WO2023276846A1 - 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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WO2023276846A1
WO2023276846A1 PCT/JP2022/025063 JP2022025063W WO2023276846A1 WO 2023276846 A1 WO2023276846 A1 WO 2023276846A1 JP 2022025063 W JP2022025063 W JP 2022025063W WO 2023276846 A1 WO2023276846 A1 WO 2023276846A1
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component
group
conductive silicone
silicone composition
heat
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French (fr)
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翔太 秋場
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Shin Etsu Chemical Co Ltd
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Priority to US18/575,346 priority Critical patent/US20250223444A1/en
Priority to JP2023531878A priority patent/JP7650612B2/ja
Priority to KR1020247003492A priority patent/KR20240028463A/ko
Priority to EP22832993.4A priority patent/EP4365238A4/en
Priority to CN202280046667.8A priority patent/CN117580912A/zh
Publication of WO2023276846A1 publication Critical patent/WO2023276846A1/ja
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    • 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
    • C08L83/06—Polysiloxanes containing silicon bound to oxygen-containing groups
    • H—ELECTRICITY
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    • 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
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    • 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
    • H—ELECTRICITY
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    • H10W40/00—Arrangements for thermal protection or thermal control
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    • C—CHEMISTRY; METALLURGY
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    • 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
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    • C08G77/12—Polysiloxanes containing silicon bound to hydrogen
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    • 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
    • C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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    • C08K2003/0806—Silver
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/006—Additives being defined by their surface area
    • 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
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K2201/016—Additives defined by their aspect ratio
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10W—GENERIC PACKAGES, INTERCONNECTIONS, CONNECTORS OR OTHER CONSTRUCTIONAL DETAILS OF DEVICES COVERED BY CLASS H10
    • H10W40/00—Arrangements for thermal protection or thermal control
    • H10W40/70—Fillings or auxiliary members in containers or in encapsulations for thermal protection or control

Definitions

  • the present invention relates to a silicone composition with excellent thermal conductivity, a semiconductor device, and a method for manufacturing the same.
  • Patent Document 1 describes a silicone grease composition in which a specific organopolysiloxane is blended with spherical hexagonal aluminum nitride powder having a certain particle size range.
  • Patent Document 2 describes a thermally conductive silicone grease in which an aluminum nitride powder having a fine particle size and an aluminum nitride powder having a coarse particle size are combined.
  • Patent Document 4 discloses a thermally conductive grease composition using aluminum nitride powder surface-treated with an organosilane. ing.
  • Patent Document 5 discloses a thermally conductive silicone composition obtained by adding diamond, zinc oxide and a dispersant to a silicone resin.
  • Patent Document 6 discloses a thermally conductive grease composition in which a base oil such as silicone oil and metal aluminum powder are mixed. ing.
  • Patent Document 8 discloses Japanese Patent No. 3130193, Japanese Patent No. 3677671, etc., which use silver powder with high thermal conductivity as a filler.
  • JP-A-2-153995 JP-A-3-14873 JP-A-10-110179 JP-A-2000-63872 JP-A-2002-30217 JP-A-2000-63873 JP 2008-222776 A Japanese Patent No. 3130193 Japanese Patent No. 3677671
  • an object of the present invention is to provide a thermally conductive silicone composition that exhibits a good heat dissipation effect.
  • the present inventors have found that a silver powder having a specific tap density, specific surface area and aspect ratio and a spherical silver powder having a specific particle size are incorporated into a specific organopolysiloxane.
  • the inventors have found that the cured product of the mixed composition has extremely excellent thermal conductivity, and completed the present invention. That is, the present invention provides the following thermally conductive silicone composition and the like.
  • a thermally conductive silicone composition containing the following components (A), (B), (C), (D) and (E).
  • (A) Organopolysiloxane having a kinematic viscosity at 25° C. of 10 to 100,000 mm 2 /s and containing at least two silicon-bonded alkenyl groups per molecule: 100 parts by mass
  • E) An average particle size of 0.5 to 100 ⁇ m, a tap density of 4.0 g/cm 3 or more, and a specific
  • ⁇ 3> A cured product of the thermally conductive silicone composition according to ⁇ 1> or ⁇ 2>.
