WO2022264790A1 - Feuille thermoconductrice et procédé de production de feuille thermoconductrice - Google Patents

Feuille thermoconductrice et procédé de production de feuille thermoconductrice Download PDF

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WO2022264790A1
WO2022264790A1 PCT/JP2022/021880 JP2022021880W WO2022264790A1 WO 2022264790 A1 WO2022264790 A1 WO 2022264790A1 JP 2022021880 W JP2022021880 W JP 2022021880W WO 2022264790 A1 WO2022264790 A1 WO 2022264790A1
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thermally conductive
conductive sheet
conductive filler
volume
anisotropic
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English (en)
Japanese (ja)
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勇磨 佐藤
佑介 久保
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デクセリアルズ株式会社
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • 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
    • C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
    • C08K3/013—Fillers, pigments or reinforcing additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/38—Boron-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L101/00—Compositions of unspecified macromolecular compounds
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
    • H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
    • H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
    • H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K7/00—Constructional details common to different types of electric apparatus
    • H05K7/20—Modifications to facilitate cooling, ventilating, or heating

Definitions

  • This technology relates to a thermally conductive sheet and a method for manufacturing the thermally conductive sheet.
  • This application claims priority based on Japanese Patent Application No. 2021-099910 filed on June 16, 2021 in Japan, and this application is hereby incorporated by reference. Incorporated.
  • an electronic component is attached to a heat sink such as a heat dissipating fan or a heat dissipating plate via a heat conductive sheet.
  • a heat conductive sheet a silicone resin containing (dispersing) a filler such as an inorganic filler is widely used.
  • thermal conductivity of the thermally conductive sheet it is being studied to increase the filling rate of the inorganic filler blended in the matrix such as the binder resin.
  • the filling rate of the inorganic filler is increased, the flexibility of the thermally conductive sheet may be impaired, or powder of the inorganic filler may fall off. Therefore, there is a limit to increasing the filling rate of the inorganic filler in the heat conductive sheet.
  • inorganic fillers include alumina, aluminum nitride, and aluminum hydroxide.
  • the matrix may be filled with scaly particles such as boron nitride or graphite, carbon fibers, or the like. This is due to the anisotropy of thermal conductivity of scale-like particles, carbon fibers, and the like.
  • carbon fibers are known to have a thermal conductivity of about 600-1200 W/m ⁇ K in the fiber direction.
  • Boron nitride which is a scaly particle, has a thermal conductivity of about 110 W/m K in the plane direction, and a thermal conductivity of about 2 W/m K in the direction perpendicular to the plane direction.
  • carbon fibers and scaly particles are known to have anisotropic thermal conductivity.
  • the thermal conductivity of the thermally conductive sheet can be dramatically improved.
  • the heat conductive sheet is used to judge the quality of the manufactured heat conductive sheet. It is demanded that it is possible to easily determine whether or not a thermally conductive sheet has a predetermined thermal conductivity.
  • Patent Document 1 discloses a thermally conductive sheet made of a resin composition containing a resin and a scaly thermally conductive filler dispersed in the resin, wherein the scaly thermally conductive filler increases the thickness of the thermally conductive sheet.
  • a thermally conductive sheet is described in which the inclination with respect to the longitudinal direction periodically changes along one direction within the surface direction of the thermally conductive sheet.
  • the heat conductive sheet described in Patent Literature 1 has an insufficient degree of orientation of the scale-like filler and cannot be said to be a high heat conductive sheet having anisotropy, and it is considered difficult to achieve high heat conductivity.
  • This technology has been proposed in view of such conventional circumstances, and provides a thermally conductive sheet that has a high thermal conductivity and that can easily determine the quality of a desired thermally conductive sheet.
  • a thermally conductive sheet according to the present technology is a thermally conductive sheet made of a cured product of a composition containing a binder resin, an anisotropic thermally conductive filler, and a thermally conductive filler other than the anisotropic thermally conductive filler. and satisfies the following conditions 1 to 3.
  • the gloss value is less than 10 as measured by light rays incident at a position of 60° from an imaginary perpendicular to the surface of the heat conductive sheet.
  • the average particle size of the anisotropic thermally conductive filler is 15 ⁇ m or more and 45 ⁇ m or less.
  • the total content of the anisotropic thermally conductive filler and other thermally conductive fillers in the thermally conductive sheet is more than 60% by volume and less than 75% by volume.
  • a method for producing a thermally conductive sheet according to the present technology comprises a thermally conductive composition containing a curable resin composition, an anisotropic thermally conductive filler, and a thermally conductive filler other than the anisotropic thermally conductive filler. a step of extruding and then curing the thermally conductive composition to obtain a columnar cured product; and cutting the columnar cured product into a predetermined thickness in a direction substantially perpendicular to the length direction of the column. and obtaining a heat conductive sheet, and the heat conductive sheet satisfies the conditions 1 to 3 described above.
