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WO2018088417A1 - Composition de silicone thermoconductrice, article durci de celle-ci, et procédé de fabrication associé - Google Patents

Composition de silicone thermoconductrice, article durci de celle-ci, et procédé de fabrication associé Download PDF

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Publication number
WO2018088417A1
WO2018088417A1 PCT/JP2017/040203 JP2017040203W WO2018088417A1 WO 2018088417 A1 WO2018088417 A1 WO 2018088417A1 JP 2017040203 W JP2017040203 W JP 2017040203W WO 2018088417 A1 WO2018088417 A1 WO 2018088417A1
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Prior art keywords
component
group
silicone composition
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conductive silicone
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Japanese (ja)
Inventor
岩田　充弘
也実 細田
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Shin Etsu Chemical Co Ltd
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Shin Etsu Chemical Co Ltd
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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
    • 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
    • C08K3/40—Glass
    • 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
    • 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
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/16—Solid spheres
    • C08K7/18—Solid spheres inorganic
    • 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

Definitions

  • the present invention relates to a silicone composition having excellent thermal conductivity, and particularly when used as a heat radiating member for electronic components, heat-generating electronic components such as power devices, transistors, thyristors, and CPUs (central processing units) are used.
  • the present invention relates to a thermally conductive silicone composition having excellent insulating properties that can be incorporated into an electronic device without being damaged.
  • a heat-generating electronic component such as power devices, transistors, thyristors, and CPUs
  • how to remove heat generated during use is an important issue.
  • a heat-generating electronic component is generally attached to a heat-radiating fin or a metal plate via an electrically insulating heat-dissipating sheet, and the heat is released.
  • Patent Documents 1 to 6 JP-A-2005-162555, JP-A-2003-342021, JP-A-2002-280498, JP-A-2005-209765).
  • the average sphericity, the amount of hydroxyl groups, and the spherical aluminum oxide powder having an average particle diameter of 10 to 50 ⁇ m and the average particle diameter of 0.3 to 1 ⁇ m are specified.
  • a method of a high thermal conductive resin composition in which the mixing ratio and volume ratio of aluminum are defined is disclosed, although there is a description that the average particle size of spherical aluminum oxide powder is 50 ⁇ m at the maximum, the range of the coarse particle size And there is no regulation regarding the content, and there is a problem of insufficient thermal conductivity (Patent Document 5: Japanese Patent No. 5755777).
  • the present invention has been made in view of the above circumstances, and is to provide a thermally conductive silicone composition that is excellent in insulation and thermal conductivity and capable of forming an appropriate thickness, and is particularly suitable as a heat radiating member for electronic components. It is to provide a conductive silicone composition.
  • a silicone composition containing an organopolysiloxane has (B) an average sphericity of 0.8 or more and a hydroxyl group of 30 / nm 2 or less.
  • a thermally conductive silicone that can solve the above-mentioned problems by mixing a specific amount of spherical or irregularly shaped aluminum oxide powder with an average particle size of 0.1 to 5 ⁇ m in a specific ratio, and has good handleability and workability.
  • a composition can be obtained. Further, the heat conductivity at 150 ° C.
  • the heat conductive silicone composition excellent in the heat conductivity in can be obtained. Furthermore, this composition can also mix
  • the present invention provides the following inventions. 1.
  • a thermally conductive silicone composition comprising spherical aluminum oxide powder of 1 to 30% by mass, and (C) spherical or amorphous aluminum oxide powder having an average particle size of 0.1 to 5 ⁇ m,
  • the mixing ratio volume ratio ((B) :( C)) of the component (B) and the component (C) is 5: 5 to 9.5: 0.5, and the total amount of the component (B) and the component (C) Is 50 volume% or more and less than 80 volume% in the composition, and the thermal conductivity of the composition at 25 ° C. is 1.2 W / m ⁇ K or more and 5.5 W / m or more in the hot disk method according to ISO 22007-2.
  • a thermally conductive silicone composition having a viscosity of less than K and a viscosity of the composition at 25 ° C. of 5 to 800 Pa ⁇ s when measured with a spiral viscometer at a rotation speed of 10 rpm.
  • the component (D) is represented by the following general formula (1) -SiR 1 a (OR 2 ) 3-a (1) Wherein R 1 is independently an unsubstituted or substituted monovalent hydrocarbon group, R 2 is independently an alkyl group, an alkoxyalkyl group, an alkenyl group or an acyl group, and a is 0, 1 or 2 is there.) 3.
  • the thermally conductive silicone composition according to 2 which is an organopolysiloxane containing at least one silyl group represented by the formula: 1 in a molecule and having a viscosity at 25 ° C. of 0.01 to 30 Pa ⁇ s. 4). Further, (E) a spherical glass bead or amorphous glass having a maximum central particle diameter of 150 ⁇ m or more and a SiO 2 content of 50% by mass or more is contained in an amount of 10% by mass or less based on the total amount of the composition.
  • the heat conductive silicone composition in any one of. 5). 5.
  • Thermally conductive silicone composition 7).