  • a semiconductor device comprising a heat-generating electronic component and a heat radiator, wherein the cured thermally conductive silicone composition according to ⁇ 3> is interposed between the heat-generating electronic component and the heat radiator.
  • a semiconductor device characterized by: ⁇ 5> A step of heating the thermally conductive silicone composition according to ⁇ 1> or ⁇ 2> to 80° C. or higher under a pressure of 0.01 MPa or higher between the heat-generating electronic component and the radiator.
  • a method of manufacturing a semiconductor device comprising:
  • the cured product of the thermally conductive silicone composition of the present invention has excellent thermal conductivity and is therefore useful for semiconductor devices.
  • FIG. 1 is a schematic vertical cross-sectional view showing one example of a semiconductor device of the present invention
  • thermally conductive silicone composition of the present invention will be detailed below.
  • Component (A) is the base polymer of the composition of the present invention and contains at least two silicon-bonded alkenyl groups per molecule.
  • the molecular structure of component (A) includes, for example, a linear structure and a cyclic structure. These structures may have branches, but the main chain basically consists of repeating diorganosiloxane units. A linear diorganopolysiloxane in which both ends of the molecular chain are blocked with triorganosiloxy groups is preferred.
  • Component (A) has a kinematic viscosity at 25° C. of 10 to 100,000 mm 2 /s, preferably 100 to 50,000 mm 2 /s. If it is less than 10 mm 2 /s, oil bleeds easily when blended in the composition, and if it is more than 100,000 mm 2 /s, the absolute viscosity of the composition when blended in the composition increases, resulting in poor handleability. descend.
  • the kinematic viscosity of the component (A) organopolysiloxane described in this specification is the value at 25° C. measured with an Ostwald viscometer.
  • the silicon-bonded alkenyl group in component (A) preferably has 2 to 8 carbon atoms, more preferably 2 to 8 carbon atoms, such as vinyl group, allyl group, butenyl group, pentenyl group, hexenyl group and heptenyl group. are 2 to 4, and a vinyl group is particularly preferred.
  • the organopolysiloxane of component (A) has a linear structure, it suffices if it contains two or more alkenyl groups bonded to silicon atoms in one molecule, and the alkenyl groups are the ends of the molecular chain and Only one of the non-terminal moieties may be bonded to the silicon atom, or both may be bonded to the silicon atom.
  • Silicon-bonded organic groups other than alkenyl groups in component (A) include, for example, alkyl groups, particularly methyl, ethyl, propyl, ptyl, pentyl, hexyl, cyclohexyl, and heptyl groups.
  • Alkyl groups having 1 to 10 carbon atoms such as; Aryl groups, particularly aryl groups having 6 to 14 carbon atoms such as phenyl, tolyl, xylyl and naphthyl groups; Aralkyl groups, particularly benzyl and phenethyl groups aralkyl groups having 7 to 14 carbon atoms such as; halogenated alkyl groups, particularly halogenated groups having 1 to 3 carbon atoms such as chloromethyl group, 3-chloropropyl group and 3,3,3-trifluoropropyl group Examples include unsubstituted or halogen-substituted monovalent hydrocarbon groups such as alkyl groups, with methyl groups and phenyl groups being particularly preferred.
  • component (A) examples include dimethylsiloxane-methylvinylsiloxane copolymer with trimethylsiloxy group-blocked at both molecular chain ends, methylvinylpolysiloxane with trimethylsiloxy group-blocked at both molecular chain ends, and dimethyl with trimethylsiloxy group-blocked at both molecular chain ends.
  • 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, xylyl group and naphthyl group; groups; aralkyl groups such as benzyl group and phenethyl group; and halogenated alkyl groups such as chloromethyl group, 3-chloropropyl group and 3,3,3-trifluoropropyl group.
  • R 2 in the above formula examples include vinyl group, allyl group, butenyl group, pentenyl group, hexenyl group and heptenyl group.
  • the organohydrogenpolysiloxane of component (B) should have at least two silicon-bonded hydrogen atoms (hydrosilyl groups or SiH groups) per molecule, and the molecular structure is not particularly limited.
  • various conventionally known organohydrogenpolysiloxanes such as linear, cyclic, branched, and three-dimensional network structures (resinous) can be used.