  • This technology can provide a thermally conductive sheet that has high thermal conductivity and can easily determine the quality of a desired thermally conductive sheet.
  • FIG. 1 is a cross-sectional view showing an example of a heat conductive sheet.
  • FIG. 2 is a diagram for explaining an example of a gloss value measuring method.
  • FIG. 3 is a perspective view schematically showing scale-like boron nitride having a hexagonal crystal shape, which is an example of an anisotropic thermally conductive filler.
  • FIG. 4 is a cross-sectional view showing an example of a semiconductor device to which a heat conductive sheet is applied.
  • the average particle size (D50) of anisotropic thermally conductive fillers and other thermally conductive fillers means that the entire particle size distribution of the anisotropic thermally conductive fillers or other thermally conductive fillers is 100 %, it means the particle diameter when the cumulative value is 50% when the cumulative curve of the particle diameter value is obtained from the small particle diameter side of the particle diameter distribution.
  • the particle size distribution (particle size distribution) in this specification is determined by volume. Examples of the method for measuring the particle size distribution include a method using a laser diffraction particle size distribution analyzer.
  • FIG. 1 is a cross-sectional view showing an example of a heat conductive sheet 1 according to the present technology.
  • the thermally conductive sheet 1 is made of a cured composition containing a binder resin 2 , an anisotropic thermally conductive filler 3 , and a thermally conductive filler 4 other than the anisotropic thermally conductive filler 3 .
  • the thermally conductive sheet 1 has an anisotropic thermally conductive filler 3 and another thermally conductive filler 4 dispersed in a binder resin 2, and the anisotropic thermally conductive filler 3 extends in the thickness direction B of the thermally conductive sheet 1. is oriented.
  • the orientation of the anisotropic thermally conductive fillers 3 in the thickness direction B of the thermally conductive sheet 1 means, for example, that among all the anisotropic thermally conductive fillers 3 in the thermally conductive sheet 1,
  • the anisotropic thermally conductive filler 3 is a thermally conductive filler having an anisotropic shape.
  • examples of the anisotropic thermally conductive filler 3 include thermally conductive fillers having a long axis, a short axis, and a thickness (for example, scale-like thermally conductive fillers).
  • the scale-like thermally conductive filler is a thermally conductive filler having a long axis, a short axis, and a thickness, has a high aspect ratio (long axis/thickness), and is isotropic in the plane including the long axis. It has a good thermal conductivity.
  • the short axis of the scaly thermally conductive filler is a direction that intersects through the midpoint of the long axis of the scaly thermally conductive filler in a plane containing the long axis of the scaly thermally conductive filler. , refers to the length of the shortest part of the scale-like thermally conductive filler.
  • the thickness of the scale-like thermally conductive filler refers to the average value obtained by measuring the thickness of the surface including the long axis of the scale-like thermally conductive filler at 10 points.
  • the aspect ratio of the anisotropic thermally conductive filler 3 is not particularly limited, and can be appropriately selected depending on the purpose.
  • the aspect ratio of the anisotropic thermally conductive filler 3 can be in the range of 10-100.
  • the major axis, minor axis and thickness of the anisotropic thermally conductive filler 3 can be measured with, for example, a microscope, scanning electron microscope (SEM), particle size distribution meter, or the like.
  • the other thermally conductive filler 4 is a thermally conductive filler other than the anisotropic thermally conductive filler 3, that is, a thermally conductive filler that does not have anisotropy in shape.
  • FIG. 2 is a diagram for explaining an example of a gross value measurement method.
  • the formulation of the thermally conductive sheet 1 in particular, the orientation of the anisotropic thermally conductive filler 3, the average particle size of the anisotropic thermally conductive filler 3, the anisotropic thermally conductive filler 3 and the total content of other thermally conductive fillers 4, etc.
  • the anisotropic thermally conductive filler 3 is oriented. Compared to a thermally conductive sheet that has a high gloss value, it tends to have a higher gloss value because the reflected component of incident light increases.
  • the anisotropic thermally conductive filler 3 in the thermally conductive sheet 1 and the other thermally conductive filler 4 in the thermally conductive sheet 1 the anisotropic thermally conductive filler 3 in the thermally conductive sheet 1 and the When the total content of the other thermally conductive fillers 4 is reduced, the binder existing on the surface of the thermally conductive sheet 1 is more likely to be reflected than the particles (anisotropic thermally conductive fillers 3 and other thermally conductive fillers 4). The effect of the glossiness of the resin 2 tends to increase.