  • Component (B) and Component (C), comprising the step of mixing spherical aluminum oxide powder of 1 to 30% by mass and (C) spherical or amorphous aluminum oxide powder having an average particle size of 0.1 to 5 ⁇ m
  • the mixing ratio volume ratio ((B) :( C)) is 5: 5 to 9.5: 0.5
  • the total amount of the component (B) and the component (C) is 50% by volume or more and 80% by volume. %
  • the thermal conductivity of the composition at 25 ° C. is 1.2 W / m ⁇ K or more and less than 5.5 W / m ⁇ K in the hot disk method according to ISO 22007-2
  • the viscosity of the composition at 25 ° C. is a spiral viscometer A method for producing a thermally conductive silicone composition having a speed of 5 to 800 Pa ⁇ s at the time of measurement at 10 rpm.
  • thermoly conductive silicone composition that is excellent in insulation and thermal conductivity and can form an appropriate thickness.
  • the “thermally conductive silicone composition” is sometimes abbreviated as “silicone composition”.
  • the organopolysiloxane of component (A) is the main ingredient of the silicone composition of the present invention.
  • Examples of the group bonded to the silicon atom in the organopolysiloxane include methyl, ethyl, propyl, butyl, pentyl, hexyl, heptyl, octyl, nonyl, decyl, and undecyl.
  • dodecyl group dodecyl group, tridecyl group, tetradecyl group, pentadecyl group, hexadecyl group, heptadecyl group, octadecyl group, nonadecyl group, eicosyl group and other linear alkyl groups; isopropyl group, tertiary butyl group, isobutyl group, 2-methyl Branched alkyl groups such as undecyl group and 1-hexylheptyl group; cyclic alkyl groups such as cyclopentyl group, cyclohexyl group and cyclododecyl group; alkenyl groups such as vinyl group, allyl group, butenyl group, pentenyl group and hexenyl group ; Aryl such as phenyl, tolyl, xylyl, etc.
  • Aralkyl groups such as benzyl group, phenethyl group and 2- (2,4,6-trimethylphenyl) propyl group; halogenated alkyl groups such as 3,3,3-trifluoropropyl group and 3-chloropropyl group;
  • An alkyl group, an alkenyl group, and an aryl group are preferable, and a methyl group, a vinyl group, and a phenyl group are particularly preferable.
  • the viscosity of the organopolysiloxane at 25 ° C. is not limited, but is preferably in the range of 20 to 100,000 mPa ⁇ s, more preferably 50 to 100,000 mPa ⁇ s, and still more preferably 50 to 50,000 mPa ⁇ s. 100 to 50,000 mPa ⁇ s is particularly preferable. If the viscosity is too low, the physical properties of the silicone composition may be significantly reduced, and if the viscosity is too high, the handling workability of the silicone composition may be significantly reduced.
  • the molecular structure of the organopolysiloxane is not limited, and examples thereof include linear, branched, partially branched linear, and dendritic (dendrimer), preferably linear and partially branched. Linear.
  • examples of such an organopolysiloxane include a single polymer having these molecular structures, a copolymer having these molecular structures, or a mixture of these polymers.
  • organopolysiloxane examples include molecular chain both ends dimethylvinylsiloxy group-capped dimethylpolysiloxane, molecular chain both ends methylphenylvinylsiloxy group-capped dimethylpolysiloxane, molecular chain both ends dimethylvinylsiloxy group-capped dimethylsiloxane, Methylphenylsiloxane copolymer, dimethylvinylsiloxy group-capped dimethylvinylsiloxy group-capped dimethylsiloxane / methylvinylsiloxane copolymer, trimethylsiloxy group-capped dimethylsiloxane / methylvinylsiloxane copolymer, dimethylvinylsiloxy group-capped methyl (3) , 3,3-trifluoropropyl) polysiloxane, silanol group-blocked dimethylsiloxane / methylvinylsiloxane copolymer
  • the component (A) is (AI) an organopolysiloxane having an average of 0.1 or more silicon-bonded alkenyl groups in one molecule.
  • An organopolysiloxane having an average of 0.5 or more silicon atom-bonded alkenyl groups in one molecule is more preferred, and an organopolysiloxane having an average of 0.8 or more silicon atom-bonded alkenyl groups in one molecule. More preferred is siloxane. This is because when the average value of silicon-bonded alkenyl groups in one molecule is less than the lower limit of the above range, the resulting silicone composition tends not to be cured sufficiently.
  • Examples of the silicon atom-bonded alkenyl group in this organopolysiloxane include the same alkenyl groups as described above, preferably a vinyl group.
  • Examples of the group bonded to the silicon atom other than the alkenyl group in the organopolysiloxane include the same linear alkyl group, branched alkyl group, cyclic alkyl group, aryl group, aralkyl group, halogen as described above.
  • An alkyl group is exemplified, and an alkyl group and an aryl group are preferable, and a methyl group and a phenyl group are particularly preferable.
  • the component (A) is (A-II) an organopolysiloxane having at least two silanol groups or silicon atom-bonded hydrolyzable groups in one molecule.
  • the silicon atom-bonded hydrolyzable group in this organopolysiloxane include alkoxy groups such as methoxy group, ethoxy group and propoxy group; vinyloxy group, propenoxy group, isopropenoxy group, 1-ethyl-2-methylvinyloxy group Alkenoxy groups such as methoxyethoxy groups, ethoxyethoxy groups, methoxypropoxy groups, etc .; Acyloxy groups such as acetoxy groups, octanoyloxy groups, etc .; Ketoxime groups such as dimethyl ketoxime groups, methylethyl ketoxime groups; And amino groups such as diethylamino group and butylamino group; aminoxy groups such as dimethylaminoxy group and
  • the same linear alkyl group, branched alkyl group, and cyclic alkyl group as described above are used.
