tap density measuring instrument and the head distance is 20 mm, 60 times /. It is a value calculated from the volume of silver powder that has been dropped 600 times at a speed of 1 minute and compressed.
  • the aspect ratio of the silver powder of the component (D) is 1 to 30, preferably in the range of 2 to 20, and more preferably in the range of 3 to 15.
  • the aspect ratio refers to the ratio of the major axis to the minor axis (major axis / minor axis) of the particles.
  • a measuring method for example, an electron micrograph of a particle can be taken, and the major axis and the minor axis of the particle can be measured and calculated from this photograph.
  • the size of the particles can be measured by an electron micrograph from the upper surface, and the larger diameter is measured as the major axis from the electron micrograph on the upper surface.
  • the minor axis is the thickness of the particles with respect to the major axis. Particle thickness cannot be measured by electron micrograph from above.
  • the thickness of the particles when taking an electron micrograph, attach the sample table on which the particles are placed at an angle, take an electron micrograph from the top, and correct the angle of the inclination of the sample table to correct the particles.
  • the thickness of is calculated. Specifically, after taking several photographs magnified several thousand times with an electron microscope, the major axis and minor axis of 100 particles are arbitrarily measured, and the ratio of major axis to minor axis (major axis / minor axis) is determined. After calculation, the average value was calculated and used as the aspect ratio.
  • the particle size of the silver powder of the component (D) is not particularly limited, but the average particle size is preferably in the range of 0.2 to 30 ⁇ m, more preferably in the range of 1.0 to 20 ⁇ m.
  • the average particle size is the volume measured by a laser diffraction particle size analyzer after taking 1 to 2 cups of silver powder in a 100 ml beaker with a microspatella, adding about 60 ml of isopropyl alcohol, and dispersing the silver powder with an ultrasonic homogenizer for 1 minute. It is a reference volume average diameter [MV]. The measurement time was 30 seconds.
  • the method for producing the silver powder used in the present invention is not particularly limited, and examples thereof include an electrolysis method, a pulverization method, a heat treatment method, an atomizing method, and a reduction method.
  • the silver powder the one produced by the above method may be used as it is, or may be pulverized and used within a range satisfying the above numerical range.
  • the apparatus is not particularly limited, and for example, known apparatus such as a stamp mill, a ball mill, a vibration mill, a hammer mill, a rolling roller, and a mortar can be used. Of these, stamp mills, ball mills, vibration mills, and hammer mills are preferable.
  • the blending amount of the component (D) is 300 to 2,000 parts by mass with respect to 100 parts by mass of the component (A).
  • the blending amount of the component (D) is less than 300 parts by mass with respect to 100 parts by mass of the component (A)
  • the thermal resistance of the pressurized heat-cured product of the obtained composition becomes large, and when it is more than 2,000 parts by mass.
  • the hardness of the heat-cured product under pressure becomes high and the reliability deteriorates.
  • the blending amount of the component (D) is preferably in the range of 500 to 1,500 parts by mass, more preferably 600 to 1,200 parts by mass with respect to 100 parts by mass of the component (A).
  • the component (E) is a natural graphite powder or an artificial graphite powder having an average particle size of 3 ⁇ m to 50 ⁇ m. Since the heat conductive silicone composition of the present invention contains graphite powder in a specific particle size range, it has low thermal resistance and hardness after pressure heat curing, and has good heat dissipation and reliability. This is because the graphite powder suppresses excessive sintering of the silver powder without inhibiting the formation of the heat conduction path.
  • the average particle size of the graphite powder of the component (E) is 3 ⁇ m to 50 ⁇ m, preferably 8 ⁇ m to 40 ⁇ m, and more preferably 10 ⁇ m to 30 ⁇ m. If the average particle size is smaller than 3 ⁇ m, the viscosity of the composition increases and the handleability deteriorates, and if the average particle size is larger than 50 ⁇ m, the formation of a heat conduction path of the silver powder is inhibited, and the cured product of the composition. Thermal performance is reduced.
  • the average particle size of the graphite powder in the component (E) is, for example, a volume-based volume average diameter [MV] that can be measured by Microtrac MT330OEX manufactured by Nissouki Co., Ltd.
  • the natural graphite powder of the component (E) is a collection of particles made of natural graphite.
  • the main component of natural graphite is carbon.
  • the shape of natural graphite differs depending on the place of origin and the like, and includes scaly, lumpy, and soil-like shapes.
  • scaly natural graphite is graphite that is mainly produced from mines in China, the United States, India, Brazil, etc. and has a large aspect ratio.
  • Agglomerated natural graphite is a graphite with a small aspect ratio produced from a mine in Sri Lanka.
  • the artificial graphite powder of the component (E) is a collection of particles made of artificial graphite.
  • Artificial graphite is graphite obtained by treating coke or the like at a high temperature of about 3000 ° C. Examples of the shape of the artificial graphite include a plate shape and a lump shape.