  • the binder resin 2 is a silicone resin
  • the luster of the silicone resin flowing out from the thermally conductive sheet 1 becomes stronger than the reflection by the anisotropic thermally conductive filler 3 and other thermally conductive fillers 4, and the anisotropic It is considered that the decrease in the total content of the thermally conductive filler 3 and the other thermally conductive filler 4 increases the effect of the silicone resin on the gloss value.
  • the thermal conductivity of the thermally conductive sheet 1 increases as the particle diameter of the anisotropic thermally conductive filler 3 increases.
  • the particle size of the anisotropic thermally conductive filler 3 exceeds a certain value, it becomes difficult to fill the binder resin 2 with the anisotropic thermally conductive filler 3 due to the effect of the particle size. It tends to be difficult to improve the conductivity.
  • the heat conductive sheet 1 satisfies the following conditions 1 to 3.
  • the gloss value measured by the light ray 6 incident from the position of 60° from the imaginary perpendicular 5 to the surface 1A of the heat conductive sheet 1 is less than 10.
  • the average particle size of the anisotropic thermally conductive filler 3 is 15 ⁇ m or more and 45 ⁇ m or less.
  • the total content of the anisotropic thermally conductive filler 3 and the other thermally conductive filler 4 in the thermally conductive sheet 1 is more than 60% by volume and less than 75% by volume.
  • the heat conductive sheet 1 has a gloss value of less than 10, and may be 8 or less, measured with a light ray 6 incident at a position of 60° from an imaginary perpendicular 5 to the surface 1A of the heat conductive sheet 1. , 7 or less, 6.2 or less, 5.4 or less, 5.2 or less, or 3.9 or less.
  • the method for measuring the gloss value of the thermally conductive sheet 1 is the same as the method described in Examples below.
  • the thermally conductive sheet 1 When the thermally conductive sheet 1 satisfies the condition 1, as described above, the ratio of the anisotropic thermally conductive filler 3 in the thermally conductive sheet 1 tends to be high, and the thickness direction of the thermally conductive sheet 1 Good thermal conductivity. Further, when the thermally conductive sheet 1 satisfies the condition 1, the quality of the manufactured thermally conductive sheet is determined, for example, the thermally conductive sheet containing a predetermined amount of thermally conductive filler having a predetermined particle size has a predetermined thermal conductivity. can be easily determined.
  • the gloss value of the thermally conductive sheet 1 can also be measured to obtain a rough estimate of the thermal conductivity of the thermally conductive sheet 1. Furthermore, when the thermally conductive sheet 1 satisfies the condition 1, when using the thermally conductive sheet 1, it is possible to more reliably avoid erroneous image recognition when the thermally conductive sheet 1 is picked up by an automatic machine. It becomes possible to pick up the heat conductive sheet 1 more reliably.
  • the average particle size of the anisotropic thermally conductive filler 3 in the thermally conductive sheet 1 is 15 ⁇ m or more, even if it is 20 ⁇ m or more. It may be 25 ⁇ m or more, 30 ⁇ m or more, 35 ⁇ m or more, or 40 ⁇ m or more. Moreover, the average particle size of the anisotropic thermally conductive filler 3 in the thermally conductive sheet 1 is preferably in the range of 20 to 40 ⁇ m from the viewpoint of improving the thermal conductivity of the thermally conductive sheet 1 .
  • one type of anisotropic thermally conductive filler 3 may be used alone, or two or more types of anisotropic thermally conductive fillers 3 having different particle sizes may be used in combination.
  • the particle size is 20 ⁇ m with respect to the total content of the anisotropic thermally conductive fillers 3 in the thermally conductive sheet 1.
  • the content ratio of the anisotropic thermally conductive filler 3 having a diameter of 40 ⁇ m or more may be 50% by volume or more, may be 60% by volume or more, may be 70% by volume or more, or may be 80% by volume or more. It may be vol % or more, 90 vol % or more, or 100 vol %.
  • the thermally conductive sheet 1 preferably contains anisotropic thermally conductive filler 3 alone as the anisotropic thermally conductive filler 3. That is, it is preferable not to use two or more anisotropic thermally conductive fillers 3 together in the thermally conductive sheet 1 .
  • the thermally conductive sheet 1 has a total content of the anisotropic thermally conductive filler 3 and the other thermally conductive filler 4 of 60% by volume from the viewpoint of thermal conductivity and the gloss value of the condition 1 described above. It may exceed 61% by volume, may be 63% by volume or more, may be 66% by volume or more, or may be 67% by volume or more. In addition, from the viewpoint of moldability of the heat conductive sheet 1, the total content of the anisotropic heat conductive filler 3 and the other heat conductive filler 4 is less than 75% by volume, and 74% by volume. 70% by volume or less, 69% by volume or less, or 68% by volume or less. Further, in the thermally conductive sheet 1, the total content of the anisotropic thermally conductive filler 3 and the other thermally conductive filler 4 may be in the range of 63 to 67% by volume.