  • Alkenyl group, aryl group, aralkyl group, and halogenated alkyl group are used.
  • the organopolysiloxane of component (A) is not limited, but preferably (A-III) at least one silicon atom in one molecule Organopolysiloxane having a bonded alkenyl group.
  • the group bonded to the silicon atom in the organopolysiloxane include the same linear alkyl group, branched alkyl group, cyclic alkyl group, alkenyl group, aryl group, aralkyl group, and halogenated alkyl group as described above.
  • an alkyl group, an alkenyl group, and an aryl group are preferable, and a methyl group, a vinyl group, and a phenyl group are more preferable.
  • the blending amount of the component (A) is preferably 2.0 to 20.0% by mass, more preferably 2.0 to 19.0% by mass in the silicone composition.
  • Component (B) is a ratio of coarse particles having an average sphericity of 0.8 or more, a hydroxyl group of 30 particles / nm 2 or less, an average particle size of 10 ⁇ m or more and less than 50 ⁇ m, and a laser diffraction type particle size distribution of 96 to 150 ⁇ m.
  • the crystal structure of the aluminum oxide powder may be either a single crystal or a polycrystal, but the ⁇ phase is desirable from the viewpoint of high thermal conductivity and the specific gravity is preferably 3.7 or more. If the specific gravity is less than 3.7, the ratio of vacancies and low crystal phases existing inside the particles increases, and it may be difficult to increase the thermal conductivity.
  • the particle size adjustment of the aluminum oxide powder can be performed by classification and mixing operations.
  • the average sphericity is 0.8 or more, and more preferably 0.9 or more. If the average sphericity is less than 0.8, the fluidity may decrease. When the average sphericity is less than 0.8, the contact between the particles becomes remarkable, the unevenness of the sheet surface becomes large, the interface thermal resistance increases, and the thermal conductivity tends to deteriorate. Although an upper limit is not specifically limited, The closer it is to a sphere (average sphericity 1), the better.
  • the average sphericity in the present invention can be measured as follows by taking a particle image taken with a scanning electron microscope into an image analyzer, for example, “JSM-7500F” manufactured by JEOL. That is, the projected area (X) and the perimeter (Z) of the particles are measured from the photograph. When the area of a perfect circle corresponding to the perimeter (Z) is (Y), the sphericity of the particle can be displayed as X / Y.
  • the number of hydroxyl groups is 30 / nm 2 or less, and preferably 25 / nm 2 or less.
  • the lower limit is not particularly limited, but may be 5 / nm 2 .
  • the number of hydroxyl groups can be measured by a Karl Fischer coulometric titration method, for example, “Trace Moisture Analyzer CA-100” manufactured by Mitsubishi Chemical Corporation. Specifically, 0.3 to 1.0 g of a sample is put in a moisture vaporizer, and heated with an electric heater while supplying dehydrated argon gas as a carrier gas. In the Karl Fischer coulometric method, water generated at a temperature exceeding 200 ° C. and up to 900 ° C. is defined as the surface hydroxyl group amount. The concentration of the surface hydroxyl group is calculated from the measured water content and specific surface area.
  • the average particle size is 10 ⁇ m or more and less than 50 ⁇ m, preferably 20 ⁇ m or more and less than 50 ⁇ m.
  • the average particle size is less than 10 ⁇ m, the contact between the particles is reduced, and the thermal conductivity may be deteriorated due to an increase in the interparticle contact thermal resistance.
  • it is 50 ⁇ m or more, the unevenness of the sheet surface becomes large, the interfacial thermal resistance increases, and the thermal conductivity may deteriorate.
  • the proportion of coarse particles having a laser diffraction type particle size distribution of 96 to 150 ⁇ m is 0.1 to 30% by mass, more preferably 0.1 to 10% by mass, based on the entire component (B).
  • desired thickness and high thermal conductivity can be compatible.
  • the ratio of the coarse particles of 96 to 150 ⁇ m is less than 0.1% by mass of the whole, the desired thickness is not achieved at 100 to 150 ⁇ m, and high thermal conductivity cannot be achieved, and when it is 30% by mass or more, although the desired thickness of 100 to 150 ⁇ m can be achieved, the filling property of the component (B) tends to deteriorate.
  • the average particle size can be measured using a laser diffraction particle size distribution measuring device, for example, “Laser diffraction particle size distribution measuring device SALD-2300” manufactured by Shimadzu Corporation.
  • a laser diffraction particle size distribution measuring device SALD-2300 manufactured by Shimadzu Corporation.
  • SALD-2300 As an evaluation sample, 5 g of 50 cc pure water and a heat conductive powder to be measured are added to a glass beaker and stirred using a spatula, and then subjected to a dispersion treatment for 10 minutes using an ultrasonic cleaner.
  • the powder solution of the thermally conductive material that has been subjected to the dispersion treatment is added dropwise to the sampler portion of the apparatus with a dropper, and waits until the absorbance becomes measurable. The measurement is performed when the absorbance becomes stable in this way.