  • the blending amount of the component (E) is in the range of 0.3 to 100 parts by mass, preferably 1 to 20 parts by mass, and more preferably 2 to 10 parts by mass with respect to 100 parts by mass of the component (A). is there. If the blending amount is too small, it may not be possible to impart good thermal performance and reliability to the cured product of the composition, and if the blending amount is too large, the formation of a heat conduction path of the silver powder is hindered. However, the thermal performance of the cured product of the composition may decrease.
  • the thermally conductive silicone composition of the present invention may contain the following components as arbitrary components in addition to the above components (A) to (E).
  • curing reaction control agent In the composition of the present invention, in addition to the above-mentioned components (A) to (E), as an arbitrary component, all conventionally known curing reaction control agents that are said to have a curing suppressing effect on the addition reaction catalyst are used. Can be used. Examples of such compounds include phosphorus-containing compounds such as triphenylphosphine, nitrogen-containing compounds such as tributylamine, tetramethylethylenediamine and benzotriazole, sulfur-containing compounds, and acetylene compounds such as 1-ethynyl-1-cyclohexanol. , Triallyl isocyanuric acid, hydroperoxy compounds, maleic acid derivatives and the like.
  • phosphorus-containing compounds such as triphenylphosphine
  • nitrogen-containing compounds such as tributylamine, tetramethylethylenediamine and benzotriazole
  • sulfur-containing compounds sulfur-containing compounds
  • acetylene compounds such as 1-ethynyl-1
  • the degree of the curing delay effect of the curing reaction control agent varies greatly depending on the chemical structure of the curing reaction control agent. Therefore, the blending amount of the curing reaction control agent should be adjusted to an optimum amount for each of the curing reaction control agents to be used, and such adjustment can be easily performed by a method well known to those skilled in the art. In general, if the blending amount is too small, the long-term storage stability of the composition of the present invention cannot be obtained at room temperature, and conversely, if the blending amount is too large, curing of the composition is inhibited.
  • Examples of the inorganic compound powder and organic compound material that can be blended other than the component (D) and the component (E) are Metal powders such as aluminum, gold, copper, nickel, indium, gallium, and metallic silicon; Diamond powder; Carbon materials such as carbon fiber; Metal oxide powders such as zinc oxide, titanium oxide, magnesium oxide, alumina, iron oxide, silicon dioxide (fumed silica, crystalline silica, precipitated silica, etc.); Metal hydroxide powder such as aluminum hydroxide; Nitride powder such as boron nitride and aluminum nitride; Carbonates such as magnesium carbonate, calcium carbonate, zinc carbonate; Hollow filler; silsesquioxane; layered mica; diatomaceous earth; glass fiber; silicone rubber powder; silicone resin powder and the like.
  • Metal powders such as aluminum, gold, copper, nickel, indium, gallium, and metallic silicon
  • Diamond powder Carbon materials such as carbon fiber
  • Metal oxide powders such as zinc oxide, titanium oxide, magnesium oxide, alumina, iron oxide
  • inorganic compound powder and organic compound material having high thermal conductivity include aluminum powder, zinc oxide powder, titanium oxide powder, magnesium oxide powder, alumina powder, aluminum hydroxide powder, boron nitride powder, aluminum nitride powder, diamond powder, and gold.
  • examples include powder, copper powder, nickel powder, indium powder, gallium powder, metallic silicon powder, silicon dioxide powder, and carbon fiber. These may be used alone or in combination of two or more.
  • the surfaces of these inorganic compound powders and organic compound materials may be hydrophobized with organosilane, organosilazane, organopolysiloxane, organic fluorine compounds, etc., if necessary.
  • the average particle size of the inorganic compound powder and the organic compound material is preferably 0.5 to 100 ⁇ m, preferably 1 to 50 ⁇ m, because the filling rate into the obtained composition increases when the average particle size is 0.5 ⁇ m or more and 100 ⁇ m or less. More preferred.
  • the filling rate into the obtained composition increases, so that the range of 10 to 500 ⁇ m is preferable, and the range of 30 to 300 ⁇ m is more preferable.
  • the fluidity of the composition is high and the handleability of the composition is improved. It is preferably 1 to 3,000 parts by mass, more preferably 5 to 2,000 parts by mass.
  • an organopolysiloxane containing one hydrogen atom or alkenyl group bonded to a silicon atom in one molecule a hydrogen atom bonded to a silicon atom and an alkenyl. It may contain an organopolysiloxane containing neither of the groups, an organic solvent, a heat resistance imparting agent, a flame retardant imparting agent, a plasticizing agent, a thixotropy imparting agent, a dye, an antifungal agent and the like.
  • the method for producing the silicone composition of the present invention may follow a conventionally known method for producing a silicone composition, and is not particularly limited.
  • the above components (A) to (E) and, if necessary, other components can be added to Trimix, Twinmix, Planetary Mixer (all mixers manufactured by Inoue Seisakusho Co., Ltd., registered trademark), Ultramixer (Mizuho). It can be manufactured by mixing with a mixer such as a mixer manufactured by Kogyo Co., Ltd. (registered trademark) or Hibis Dispermix (mixer manufactured by Primix Corporation, registered trademark) for 10 minutes to 4 hours. Further, if necessary, the mixture may be mixed while heating at a temperature in the range of 50 to 200 ° C.