  • the component (B) organohydrogenpolysiloxane has 2 or more, preferably 3 or more (usually about 3 to 500, preferably 3 to 200, more preferably about 3 to 100) per molecule. It has a hydrogen atom (hydrosilyl group or SiH group) bonded to a silicon atom.
  • these SiH groups may be located at either the molecular chain terminal or the non-molecular chain terminal, or may be located at both of them. may be
  • the number of silicon atoms in one molecule of component (B) is preferably about 2 to 1,000, more preferably about 3 to 300, still more preferably about 4 to 150.
  • the kinematic viscosity of component (B) at 25° C. is preferably 10 to 100,000 mm 2 /s, more preferably 20 to 50,000 mm 2 /s.
  • the kinematic viscosity of the component (B) organopolysiloxane described in this specification is the value at 25° C. measured with an Ostwald viscometer.
  • component (B) for example, an organohydrogenpolysiloxane represented by the following average compositional formula (1) is used.
  • R 3 is an unsubstituted or substituted monovalent hydrocarbon group bonded to a silicon atom, preferably having 1 to 14 carbon atoms, more preferably 1 to 10 carbon atoms, excluding an aliphatic unsaturated group and 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 ⁇ 2.0, 0.01 ⁇ b ⁇ 1.0, and a positive number satisfying 1.0 ⁇ a + b ⁇ 2.5)
  • R 3 examples 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, Alkyl groups such as a decyl group; Aryl groups such as a phenyl group, a tolyl group, a xylyl group and a naphthyl group; Aralkyl groups such as a benzyl group, a phenylethyl group and a phenylpropyl group; Groups entirely substituted with halogen atoms such as fluorine, bromine and chlorine, such as chloromethyl group, 3-chloropropyl group, bromoethyl group, 3,3,3-trifluoropropyl group and the like, preferably alkyl group , an
  • (B) component can be obtained by a known manufacturing method.
  • 1,3,5,7-tetramethyl-1,3,5,7-tetrahydrocyclotetrasiloxane (in some cases, the cyclotetrasiloxane and octamethylcyclotetrasiloxane mixture) and a siloxane compound that serves as a source of terminal groups such as hexamethyldisiloxane and 1,3-dihydro-1,1,3,3-tetramethyldisiloxane, or octamethylcyclotetrasiloxane and 1,3 -Dihydro-1,1,3,3-tetramethyldisiloxane is equilibrated at a temperature of about -10 to +40°C in the presence of a catalyst such as sulfuric acid, trifluoromethanesulfonic acid, or methanesulfonic acid. be done.
  • a catalyst such as sulfuric acid, trifluoromethanesulfonic acid
  • component (B) examples include 1,1,3,3-tetramethyldisiloxane, 1,3,5,7-tetramethylcyclotetrasiloxane, tris(dimethylhydrogensiloxy)methylsilane, tris(dimethylhydrogensiloxy) gensiloxy)phenylsilane, trimethylsiloxy group-blocked methylhydrogenpolysiloxane at both molecular chain ends, dimethylsiloxane-methylhydrogensiloxane copolymer blocked at both molecular chain ends with trimethylsiloxy groups, dimethylsiloxane-blocked at both molecular chain ends with trimethylsiloxy groups Methylhydrogensiloxane/methylphenylsiloxane copolymer, dimethylpolysiloxane with dimethylhydrogensiloxy group-blocked at both molecular chain ends, dimethylpolysiloxane/methylhydrogensiloxane copolymer with dimethylhydrogensil
  • the amount of component (B) is such that the amount of silicon-bonded hydrogen atoms (SiH groups) in component (B) is 0.8 to 6, preferably 1, per alkenyl group in the entire composition.
  • the amount is within the range of 0.5 to 3.0.
  • the ratio of silicon-bonded alkenyl groups in component (A) to alkenyl groups present in the entire composition is preferably 50 to 100 mol %, more preferably 80 to 100 mol %.
  • the amount of SiH groups in component (B) per silicon-bonded alkenyl group in component (A) is The amount is in the range of 0.5 to 10, preferably 1.0 to 8.0. If the amount of component (B) is too small, the adhesion to the substrate may be poor, and if it is too large, heat dissipation may be reduced.