  • the particle size distribution is calculated from the data of the light intensity distribution of the diffracted / scattered light by the particles detected by the sensor.
  • the average particle size is obtained by multiplying the value of the measured particle size by the relative particle amount (difference%) and dividing by the total relative particle amount (100%).
  • the average particle diameter is the average diameter of the particles. Further, the ratio of coarse particles of 96 ⁇ m or more can be easily determined from the overall particle size distribution.
  • the component (C) is an aluminum oxide powder having an average particle size of 0.1 to 5 ⁇ m, preferably 0.5 to 2 ⁇ m, and may be spherical or irregular. Other than the spherical shape is an indefinite shape. As long as the present invention is not impaired, one kind may be used alone, or two or more kinds having different average particle diameters may be used in combination. When the average particle diameter is less than 0.1 ⁇ m, the contact between the particles decreases, and the thermal conductivity tends to deteriorate due to an increase in the interparticle contact thermal resistance. On the other hand, if it exceeds 5 ⁇ m, the unevenness of the sheet surface becomes large, the interfacial thermal resistance increases, and the thermal conductivity tends to deteriorate.
  • the average sphericity is 0.8 or more and the number of hydroxyl groups is 30 / nm 2 or less as in the case of the component (B).
  • the measuring method of an average particle diameter, average sphericity, and a hydroxyl group is the same as (B) component.
  • the mixing ratio volume ratio of the component (B) and the component (C) is 5: 5 to 9.5: 0.5, and more preferably 6: 4 to 9: 1.
  • the ratio of the component (B) is smaller than 5 by volume ratio (the sum of the components (B) and (C) is 10, the same applies hereinafter)
  • the filling properties of the components (B) and (C) tend to deteriorate.
  • the ratio of (C) component becomes larger than 9.5, it becomes difficult to pack (B) component and (C) component densely, and thermal conductivity tends to decrease.
  • the total blending amount of the component (B) and the component (C) is 50% by volume or more and less than 80% by volume in the silicone composition, and preferably 60% by volume or more and less than 80% by volume. If the blending amount is less than 50% by volume, the thermal conductivity of the silicone composition may be insufficient, and if it is 80% by volume or more, it may be difficult to fill the thermally conductive filler and may become putty.
  • (D) In this invention, it is preferable that (D) silane coupling agent is further included and (B) component and (C) component are surface-treated with (D) silane coupling agent.
  • Examples of (D) silane coupling agents include vinyl silane coupling agents, epoxy silane coupling agents, acrylic silane coupling agents, and long-chain alkyl silane coupling agents. Two or more kinds can be used in appropriate combination. Among these, a long chain alkyl silane coupling agent is preferable, and decyltrimethoxysilane is preferable.
  • Component (B) component and (C) component surface treatment methods include spray methods using fluid nozzles, shearing stirring methods, dry methods such as ball mills and mixers, water-based or organic solvents A wet method such as a system can be adopted. The stirring method is performed so that the spherical aluminum oxide powder is not destroyed. The system temperature in the dry method or the drying temperature after the treatment is appropriately determined in the region where the surface treatment agent does not volatilize or decompose, depending on the type of the surface treatment agent, but is 80 to 180 ° C.
  • the amount of the component (DI) used for treatment is preferably 0.1 to 5 parts by mass with respect to 100 parts by mass in total of the component (B) and the component (C). If the amount is less than 0.1 parts by mass, the effect is small.
  • (D-II) an organo having at least one silyl group represented by the following general formula (1) in one molecule and having a viscosity at 25 ° C. of 0.01 to 30 Pa ⁇ s Polysiloxane is mentioned.
  • R 1 is independently an unsubstituted or substituted monovalent hydrocarbon group
  • R 2 is independently an alkyl group, an alkoxyalkyl group, an alkenyl group or an acyl group, and a is 0, 1 or 2 is there.
  • component (D-II) examples include organopolysiloxanes represented by the following general formula (2). Wherein R 1 is independently an unsubstituted or substituted monovalent hydrocarbon group, R 2 is independently an alkyl group, an alkoxyalkyl group, an alkenyl group or an acyl group, and b is an integer of 2 to 100 And a is 0, 1 or 2.)
  • R 1 is independently an unsubstituted or substituted monovalent hydrocarbon group having preferably 1 to 10 carbon atoms, more preferably 1 to 6 carbon atoms, still more preferably 1 to 3 carbon atoms.
  • Examples thereof include a linear alkyl group, a branched alkyl group, a cyclic alkyl group, an alkenyl group, an aryl group, an aralkyl group, and a halogenated alkyl group.
  • Examples of the linear alkyl group include a methyl group, an ethyl group, a propyl group, a hexyl group, an octyl group, and a decyl group.
  • Examples of the branched alkyl group include isopropyl group, isobutyl group, tert-butyl group, 2-ethylhexyl group and the like.
  • Examples of the cyclic alkyl group include a cyclopentyl group and a cyclohexyl group.
  • Examples of the alkenyl group include a vinyl group and an allyl group.
  • Examples of the aryl group include a phenyl group and a tolyl group.
  • Examples of the aralkyl group include 2-phenylethyl group and 2-methyl-2-phenylethyl group.
  • halogenated alkyl group examples include 3,3,3-trifluoropropyl group, 2- (nonafluorobutyl) ethyl group, 2- (heptadecafluorooctyl) ethyl group and the like.