  • the content of the anisotropic thermally conductive filler 3 in the thermally conductive sheet 1 is preferably more than 20% by volume from the viewpoint of the thermal conductivity of the thermally conductive sheet 1 and the gloss value of Condition 1 described above, and 23% by volume. % or more, 25 volume % or more, or 26 volume % or more.
  • the content of the anisotropic thermally conductive filler 3 in the thermally conductive sheet 1 is preferably less than 35% by volume from the viewpoint of moldability of the thermally conductive sheet 1, and even if it is 30% by volume or less. It may be 28% by volume or less, or 27% by volume or less.
  • the content of the anisotropic thermally conductive filler 3 in the thermally conductive sheet 1 may be in the range of 23 to 27% by volume.
  • the content of the other thermally conductive filler 4 in the thermally conductive sheet 1 may be 10% by volume or more, may be 15% by volume or more, or may be 20% by volume or more, It may be 25% by volume or more, 30% by volume or more, or 35% by volume or more.
  • the upper limit of the content of the other thermally conductive filler 4 in the thermally conductive sheet 1 may be 50% by volume or less, may be 45% by volume or less, or may be 40% by volume or less. good too.
  • the content of the other thermally conductive filler 4 in the thermally conductive sheet 1 may be in the range of 30 to 50% by volume, may be in the range of 35 to 45% by volume, and may be in the range of 37 to 42% by volume. % may be in the range.
  • a thermally conductive sheet 1 that is, a cured product of a composition containing a binder resin 2, an anisotropic thermally conductive filler 3, and another thermally conductive filler 4, satisfying the conditions 1 to 3 described above.
  • the sheet tends to have more anisotropic thermally conductive fillers 3 oriented along the thickness direction B as the L* value in the L*a*b* color system of the sheet surface increases.
  • the thermal conductivity of is good. Therefore, the heat conductive sheet 1 preferably has an L* value of 70 or more, may be 75 or more, may be 77 or more, or may be 80 in the L*a*b* color system of the sheet surface. It may be 85 or more, 88 or more, or 89 or more.
  • the upper limit of the L* value of the sheet surface in the L*a*b* color system of the heat conductive sheet 1 is preferably 95 or less, and may be 90 or less.
  • the L*a*b color system is, for example, a color system described in "JIS Z 8781", and is indicated by arranging each color in a spherical color space.
  • lightness is indicated by the position in the vertical axis (z-axis) direction
  • hue is indicated by the position in the outer peripheral direction
  • saturation is indicated by the distance from the central axis.
  • the position in the vertical axis (z-axis) direction indicating brightness is indicated by L*.
  • the value of lightness L* is a positive number, and the smaller the number, the lower the lightness, which tends to be darker. Specifically, the value of L* varies from 0, which corresponds to black, to 100, which corresponds to white.
  • the positive direction of the x-axis is the red direction
  • the positive direction of the y-axis is the yellow direction
  • the negative direction of the x-axis is the green direction
  • the y The negative direction of the axis is the blue direction.
  • Position along the x-axis is represented by a*, which ranges from -60 to +60.
  • Position along the y-axis is represented by b*, which ranges from -60 to +60.
  • a* and b* are positive and negative numbers representing chromaticity, and the closer they are to 0, the darker they become. Hue and saturation are represented by these a* and b* values.
  • the thermal conductivity of the thermal conductive sheet 1 is preferably as high as possible from the viewpoint of high thermal conductivity. ⁇ K or more, 8.4 W / m ⁇ K or more, 8.7 W / m ⁇ K or more, 10.3 W / m ⁇ K or more .
  • the thermal conductivity of the thermally conductive sheet 1 can be measured by the method described in Examples below.
  • the thickness of the heat conductive sheet 1 is not particularly limited, and can be appropriately selected according to the purpose.
  • the thickness of the heat conductive sheet can be 0.05 mm or more, and can be 0.1 mm or more.
  • the upper limit of the thickness of the heat conductive sheet may be 5 mm or less, may be 4 mm or less, or may be 3 mm or less.
  • the thickness of the heat conductive sheet 1 is preferably 0.1 to 4 mm.
  • the thickness of the thermally conductive sheet 1 can be obtained, for example, by measuring the thickness B of the thermally conductive sheet 1 at five arbitrary points and calculating the arithmetic average value thereof.
  • the binder resin 2 is for holding the anisotropic thermally conductive filler 3 and other thermally conductive fillers 4 within the thermally conductive sheet 1 .
  • the binder resin 2 is selected according to properties such as mechanical strength, heat resistance, and electrical properties required for the heat conductive sheet 1 .