  • the thermally conductive silicone composition of the present invention preferably has an absolute viscosity measured at 25 ° C. of 10 to 600 Pa ⁇ s, more preferably 15 to 500 Pa ⁇ s, and preferably 15 to 400 Pa ⁇ s. Is more preferable.
  • the absolute viscosity can be obtained by preparing each component in the above-mentioned blending amount.
  • the absolute viscosity is the result of measurement using, for example, a model number PC-1TL (10 rpm) manufactured by Malcolm Co., Ltd.
  • the thermally conductive silicone composition of the present invention is cured by heating the thermally conductive silicone composition obtained as described above to 80 ° C. or higher under a pressure of 0.01 MPa or higher.
  • the properties of the cured product thus obtained are not limited, and examples thereof include gel-like, low-hardness rubber-like, and high-hardness rubber-like.
  • a cured product of the heat conductive silicone composition of the present invention is interposed between the surface of a heat-generating electronic component and a radiator. It is preferable to interpose a cured product of the thermally conductive silicone composition of the present invention in a thickness of 10 to 500 ⁇ m. A typical structure is shown in FIG. 1, but the present invention is not limited thereto.
  • a cured product 3 of the heat conductive silicone composition of the present invention is interposed between a heat-generating electronic component 2 such as a CPU mounted on a substrate 1 and a radiator 4 such as a lid. The heat generated by the heat-generating electronic component 2 is transferred to the heat radiating body 4 via the cured product 3 and radiated to the outside.
  • the thermally conductive silicone composition of the present invention is heated to 80 ° C. or higher in a state where a pressure of 0.01 MPa or higher is applied between a heat-generating electronic component and a radiator. Has a step to do.
  • the applied pressure is preferably 0.05 MPa to 100 MPa, more preferably 0.1 MPa to 100 MPa.
  • the heating temperature is preferably 100 ° C. to 300 ° C., more preferably 120 ° C. to 300 ° C., and even more preferably 140 ° C. to 300 ° C.
  • Viscosity, thermal resistance and Asker C hardness were measured as follows.
  • Component (C) Solution of component (A) of platinum-divinyltetramethyldisiloxane complex (containing 1% by mass as platinum atom)
  • D Component (D-1): Silver powder having a tap density of 6.6 g / cm 3 , a specific surface area of 0.28 m 2 / g, and an aspect ratio of 8 (D-2): Tap density of 6.0 g / Silver powder (D-3) with cm 3 , specific surface area 0.91 m 2 / g, aspect ratio 3: tap density 3.0 g / cm 3 , specific surface area 2.0 m 2 / g, aspect ratio 30 Silver powder
  • Comparative example Scales with an average particle size of 2 ⁇ m
  • Natural graphite (E-7) (Comparative example): Scale-like natural graphite with an average particle size of 55 ⁇ m
  • Examples 1 to 14 and [Comparative Examples 1 to 6]
  • the compositions shown in Tables 1 to 3 below were mixed as follows to obtain the compositions of Examples 1 to 14 and Comparative Examples 1 to 6. That is, take the components (A) and (D) in a 5 liter planetary mixer (manufactured by Inoue Seisakusho Co., Ltd.), add the components (C), (E) and (F), and mix at 25 ° C. for 1.5 hours. did. Next, the component (B) was added and mixed so as to be uniform, and the above test was performed on the obtained composition. The results are shown in Tables 1 to 3.
  • the unit of the blending amount of the components (A) to (F) is a mass part.
  • the unit of the blending amount of the components (A) to (F) is a mass part.
  • the unit of the blending amount of the components (A) to (F) is a mass part.
  • the absolute viscosities of the thermally conductive silicone compositions of Examples 1 to 14 were in an appropriate range, and their handleability was excellent.
  • the thermal resistance of the cured product obtained by pressurizing and heating these thermally conductive silicone compositions was small, and these cured products had high heat dissipation. Further, the hardness of these cured products was not too high, and these cured products were highly reliable as they were interposed between the heat-generating electronic component and the radiator.
  • the amount of silver powder blended was too small.
  • the thermal resistance of the cured product of the thermally conductive silicone composition of Comparative Example 1 was large, and the heat dissipation of this cured product was low.
  • the hardness of the cured product of the heat conductive silicone composition of Comparative Example 2 in which the amount of silver powder is too large is high, and this cured product is unreliable as it is interposed between the heat-generating electronic component and the radiator. there were.
  • the average particle size of graphite was too large.
  • the thermal resistance of the cured product of the thermally conductive silicone composition of Comparative Example 6 was large, and the heat dissipation of this cured product was low.
  • the present invention is not limited to the above embodiment.
  • the above-described embodiment is an example, and any object having substantially the same configuration as the technical idea described in the claims of the present invention and exhibiting the same effect and effect is the present invention. Is included in the technical scope of.
  • Substrate 1 ... Substrate, 2 ... Heat-generating electronic component (CPU), 3 ... A cured product layer of a heat conductive silicone composition, 4 ... A radiator (lid).
  • CPU Central Processing Unit

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