  • R 1 is preferably a methyl group or a phenyl group.
  • R 2 is independently an alkyl group, an alkoxyalkyl group, an alkenyl group or an acyl group.
  • alkyl group include linear alkyl groups, branched alkyl groups, and cyclic alkyl groups similar to those exemplified for R 1 .
  • alkoxyalkyl group include a methoxyethyl group and a methoxypropyl group.
  • alkenyl group include those similar to those exemplified for R 1 .
  • the number of carbon atoms is preferably 1-8.
  • the acyl group include an acetyl group and an octanoyl group.
  • R 2 is preferably an alkyl group, particularly preferably a methyl group or an ethyl group.
  • b is an integer of 2 to 100, preferably 5 to 50. a is 0, 1 or 2, preferably 0.
  • organopolysiloxane of component (D-II) include the following. (In the formula, Me is a methyl group.)
  • the viscosity of the (D-II) component organopolysiloxane at 25 ° C. is usually 0.01 to 30 Pa ⁇ s, preferably 0.01 to 10 Pa ⁇ s. If the viscosity is lower than 0.01 Pa ⁇ s, oil bleed is likely to occur from the silicone composition, and there is a risk that it will easily sag. When the viscosity is higher than 30 mPa ⁇ s, the fluidity of the resulting silicone composition becomes extremely poor, and the coating workability may be deteriorated. This viscosity is a value measured by a rotational viscometer (the same applies hereinafter).
  • the blending amount of the component (D-II) is preferably 5 to 900 parts by weight, more preferably 10 to 900 parts by weight, and still more preferably 20 to 700 parts by weight with respect to 100 parts by weight of the component (A).
  • (E) component In the silicone composition of the present invention, (E) spherical glass beads or amorphous glass having a maximum center particle diameter of 150 ⁇ m or more and a SiO 2 content of 50% by mass or more are added to the total amount of the silicone composition. It is preferable to blend 10% by mass or less.
  • the component (E) is characterized in that the maximum value of the center particle diameter is larger than the average particle diameter of the component (B), and the upper limit is not particularly limited, but can be 300 ⁇ m or less.
  • the component (E) is preferably spherical rather than indefinite, and when the component (E) is spherical glass beads, the average sphericity is 0.8 or more, as in the component (B). Is preferred.
  • the component (E) is preferably added in a small amount within the range not impairing the present invention.
  • the total amount of the silicone composition is (
  • the amount of component F) is preferably 10% by mass or less (0 to 10% by mass).
  • the central particle diameter can be measured by a laser diffraction method using, for example, “Laser diffraction particle size distribution analyzer SALD-2300” manufactured by Shimadzu Corporation.
  • the thermally conductive silicone composition of the present invention may be used as it is, or may further be mixed with a curing agent to form a curable composition.
  • the curable thermally conductive silicone composition includes the following three forms.
  • the organopolysiloxane (A) as the base polymer is an organopolysiloxane having the above components (AI) to (A-III). Siloxane can be used and the above-mentioned thermally conductive fillers (B) and (C) can be blended.
  • [I] Addition reaction curable heat conductive silicone composition [II] Condensation reaction curable heat conductive silicone composition
  • the silicone composition is an addition reaction curable type thermal conductive silicone composition that cures by a hydrosilylation reaction
  • the component I) is used, and the following components are further included.
  • the curing agents are the following components (F) and (G).
  • H Addition reaction control agent as required
  • Organohydrogenpolysiloxane having at least two hydrogen atoms directly bonded to silicon atoms is a component that acts as a crosslinking agent.
  • Examples of the group bonded to the silicon atom bond of the organohydrogenpolysiloxane include the same linear alkyl group, branched alkyl group, cyclic alkyl group, aryl group, aralkyl group, and halogenated alkyl group as described above.
  • An alkyl group and an aryl group are preferable, and a methyl group and a phenyl group are particularly preferable.
  • the molecular structure of the component (F) is not limited, but is preferably in the range of 1 to 100,000 mPa ⁇ s, more preferably in the range of 1 to 5,000 mPa ⁇ s.
  • the molecular structure of the component (F) is not limited, and examples thereof include linear, branched, partially branched linear, cyclic, and dendritic (dendrimer). Examples of such organopolysiloxanes include single polymers having these molecular structures, copolymers comprising these molecular structures, or mixtures thereof.
  • component (F) for example, molecular chain both ends dimethylhydrogensiloxy group-blocked dimethylpolysiloxane, molecular chain both ends trimethylsiloxy group-blocked dimethylsiloxane / methylhydrogensiloxane copolymer, molecular chain both ends dimethylhydrogensiloxy group-blocked Dimethylsiloxane / methylhydrogensiloxane copolymer, siloxane unit represented by the formula: (CH 3 ) 3 SiO 1/2 and siloxane unit represented by the formula: (CH 3 ) 2 HSiO 1/2 and formula: SiO 4 /
  • the organosiloxane copolymer which consists of the siloxane unit represented by 2 is mentioned, It can use individually by 1 type or in combination of 2 or more types.
  • the amount of the component (F) is an amount necessary for curing the silicone composition.
  • the amount of the component (F) in the component (F) is 1 mol of silicon-bonded alkenyl groups in the component (AI).