  • the binder resin 2 can be selected from thermoplastic resins, thermoplastic elastomers, and thermosetting resins.
  • thermoplastic resins include polyethylene, polypropylene, ethylene- ⁇ -olefin copolymers such as ethylene-propylene copolymers, polymethylpentene, polyvinyl chloride, polyvinylidene chloride, polyvinyl acetate, ethylene-vinyl acetate copolymers, Fluorinated polymers such as polyvinyl alcohol, polyvinyl acetal, polyvinylidene fluoride and polytetrafluoroethylene, polyethylene terephthalate, polybutylene terephthalate, polyethylene naphthalate, polystyrene, polyacrylonitrile, styrene-acrylonitrile copolymer, acrylonitrile-butadiene-styrene copolymer Polymer (ABS) resin, polyphenylene-ether copolymer (PPE) resin, modified PPE resin, aliphatic polyamides, aromatic polyamides, polyimide, polyamideimide, polymeth
  • Thermoplastic elastomers include styrene-butadiene block copolymers or hydrogenated products thereof, styrene-isoprene block copolymers or hydrogenated products thereof, styrene-based thermoplastic elastomers, olefin-based thermoplastic elastomers, and vinyl chloride-based thermoplastic elastomers. , polyester-based thermoplastic elastomers, polyurethane-based thermoplastic elastomers, polyamide-based thermoplastic elastomers, and the like.
  • Thermosetting resins include crosslinked rubbers, epoxy resins, phenolic resins, polyimide resins, unsaturated polyester resins, diallyl phthalate resins, and the like.
  • Specific examples of crosslinked rubber include natural rubber, acrylic rubber, butadiene rubber, isoprene rubber, styrene-butadiene copolymer rubber, nitrile rubber, hydrogenated nitrile rubber, chloroprene rubber, ethylene-propylene copolymer rubber, chlorinated polyethylene rubber, Chlorosulfonated polyethylene rubber, butyl rubber, halogenated butyl rubber, fluororubber, urethane rubber, and silicone rubber.
  • a silicone resin is preferable from the viewpoint of adhesion between the heat generating surface of the heat generating body (eg, electronic component) and the heat sink surface, and from the viewpoint of satisfying the condition 1 described above.
  • the silicone resin for example, a two-component addition reaction type silicone resin composed of a silicone having an alkenyl group as a main component, a main agent containing a curing catalyst, and a curing agent having a hydrosilyl group (Si—H group).
  • the alkenyl group-containing silicone for example, a vinyl group-containing polyorganosiloxane can be used.
  • the curing catalyst is a catalyst for promoting the addition reaction between the alkenyl group in the alkenyl group-containing silicone and the hydrosilyl group in the hydrosilyl group-containing curing agent.
  • the curing catalyst well-known catalysts used for hydrosilylation reaction can be used.
  • platinum group curing catalysts such as platinum group metals such as platinum, rhodium and palladium, and platinum chloride can be used.
  • the curing agent having hydrosilyl groups for example, polyorganosiloxane having hydrosilyl groups can be used.
  • the binder resin 2 may be used individually by 1 type, and may use 2 or more types together.
  • the content of the binder resin 2 in the heat conductive sheet 1 is not particularly limited, and can be appropriately selected according to the purpose.
  • the content of the binder resin 2 in the heat conductive sheet 1 may be more than 25% by volume, may be 30% by volume or more, may be 32% by volume or more, or may be 33% by volume or more.
  • the upper limit of the content of the binder resin 2 in the heat conductive sheet 1 can be 60% by volume or less, may be 50% by volume or less, or may be 40% by volume or less. It may be vol% or less.
  • the content of the binder resin 2 in the heat conductive sheet 1 is preferably more than 25% by volume and less than 40% by volume, and is 33 to 37% by volume. There may be.
  • the material of the anisotropic thermally conductive filler 3 is not particularly limited, and examples thereof include boron nitride (BN), mica, alumina, aluminum nitride, silicon carbide, silica, zinc oxide, and molybdenum disulfide. Boron nitride is preferable from the viewpoint of the rate and the gloss value of Condition 1 described above.
  • the anisotropic thermally conductive filler 3 may be used singly or in combination of two or more.
  • FIG. 3 is a perspective view schematically showing scale-like boron nitride 3A having a hexagonal crystal shape, which is an example of the anisotropic thermally conductive filler 3.
  • a represents the long axis of the scaly boron nitride 3A
  • b represents the thickness of the scaly boron nitride 3A
  • c represents the short axis of the scaly boron nitride 3A.
  • the anisotropic thermally conductive filler 3 it is possible to use scale-like boron nitride 3A having a hexagonal crystal shape as shown in FIG. preferable.