  • Component (C) Any catalyst can be used as the hydrosilylation reaction catalyst of component (C) as long as it promotes the addition reaction between the alkenyl group in component (A) and the SiH group in component (B).
  • platinum-based catalysts such as chloroplatinic acid, alcohol-modified chloroplatinic acid, chloroplatinic acid and olefins, vinylsiloxane or coordination compounds with acetylene compounds; palladium-based catalysts such as tetrakis (triphenylphosphine) palladium; chlorotris ( A rhodium-based catalyst such as triphenylphosphine)rhodium is used as the component (C), and a platinum-based catalyst such as a platinum-divinyltetramethyldisiloxane complex is particularly preferred.
  • the amount of component (C) to be blended is not particularly limited as long as it is an effective amount as a hydrosilylation reaction catalyst. preferably 0.1 to 2,000 ppm, more preferably 1 to 1,500 ppm. When the amount added is within this range, the addition reaction is sufficiently accelerated, the composition is sufficiently cured, and it is economically advantageous.
  • the type of metal catalyst is not particularly limited as long as it is a metal having effective activity as a catalyst for hydrosilylation reaction, but platinum or the like having activity to split hydrogen gas into atoms is useful.
  • 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 2.0 to 50.0. is. If the tap density of the component (D) silver powder is less than 3.0 g/cm 3 , the filling rate of the component (D) into the composition cannot be increased, resulting in an increase in the viscosity of the composition and poor workability.
  • the range of 3.0 g/cm 3 to 10.0 g/cm 3 is preferable, the range of 4.5 g/cm 3 to 10.0 g/cm 3 is more preferable, and the range of 6.0 g/cm 3 to 10.0 g/cm 3 is more preferable. /cm 3 range is more preferred. If the specific surface area of the component (D) silver powder is greater than 2.0 m 2 /g, the filling rate of the component (D) into the composition cannot be increased, and the viscosity of the composition increases, resulting in poor workability.
  • the range of 0.08 m 2 /g to 2.0 m 2 /g is preferable, the range of 0.08 m 2 /g to 1.0 m 2 /g is more preferable, and the range of 0.08 m 2 /g to 0.5 m 2 is preferable. /g range is more preferred.
  • the tap density described in this specification is obtained by weighing 100 g of silver powder, gently dropping the silver powder into a 100 ml graduated cylinder with a funnel, placing the cylinder on a tap density measuring instrument, dropping the distance of 20 mm, 60 times / It is a value calculated from the volume of silver powder that has been dropped and compressed 600 times per minute.
  • the silver powder of component (D) has an aspect ratio of 2.0 to 50.0, preferably 3.0 to 30.0, and more preferably 3.0 to 20.0. .
  • the aspect ratio refers to the ratio of the major axis to the minor axis of a particle (major axis/minor axis).
  • a measuring method for example, an electron microscope photograph of the particles is taken, and the long and short diameters of the particles are measured from the photograph, and the calculation can be performed.
  • the particle size can be measured by an electron micrograph taken from the top, and the larger diameter of the top electron micrograph is measured as the major axis.
  • the minor diameter is the thickness of the particle with respect to the major diameter. Particle thickness cannot be measured in electron micrographs from the top.
  • the thickness of a particle In order to measure the thickness of a particle, when taking an electron micrograph, tilt the sample table on which the particle is placed, and then take the electron micrograph from the top. It is sufficient to calculate the thickness of 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 the major axis to the minor axis (major axis/minor axis) is calculated. Calculations were performed, and the average value was obtained to obtain the aspect ratio.
  • the particle size of the component (D) silver powder is not particularly limited, but the average particle size is preferably in the range of 0.2 to 50 ⁇ m, particularly preferably in the range of 1.0 to 30 ⁇ m.
  • the average particle size described in this specification is obtained by taking 1 to 2 cups of silver powder in a 100 ml beaker with a micro spatula, adding about 60 ml of isopropyl alcohol, dispersing the silver powder for 1 minute with an ultrasonic homogenizer, and then laser diffraction. It is a volume-based volume mean diameter [MV] measured by a particle size analyzer. The measurement time was 30 seconds.
  • the method for producing the silver powder used in the present invention is not particularly limited, but silver powder produced by a reduction method is preferred.