  • the amount of silicon-bonded hydrogen atoms is preferably in the range of 0.1 to 10 mol, more preferably in the range of 0.1 to 5 mol, particularly 0.1
  • the amount is preferably in the range of ⁇ 3.0 mol. This is because when the content of this component is less than the lower limit of the above range, the resulting silicone composition tends not to be cured sufficiently, while when the upper limit of the above range is exceeded, it is obtained. In some cases, the silicone cured product becomes very hard and a large number of cracks are generated on the surface.
  • the platinum group metal curing catalyst is a catalyst for accelerating the curing of the silicone composition.
  • a catalyst for accelerating the curing of the silicone composition for example, chloroplatinic acid, chloroplatinic acid alcohol solution, platinum olefin complex, platinum alkenylsiloxane complex, platinum Of the carbonyl complex.
  • the blending amount of the component (G) is an amount necessary for curing the silicone composition.
  • the platinum metal in the component (G) is 0.01% by mass with respect to the component (AI).
  • the amount is preferably in the range of ⁇ 1,000 ppm, and particularly preferably in the range of 0.1 to 500 ppm. This is because when the blending amount of the component (G) is less than the lower limit of the above range, the resulting silicone composition tends not to be cured sufficiently, and on the other hand, the blending amount exceeds the upper limit of the above range. The curing rate of the resulting silicone composition is not significantly improved.
  • a curing reaction inhibitor can be blended in order to adjust the curing rate of the silicone composition and improve the handling workability.
  • the curing reaction inhibitor include acetylene compounds such as 2-methyl-3-butyn-2-ol, 2-phenyl-3-butyn-2-ol, 1-ethynyl-1-cyclohexanol; 3-methyl-3 -Ene-in compounds such as pentene-1-in and 3,5-dimethyl-3-hexen-1-in; other examples include hydrazine compounds, phosphine compounds, mercaptan compounds, etc. Two or more kinds can be used in appropriate combination.
  • the amount of component (H) is not particularly limited, but is preferably 0.0001 to 1.0% by mass with respect to the silicone composition. By setting it as the said range, the workability
  • the silicone composition is a condensation reaction curable heat conductive silicone composition
  • the component (A-II) shown above is used as (A) above, Furthermore, it contains the following components, and the curing agent is the following component (I).
  • (J) If necessary, a catalyst for condensation reaction
  • Examples of the silicon-bonded hydrolyzable group in component (I) include the same alkoxy groups, alkoxyalkoxy groups, acyloxy groups, ketoxime groups, alkenoxy groups, amino groups, aminoxy groups, and amide groups as described above.
  • the silicon atom of the silane includes, for example, the same linear alkyl group, branched alkyl group, cyclic alkyl group, alkenyl group, aryl group, aralkyl group, halogen as described above.
  • An alkyl group may be bonded.
  • Examples of such silanes or partial hydrolysates thereof include methyltriethoxysilane, vinyltriethoxysilane, vinyltriacetoxysilane, and ethyl orthosilicate.
  • the amount of the component (I) is an amount necessary for curing the silicone composition, and specifically, within a range of 0.01 to 20 parts by mass with respect to 100 parts by mass of the component (A-II). In particular, it is preferably in the range of 0.1 to 10 parts by mass. If the content of this silane or its partial hydrolyzate is less than the lower limit of the above range, the storage stability of the resulting silicone composition may be lowered, whereas it exceeds the upper limit of the above range. If it is in an amount, curing of the resulting silicone composition may be remarkably slowed.
  • the component (J) is an optional component, and is not essential when, for example, a silane having a hydrolyzable group such as an aminoxy group, an amino group, or a ketoxime group is used as a curing agent.
  • condensation reaction catalysts include organic titanates such as tetrabutyl titanate and tetraisopropyl titanate; organic titanium such as diisopropoxybis (acetylacetate) titanium and diisopropoxybis (ethylacetoacetate) titanium.
  • organoaluminum compounds such as aluminum tris (acetylacetonate) and aluminum tris (ethylacetoacetate); organoaluminum compounds such as zirconium tetra (acetylacetonate) and zirconium tetrabutyrate; dibutyltin dioctoate, dibutyltin dilaurate, Organic tin compounds such as butyltin-2-ethylhexoate; organics such as tin naphthenate, tin oleate, tin butyrate, cobalt naphthenate, zinc stearate Rubonic acid metal salts; amine compounds such as hexylamine and dodecylamine phosphate; and salts thereof; quaternary ammonium salts such as benzyltriethylammonium acetate; lower fatty acid salts of alkali metals such as potassium acetate and lithium nitrate; dimethylhydroxy
  • the blending amount may be an amount necessary for curing the silicone composition, and specifically, 0.01 to 20 parts by mass with respect to 100 parts by mass of the component (A). It is preferably within the range, and particularly preferably within the range of 0.1 to 10 parts by mass. This is because when the catalyst is essential, if the content of the catalyst is less than the lower limit of the above range, the resulting silicone composition tends not to be sufficiently cured, whereas the above range. This is because the storage stability of the resulting silicone composition tends to decrease when the upper limit of the above is exceeded.
  • (K) organic peroxides examples include benzoyl peroxide, dicumyl peroxide, 2,5-dimethylbis (2,5-t-butylperoxy) hexane, di-t-butyl peroxide, t- Butyl perbenzoate is mentioned.