  • a scaly thermally conductive filler eg, scaly boron nitride 3A
  • a spherical thermally conductive filler eg, spherical boron nitride
  • the average particle size of the anisotropic thermally conductive filler 3 can be appropriately selected according to the purpose within a range that satisfies the condition 2 described above.
  • the content of the anisotropic thermally conductive filler 3 in the thermally conductive sheet 1 can be appropriately selected according to the purpose within the range that satisfies the condition 3 described above.
  • thermally conductive fillers 4 include spherical, powdery, granular, and other thermally conductive fillers. From the viewpoint of the thermal conductivity of the thermally conductive sheet 1, the material of the other thermally conductive filler 4 is preferably, for example, a ceramic filler. Specific examples include aluminum oxide (alumina, sapphire), aluminum nitride, aluminum hydroxide, zinc oxide, boron nitride, zirconia, silicon carbide and the like. Other thermally conductive fillers 4 may be used singly or in combination of two or more.
  • alumina and It preferably contains at least one of aluminum nitride, zinc oxide and aluminum hydroxide.
  • aluminum nitride and alumina can be used in combination.
  • the average particle size of aluminum nitride may be less than 30 ⁇ m, may be 0.1 to 10 ⁇ m, may be 0.5 to 5 ⁇ m, may be 0.5 to 5 ⁇ m, and may be 1 to 1 ⁇ m. It may be 3 ⁇ m, or it may be 1 to 2 ⁇ m.
  • the average particle size of alumina can be 0.1 to 10 ⁇ m, may be 0.1 to 8 ⁇ m, or even be 0.1 to 7 ⁇ m from the viewpoint of the specific gravity of the heat conductive sheet 1. Well, it may be 0.1-3 ⁇ m.
  • the content of the other thermally conductive fillers 4 in the thermally conductive sheet 1 can be appropriately selected according to the purpose within the range that satisfies the condition 3 described above.
  • the content of aluminum nitride particles in the thermally conductive sheet 1 is 10 to 25% by volume (especially 17 to 23% by volume).
  • the content of alumina particles is preferably 10 to 25% by volume (especially 17 to 23% by volume).
  • the thermally conductive sheet 1 is a cured product of a composition containing a silicone resin as a binder resin 2, boron nitride as an anisotropic thermally conductive filler 3, and alumina and aluminum nitride as other thermally conductive fillers 4. It is preferable to consist of Moreover, in the heat conductive sheet 1, the content of boron nitride as the anisotropic heat conductive filler 3 is preferably more than 20% by volume and less than 35% by volume.
  • the heat conductive sheet 1 may further contain components other than the components described above within a range that does not impair the effects of the present technology.
  • Other components include, for example, coupling agents, dispersants, curing accelerators, retarders, tackifiers, plasticizers, flame retardants, antioxidants, stabilizers, colorants, solvents and the like.
  • the thermally conductive sheet 1 includes the anisotropic thermally conductive filler 3 and/or Alternatively, other thermally conductive fillers 4 treated with a coupling agent may be used.
  • the manufacturing method of the thermally conductive sheet 1 has the following process A, process B, and process C.
  • step A by dispersing the anisotropic thermally conductive filler 3 and the other thermally conductive filler 4 in the binder resin 2, the binder resin 2, the anisotropic thermally conductive filler 3, and the other thermally conductive
  • a thermally conductive composition which contains a conductive filler 4.
  • the thermally conductive composition contains the above-described other components as necessary, and is uniformly mixed by a known method. It can be prepared by mixing.
  • step B the thermally conductive composition prepared in step A is extruded and then cured to obtain a columnar cured product (molded block).
  • the method of extrusion molding is not particularly limited, and various known extrusion molding methods can be appropriately employed depending on the viscosity of the thermally conductive composition, the properties required for the thermally conductive sheet 1, and the like.
  • the extrusion molding method when the thermally conductive composition is extruded through a die, the binder resin 2 in the thermally conductive composition flows, and the anisotropic thermally conductive filler 3 is oriented along the flow direction.
  • the size and shape of the columnar cured product obtained in step B can be determined according to the required size of the heat conductive sheet 1.
  • a rectangular parallelepiped having a cross-sectional length of 0.5 to 15 cm and a width of 0.5 to 15 cm can be used.
  • the length of the rectangular parallelepiped may be determined as required.
  • step C the column-shaped cured product obtained in step B is cut into a predetermined thickness in the length direction of the column to obtain the heat conductive sheet 1 .
  • the anisotropic thermally conductive filler 3 is exposed on the surface (cut surface) of the thermally conductive sheet 1 obtained in step C.
  • the cutting method is not particularly limited, and can be appropriately selected from known slicing devices (preferably an ultrasonic cutter) according to the size and mechanical strength of the cured columnar product.