  • the silver powder produced by the above method may be used as it is, or it may be pulverized within the range satisfying the above numerical range.
  • the device is not particularly limited, and known devices such as stamp mill, ball mill, vibration mill, hammer mill, rolling roller, and mortar can be used. Among them, stamp mills, ball mills, vibration mills, and hammer mills are preferred.
  • the blending amount of component (D) is 500 to 3,000 parts by mass with respect to 100 parts by mass of component (A). If the amount of component (D) is less than 500 parts by mass relative to 100 parts by mass of component (A), the cured product of the resulting composition will have poor thermal conductivity. The fluidity of the composition deteriorates, and the handleability of the composition deteriorates.
  • Component (D) is added in an amount of preferably 600 to 2,000 parts by mass, more preferably 700 to 1,500 parts by mass, per 100 parts by mass of component (A).
  • Component (E) has an average particle size of 0.5 to 100 ⁇ m, a tap density of 4.0 g/cm 3 or more, a specific surface area of 1.5 m 2 /g or less, and an aspect ratio of It is a spherical silver powder of less than 2.0. If the average particle diameter of the component (E) spherical silver powder is less than 0.5 ⁇ m, the cured product of the resulting composition will have poor thermal conductivity. If the thickness is larger than 100 ⁇ m, it becomes difficult to form a heat path in the cured product of the resulting composition, resulting in poor thermal conductivity.
  • the filling rate of component (E) in the composition cannot be increased, and the viscosity of the composition increases, resulting in poor workability.
  • the range of 4.0 g/cm 3 to 10.0 g/cm 3 is preferable, the range of 4.5 g/cm 3 to 10.0 g/cm 3 is more preferable, and the range of 6.0 g/cm 3 to 10 g/cm 3 is more preferable.
  • a range of 0.0 g/cm 3 is more preferred.
  • the specific surface area of the component (E) spherical silver powder is greater than 1.5 m 2 /g, the filling rate of the component (E) into the composition cannot be increased, resulting in an increase in the viscosity of the composition and poor workability.
  • the aspect ratio of the component (E) spherical silver powder is less than 2.0, preferably 1.5 or less, more preferably 1.2 or less.
  • the aspect ratio refers to the ratio of the major axis to the minor axis of a particle (long axis/short axis).
  • the measuring method is the same as above.
  • the method for producing the (E) component spherical silver powder is not particularly limited, but the atomization method is preferable.
  • the blending amount of component (E) is 500 to 3,000 parts by mass with respect to 100 parts by mass of component (A). If the amount of component (E) is less than 500 parts by mass with respect to 100 parts by mass of component (A), the cured product of the resulting composition will have poor thermal conductivity. The liquidity of the liquid deteriorates and the handleability deteriorates.
  • Component (E) is added in an amount of preferably 600 to 2,000 parts by mass, more preferably 700 to 1,500 parts by mass, per 100 parts by mass of component (A).
  • the ratio ⁇ / ⁇ of the mass ⁇ of component (D) to the mass ⁇ of component (E) is preferably in the range of 0.1 to 6, more preferably in the range of 0.2 to 5.5, and 0.5 to 5. is more preferred, and the range of 0.8 to 4 is most preferred. If it is such a range, the heat conductivity of the hardened
  • thermally conductive silicone composition of the present invention may contain the following components as optional components in addition to the above components (A) to (E).
  • the composition of the present invention may use a curing reaction control agent having a curing inhibitory effect on the addition reaction catalyst.
  • a curing reaction control agent having a curing inhibitory effect on the addition reaction catalyst.
  • examples of such compounds include phosphorus-containing compounds (triphenylphosphine, etc.), nitrogen-containing compounds (tributylamine, tetramethylethylenediamine, benzotriazole, etc.), sulfur-containing compounds, acetylene compounds (1-ethynyl-1-cyclo hexanol, etc.), triallyl isocyanuric acid, hydroperoxy compounds, maleic acid derivatives, and the like.
  • the degree of curing retardation effect of the curing reaction control agent varies greatly depending on the chemical structure of the curing reaction control agent.
  • the amount of the curing reaction control agent to be added should be adjusted to the optimum amount for each curing reaction control agent used, and such adjustment can be easily carried out by methods well known to those skilled in the art.