  • the amount of the component (K) is an amount necessary for curing the silicone composition. Specifically, the amount is 0.1 to 5 parts by mass with respect to 100 parts by mass of the organopolysiloxane of the component (A-III). The range of is preferable. When the blending amount of the component (K) is less than the lower limit of the above range, the resulting silicone composition tends not to be cured sufficiently, while the silicone composition obtained even when blending an amount exceeding the upper limit of the above range. The curing rate of the object is not significantly improved and may cause voids.
  • a filler such as zinc oxide, fumed silica, precipitated silica, fumed titanium oxide, etc.
  • this filler Filler whose surface is hydrophobized with an organosilicon compound
  • Adhesive agent such as 3-glycidoxypropyltrimethoxysilane, 3-methacryloxypropyltrimethoxysilane
  • Other pigments, dyes, fluorescent dyes, heat-resistant additives In addition, a flame retardant imparting agent such as a triazole compound or a plasticizer may be contained.
  • thermally conductive fillers other than (B) component for example, aluminum powder, copper powder, silver powder, nickel powder, gold powder, zinc oxide powder , Magnesium oxide powder, boron nitride powder, aluminum nitride powder, diamond powder, carbon powder and the like.
  • the silicone composition of the present invention can be prepared by uniformly mixing a predetermined amount of each of the above components.
  • A an organopolysiloxane
  • B The ratio of coarse particles having an average sphericity of 0.8 or more, a hydroxyl group of 30 / nm 2 or less, an average particle diameter of 10 ⁇ m or more and less than 50 ⁇ m, and a laser diffraction type particle size distribution of 96 to 150 ⁇ m is 0% of the total component (B).
  • Component (B) and Component (C), comprising the step of mixing spherical aluminum oxide powder of 1 to 30% by mass and (C) spherical or amorphous aluminum oxide powder having an average particle size of 0.1 to 5 ⁇ m
  • the mixing ratio volume ratio ((B) :( C)) is 5: 5 to 9.5: 0.5
  • the total amount of the component (B) and the component (C) is 50% by volume or more and 80% by volume. %
  • the thermal conductivity of the composition is 1.2 W / m ⁇ K or more and less than 5.5 W / m ⁇ K
  • the viscosity of the composition at 25 ° C. is 10 rpm.
  • a method for producing a thermally conductive silicone composition having a pressure of 5 to 800 Pa ⁇ s at the time of measurement can be mentioned. Furthermore, the process of mixing arbitrary components may be included.
  • the thermal conductivity of the thermally conductive silicone composition is 1.2 W / m ⁇ K or more and less than 5.5 W / m ⁇ K in the hot disk method according to ISO 22007-2, and is 1.5 to 5.5 W / m ⁇ K is more preferable.
  • the measurement temperature is 25 ° C.
  • the viscosity of the thermally conductive silicone composition at 25 ° C. is 5 to 800 Pa ⁇ s, preferably 30 to 600 Pa ⁇ s, when the rotational speed is measured at 10 rpm with a spiral viscometer.
  • the method for curing it is not limited.
  • the silicone composition is molded and then allowed to stand at room temperature, the silicone composition is molded and then heated to 40 to 200 ° C. And a silicone elastomer molded article is obtained.
  • the properties of the silicone rubber thus obtained are not limited, and examples thereof include a gel shape, a low hardness rubber shape, and a high hardness rubber shape.
  • the cured thickness is preferably 150 ⁇ m or more. Although an upper limit is not specifically limited, When the magnitude
  • the silicone composition was poured into a mold having a cured thickness of 6 mm and cured at 100 ° C. for 1 hour. Next, when two cured products having a thickness of 6 mm are stacked and measured with an Asker C hardness meter, 3 to 90 is preferable, and 5 to 80 is more preferable.
  • the thermal conductivity of the cured product at 150 ° C. is preferably 0.7 W / m ⁇ K or more and less than 4.0 W / m ⁇ K, preferably 1.0 W / m ⁇ K or more and 4 or more in the hot disk method according to ISO 22007-2. Less than 0.0 W / m ⁇ K is more preferable.
  • the thermal conductivity of the cured product at 25 ° C. is 1.2 W / m ⁇ K or more and less than 5.5 W / m ⁇ K in the hot disk method according to ISO 22007-2, and is 1.5 to 5.5 W. / M ⁇ K is more preferable. Incidentally, at 25 ° C., the temperature at 150 ° C.
  • the thermal conductivity estimated from each temperature in the linear line obtained by plotting the thermal conductivity obtained at 25 ° C. and 150 ° C. is also It is covered by the present invention.
  • Component A-1 Dimethylpolysiloxane A-2 having a viscosity at 25 ° C. of 400 mPa ⁇ s, both ends blocked with dimethylvinylsilyl groups, and a Vi group amount of 0.018 mol / 100 g: Shin-Etsu Chemical Industrial KF-54, specific gravity (25 ° C.) of 1.07, kinematic viscosity (25 ° C.) 400 mm 2 / s molecular chain both ends trimethylsiloxy group-blocked dimethylsiloxane / diphenylsiloxane copolymer
  • A-3 Shin-Etsu Chemical Industrial KF-50-1,000cs, specific gravity (25 ° C) is 1.00, kinematic viscosity (25 ° C) is 1,000 mm 2 / s molecular chain both ends trimethylsiloxy group-blocked dimethyls
  • (B) Component Spherical aluminum oxide having the properties shown in the following table
  • the coarse particle content shown here is the ratio of the coarse particles of 96 to 150 ⁇ m to the whole particle size distribution obtained by the laser diffraction type particle size distribution.