  • the cutting direction of the columnar cured product is 60 to 120 degrees with respect to the extrusion direction because the anisotropic thermally conductive filler 3 is oriented in the extrusion direction in some cases.
  • the cutting direction of the columnar cured product is not particularly limited except for the above, and can be appropriately selected according to the purpose of use of the heat conductive sheet 1 and the like.
  • the method for manufacturing the thermally conductive sheet 1 is not limited to the example described above, and for example, after the step C, the step D of pressing the cut surface may be further included.
  • the step D of pressing By further including the step D of pressing, the surface of the heat conductive sheet 1 obtained in the step C is made smoother, and the adhesion with other members can be further improved.
  • a pair of pressing devices comprising a flat plate and a press head having a flat surface can be used.
  • the pressure for pressing can be, for example, 0.1 to 100 MPa.
  • the pressing temperature can be from 0 to 180.degree. C., can be within the temperature range of room temperature (eg, 25.degree. C.) to 100.degree.
  • the thermally conductive sheet 1 is, for example, an electronic device (thermal device) having a structure arranged between a heat generating body and a radiator so that the heat generated by the heat generating body is released to the heat radiator.
  • An electronic device has at least a heating element, a radiator, and a thermally conductive sheet 1, and may further have other members as necessary.
  • the heating element is not particularly limited, for example, integrated circuit elements such as CPU, GPU (Graphics Processing Unit), DRAM (Dynamic Random Access Memory), flash memory, transistors, resistors, etc. Electronic parts that generate heat in electric circuits etc.
  • the heating element also includes components for receiving optical signals, such as optical transceivers in communication equipment.
  • the radiator is not particularly limited, and examples include those used in combination with integrated circuit elements, transistors, optical transceiver housings, such as heat sinks and heat spreaders.
  • Materials for the heat sink and heat spreader include, for example, copper and aluminum.
  • a heat pipe is, for example, a cylindrical, substantially cylindrical, or flat cylindrical hollow structure.
  • FIG. 4 is a cross-sectional view showing an example of a semiconductor device to which a heat conductive sheet is applied.
  • the heat conductive sheet 1 is mounted on a semiconductor device 50 built in various electronic devices, and sandwiched between a heat generator and a radiator.
  • a semiconductor device 50 shown in FIG. 4 includes an electronic component 51 , a heat spreader 52 , and a heat conductive sheet 1 .
  • sandwiching the heat conductive sheet 1 between the heat spreader 52 and the heat sink 53 , together with the heat spreader 52 a heat dissipation member for dissipating the heat of the electronic component 51 is configured.
  • the mounting location of the heat conductive sheet 1 is not limited to between the heat spreader 52 and the electronic component 51 or between the heat spreader 52 and the heat sink 53, but can be appropriately selected according to the configuration of the electronic device or semiconductor device.
  • the heat spreader 52 is formed, for example, in the shape of a square plate, and has a main surface 52a facing the electronic component 51 and side walls 52b erected along the outer circumference of the main surface 52a.
  • the heat spreader 52 is provided with the heat conductive sheet 1 on the principal surface 52a surrounded by the side walls 52b, and is provided with the heat sink 53 via the heat conductive sheet 1 on the other surface 52c opposite to the principal surface 52a.
  • Example 1 33% by volume of silicone resin, 27% by volume of scaly boron nitride (D50 is 40 ⁇ m) whose crystal shape is hexagonal, 20% by volume of aluminum nitride (D50 is 1.2 ⁇ m), and spherical alumina particles (D50 is A thermally conductive composition was prepared by uniformly mixing 2 ⁇ m) with 20% by volume. This thermally conductive composition is poured into a mold (opening: 50 mm ⁇ 50 mm) having a rectangular parallelepiped internal space by an extrusion molding method, and heated in an oven at 60 ° C. for 4 hours to form a columnar cured product ( A compact block) was formed.
  • a mold opening: 50 mm ⁇ 50 mm
  • a release polyethylene terephthalate film was attached to the inner surface of the mold so that the release-treated surface faced the inside.
  • cutting (slicing) the obtained columnar cured product into a sheet having a thickness of 2 mm with an ultrasonic cutter in a direction substantially perpendicular to the length direction of the column scale-like boron nitride is obtained.
  • a heat conductive sheet oriented in the thickness direction of the sheet was obtained.
  • Example 2 In Example 2, 33% by volume of silicone resin, 27% by volume of scaly boron nitride (D50 is 30 ⁇ m) whose crystal shape is hexagonal, 20% by volume of aluminum nitride (D50 is 1.2 ⁇ m), and spherical A thermally conductive sheet was obtained in the same manner as in Example 1, except that a thermally conductive composition was prepared by uniformly mixing 20% by volume of alumina particles (D50: 2 ⁇ m).