  • a curing reaction inhibitor is added to the composition of the present invention, long-term storage stability of the composition of the present invention at room temperature can be obtained. may be hindered.
  • Inorganic compound powders and/or organic compound materials other than components (D) and (E) include aluminum, gold, copper, and nickel. , indium, gallium, palladium, metal powder such as silicon; diamond powder; carbon materials such as carbon fiber, graphene, graphite, carbon nanotube, carbon black; zinc oxide, titanium oxide, magnesium oxide, alumina, iron oxide, silicon dioxide Metal oxide powder such as (fumed silica, crystalline silica, precipitated silica, etc.); Metal hydroxide powder such as aluminum hydroxide; Nitride powder such as boron nitride and aluminum nitride; Magnesium carbonate, calcium carbonate, carbonate carbonate such as zinc; hollow filler; silsesquioxane; layered mica; diatomaceous earth; glass fiber; silicone rubber powder; Among these, those having high thermal conductivity are preferable.
  • Inorganic compound powder and/or organic compound material with 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, and diamond powder. , gold powder, copper powder, carbon powder, nickel powder, indium powder, gallium powder, metallic silicon powder, silicon dioxide powder, carbon fiber, graphene, graphite and carbon nanotubes. These may be used individually by 1 type, or may use 2 or more types together.
  • 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 in the range of 0.5 to 100 ⁇ m, particularly 1 A range of ⁇ 50 ⁇ m is preferred.
  • the fiber length of the carbon fiber is less than 10 ⁇ m or more than 500 ⁇ m, the filling rate in the obtained composition does not increase, so the range of 10 to 500 ⁇ m is preferable, and the range of 30 to 300 ⁇ m is particularly preferable.
  • the total amount of the inorganic compound powder and the organic compound material is more than 3,000 parts by mass with respect to 100 parts by mass of component (A), the flowability of the composition deteriorates and the handleability of the composition deteriorates. .1 to 3,000 parts by weight is preferred, and 1 to 2,000 parts by weight is particularly preferred.
  • composition of the present invention may include, as other optional components within a range that does not impair the object of the present invention, for example, an organopoly Siloxanes, organopolysiloxanes containing neither silicon-bonded hydrogen atoms nor alkenyl groups, organic solvents, heat resistance imparting agents, flame retardant imparting agents, plasticizers, thixotropy imparting agents, dyes, antifungal agents, etc. may be included.
  • the method for manufacturing the thermally conductive silicone composition of the present invention is not particularly limited as long as it follows a conventionally known method for manufacturing a silicone composition.
  • the above components (A) to (E) and, if necessary, other components may be added to Trimix, Twinmix, Planetary Mixer (all are mixers manufactured by Inoue Seisakusho Co., Ltd., registered trademarks), Ultra Mixer (Mizuho It can be produced by mixing for 10 minutes to 4 hours with a mixer such as a mixer manufactured by Kogyo Co., Ltd., Hivis Dispermix (mixer manufactured by Primix Co., Ltd., registered trademark).
  • mixing may be performed while heating at a temperature in the range of 30 to 200°C.
  • the thermally conductive silicone composition of the present invention preferably has an absolute viscosity measured at 25°C of 10 to 1,000 Pa ⁇ s, more preferably 50 to 700 Pa ⁇ s, and more preferably 80 to 600 Pa ⁇ s. Some are even more preferred. When the absolute viscosity is within the above range, a good grease can be provided and workability is also excellent.
  • the absolute viscosity can be obtained by adjusting the blending amount of each component as described above. The above absolute viscosity can be measured, for example, using Model No. PC-1TL (10 rpm) manufactured by Malcom 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, but examples thereof include gel-like, low-hardness rubber-like, and high-hardness rubber-like properties.
  • the semiconductor device of the present invention is characterized in that the cured product of the thermally conductive silicone composition of the present invention is interposed between the surface of the heat-generating electronic component and the radiator.
  • the cured product of the thermally conductive silicone composition of the present invention is preferably interposed with a thickness of 10 to 200 ⁇ m.
  • FIG. 1 is a schematic longitudinal sectional view showing one example of the semiconductor device of the present invention.
  • a thermally conductive silicone composition layer 3 is interposed, and the thermally conductive silicone composition layer 3 is a cured product of the thermally conductive silicone composition of the present invention.