  • Component (C) Spherical or amorphous aluminum oxide having the properties shown in the table below
  • Component E-1 GL particle size series M-9 manufactured by Potters Ballotini (maximum value of the center particle diameter is 180 ⁇ m), spherical glass beads having a SiO 2 content of 99.4% by mass
  • Example 1 to 16 Comparative Examples 1 to 16
  • a silicone composition was prepared by the method shown below, and a thermally conductive molded product was obtained using this silicone composition. Using these, evaluation was carried out by the method shown below. The results are also shown in the table.
  • the above components were mixed as shown below in the blending amounts shown in Tables 3 to 6 to obtain a silicone composition. That is, the components (A), (B), (C), and (D) were added to the 5 liter gate mixer (Inoue Seisakusho Co., Ltd., trade name: 5 liter planetary mixer) in the blending amounts shown in Table 1, The mixture was deaerated and heated at 150 ° C. for 2 hours. Then, it cools until it becomes normal temperature (25 degreeC), (G) component is added, it mixes at room temperature (25 degreeC) so that it may become uniform, (H) component is added continuously, and it is room temperature so that it may become uniform (25 ° C).
  • 5 liter gate mixer Inoue Seisakusho Co., Ltd., trade name: 5 liter planetary mixer
  • the components (E) and (F) were added and deaerated and mixed at room temperature so as to be uniform.
  • the initial viscosity, the hardness after curing, and the thermal conductivity before and after curing were evaluated by the following methods. The results are also shown in the table.
  • the initial viscosity of the silicone composition was a value at 25 ° C., and a spiral viscometer: Malcolm viscometer (type PC-10AA, rotation speed 10 rpm) was used for the measurement.
  • a spiral viscometer Malcolm viscometer (type PC-10AA, rotation speed 10 rpm) was used for the measurement.
  • the silicone composition was poured into a mold having a cured thickness of 6 mm and cured at 100 ° C. for 1 hour. Next, two 6 mm thick cured products were stacked and measured with an Asker C hardness meter.
  • the thermal conductivity before curing of the silicone composition at 25 ° C. was measured using a hot disk method thermophysical property measuring apparatus TPS 2500 S manufactured by Kyoto Electronics Industry Co., Ltd.
  • the silicone composition was poured into a mold having a cured thickness of 6 mm and cured at 100 ° C. for 1 hour.
  • cured material in 25 degreeC and 150 degreeC was measured.

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Abstract

L'invention concerne une composition de silicone thermoconductrice qui contient (A) un organopolysiloxane, (B) une poudre d'oxyde d'aluminium sphérique de sphéricité moyenne supérieure ou égale à 0,8, de 30 groupes hydroxyle /ｎｍ2 ou moins, de diamètre particulaire moyen compris supérieur ou égal à 10μｍ et inférieur ou égal à 50μｍ, et de proportion de particules grossières de 96 à 150μｍ comprise entre 0,1 et 30% en masse de l'ensemble du composant, et (C) une poudre d'oxyde d'aluminium sphérique ou de forme indéterminée de diamètre particulaire moyen compris entre 0,1 et 5μｍ. Plus précisément, l'invention concerne une composition de silicone thermoconductrice qui présente un rapport desdits composants (B) et (C) compris entre ５：５ et ９,５：０,５, une quantité totale de composants (B) et (C) supérieure ou égale à 50 et inférieure à 80%, une thermoconduction supérieure ou égale à １,２Ｗ／ｍ・Ｋ et inférieure à ５,５Ｗ／ｍ・Ｋ, et une viscosité à 25°C comprise entre 5 et 800Pa.s lors d'une mesure à l'aide d'un viscosimètre à spirale à une fréquence de rotation de 10rpm.
PCT/JP2017/040203 2016-11-09 2017-11-08 Composition de silicone thermoconductrice, article durci de celle-ci, et procédé de fabrication associé Ceased WO2018088417A1 (fr)

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JP7346761B1 (ja) 2023-04-27 2023-09-19 旭化成ワッカーシリコーン株式会社 熱伝導性シリコーン組成物および熱伝導性シリコーン組成物の製造方法
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KR20220024818A (ko) * 2019-06-24 2022-03-03 신에쓰 가가꾸 고교 가부시끼가이샤 고열전도성 실리콘 조성물 및 그 경화물
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JP7346761B1 (ja) 2023-04-27 2023-09-19 旭化成ワッカーシリコーン株式会社 熱伝導性シリコーン組成物および熱伝導性シリコーン組成物の製造方法
JP2024158046A (ja) * 2023-04-27 2024-11-08 旭化成ワッカーシリコーン株式会社 熱伝導性シリコーン組成物および熱伝導性シリコーン組成物の製造方法
WO2025187352A1 (fr) * 2024-03-04 2025-09-12 信越化学工業株式会社 Tube thermorétractable en silicone thermoconductrice

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