  • the thermally conductive silicone composition of the present invention is heated to 80° C. or higher under a pressure of 0.01 MPa or higher between a heat-generating electronic component and a radiator.
  • a method of heating is preferred.
  • the applied pressure is preferably 0.01 MPa or more, particularly preferably 0.05 MPa to 100 MPa, further preferably 0.1 MPa to 100 MPa.
  • the heating temperature must be 80°C or higher, preferably 100°C to 300°C, more preferably 120°C to 300°C, still more preferably 140°C to 300°C.
  • kinematic viscosities of components (A) and (B) are values at 25° C. measured with an Ostwald viscometer. Components used in Examples and Comparative Examples are shown below.
  • Component A-1 Dimethylpolysiloxane having both ends blocked with dimethylvinylsilyl groups and having a kinematic viscosity of 600 mm 2 /s at 25°C
  • Component B-1 Organohydrogenpolysiloxane represented by the following formula (kinematic viscosity at 25°C: 30 mm 2 /s)
  • Component C-1 (platinum catalyst): A-1 solution of platinum-divinyltetramethyldisiloxane complex, containing 1 wt% as platinum atoms
  • Component D-1 Silver powder having a tap density of 5.5 g/cm 3 , a specific surface area of 0.8 m 2 /g, an aspect ratio of 8.0 and an average particle size of 2 ⁇ m
  • D-2 a tap density of Silver powder D-3 having a weight of 6.2 g/cm 3 , a specific surface area of 0.5 m 2 /g, an aspect ratio of 13.0 and an average particle size of 4 ⁇ m: a tap density of 9.0 g/cm 3 and a specific surface area of 0 .2 m 2 /g, aspect ratio of 30.0, average particle size of 10 ⁇ m silver powder D-4: tap density of 3.0 g/cm 3 , specific surface area of 2.0 m 2 /g, aspect ratio of 47.0 g/cm 3 .
  • silver powder D-5 tap density of 2.3 g/cm 3 , specific surface area of 1.8 m 2 /g, aspect ratio of 3.0, average particle diameter of 1 ⁇ m
  • Silver powder D-6 comparative example: silver powder having a tap density of 3.3 g/cm 3 , a specific surface area of 3.0 m 2 /g, an aspect ratio of 4.0, and an average particle diameter of 0.1 ⁇ m
  • Spherical silver powder E-5 with a specific surface area of 2.2 m 2 /g and an aspect ratio of 1.6 (comparative example): average particle diameter of 105 ⁇ m, tap density of 5.0 g/cm 3 , specific surface area of 0 .5 m 2 /g, spherical silver powder with an aspect ratio of 1.8
  • Examples 1 to 9 and Comparative Examples 1 to 8 Compositions of Examples 1 to 9 and Comparative Examples 1 to 8 were obtained by mixing as follows with the compositions shown in Tables 1 and 2 below (the numerical value of each component is parts by mass). That is, components (A), (D) and (E) were placed in a 5-liter planetary mixer (manufactured by Inoue Seisakusho Co., Ltd.) and mixed at 25° C. for 1.5 hours. Next, components (C) and (F) were added and mixed at 25°C for 15 minutes. Finally, the component (B) was added and mixed uniformly.
  • Tables 1 and 2 the numerical value of each component is parts by mass. That is, components (A), (D) and (E) were placed in a 5-liter planetary mixer (manufactured by Inoue Seisakusho Co., Ltd.) and mixed at 25° C. for 1.5 hours. Next, components (C) and (F) were added and mixed at 25°C for 15 minutes. Finally, the component (B) was added and mixed

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US18/575,346 US20250223444A1 (en) 2021-07-02 2022-06-23 Thermal conductive silicone composition, semiconductor device, and method for producing same
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KR1020247003492A KR20240028463A (ko) 2021-07-02 2022-06-23 열전도성 실리콘 조성물, 반도체 장치 및 그의 제조 방법
EP22832993.4A EP4365238A4 (en) 2021-07-02 2022-06-23 THERMALLY CONDUCTIVE SILICONE COMPOSITION, SEMICONDUCTOR DEVICE AND METHOD FOR MANUFACTURING SAME
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