  • Example 3 In Example 3, 37% by volume of silicone resin, 23% by volume of scaly boron nitride (D50 is 30 ⁇ m) whose crystal shape is hexagonal, 20% by volume of aluminum nitride (D50 is 1.2 ⁇ m), and spherical A thermally conductive sheet was obtained in the same manner as in Example 1, except that a thermally conductive composition was prepared by uniformly mixing 20% by volume of alumina particles (D50: 2 ⁇ m).
  • Example 4 In Example 4, 33% by volume of silicone resin, 27% by volume of scaly boron nitride (D50 is 20 ⁇ m) whose crystal shape is hexagonal, 20% by volume of aluminum nitride (D50 is 1.2 ⁇ m), and spherical A thermally conductive sheet was obtained in the same manner as in Example 1, except that a thermally conductive composition was prepared by uniformly mixing 20% by volume of alumina particles (D50: 2 ⁇ m).
  • Comparative Example 1 In Comparative Example 1, 40% by volume of silicone resin, 20% by volume of scaly boron nitride (D50 is 40 ⁇ m) having a hexagonal crystal shape, 30% by volume of aluminum nitride (D50 is 1.2 ⁇ m), and spherical A thermally conductive sheet was obtained in the same manner as in Example 1, except that a thermally conductive composition was prepared by uniformly mixing 10% by volume of alumina particles (D50: 2 ⁇ m).
  • Comparative Example 2 In Comparative Example 2, 40% by volume of silicone resin, 20% by volume of scaly boron nitride (D50 is 40 ⁇ m) having a hexagonal crystal shape, 20% by volume of aluminum nitride (D50 is 1.2 ⁇ m), and spherical A thermally conductive sheet was obtained in the same manner as in Example 1, except that a thermally conductive composition was prepared by uniformly mixing 20% by volume of alumina particles (D50: 2 ⁇ m).
  • Comparative Example 3 In Comparative Example 3, 40% by volume of silicone resin, 20% by volume of scaly boron nitride (D50 is 40 ⁇ m) whose crystal shape is hexagonal, 10% by volume of aluminum nitride (D50 is 1.2 ⁇ m), and spherical A thermally conductive sheet was obtained in the same manner as in Example 1, except that a thermally conductive composition was prepared by uniformly mixing 30% by volume of alumina particles (D50: 2 ⁇ m).
  • Comparative Example 4 In Comparative Example 4, 40% by volume of silicone resin, 20% by volume of scaly boron nitride (D50 is 20 ⁇ m) whose crystal shape is hexagonal, 20% by volume of aluminum nitride (D50 is 1.2 ⁇ m), and spherical A thermally conductive sheet was obtained in the same manner as in Example 1, except that a thermally conductive composition was prepared by uniformly mixing 20% by volume of alumina particles (D50: 2 ⁇ m).
  • Comparative Example 5 In Comparative Example 5, 25% by volume of silicone resin, 35% by volume of scaly boron nitride (D50 is 40 ⁇ m) whose crystal shape is hexagonal, 20% by volume of aluminum nitride (D50 is 1.2 ⁇ m), and spherical A thermally conductive composition was prepared by uniformly mixing 20% by volume of alumina particles (D50 of 2 ⁇ m).
  • Comparative Example 6 In Comparative Example 6, 33% by volume of silicone resin, 27% by volume of scaly boron nitride (D50 is 40 ⁇ m) whose crystal shape is hexagonal, 20% by volume of aluminum nitride (D50 is 1.2 ⁇ m), and spherical A thermally conductive composition was prepared by uniformly mixing 20% by volume of alumina particles (D50 of 2 ⁇ m). This thermally conductive composition was molded with a bar coater to a thickness of 2 mm and heated in an oven at 60° C. for 4 hours to obtain a thermally conductive sheet with a thickness of 2 mm.
  • scaly boron nitride D50 is 40 ⁇ m
  • aluminum nitride D50 is 1.2 ⁇ m
  • spherical A thermally conductive composition was prepared by uniformly mixing 20% by volume of alumina particles (D50 of 2 ⁇ m). This thermally conductive composition was molded with a bar coater to a thickness of 2
  • Comparative Example 7 In Comparative Example 7, 33% by volume of silicone resin, 27% by volume of scaly boron nitride (D50 is 50 ⁇ m) whose crystal shape is hexagonal, 20% by volume of aluminum nitride (D50 is 1.2 ⁇ m), and spherical A thermally conductive sheet was obtained in the same manner as in Example 1, except that a thermally conductive composition was prepared by uniformly mixing 20% by volume of alumina particles (D50: 2 ⁇ m).
  • Comparative Example 8 In Comparative Example 8, 33% by volume of silicone resin, 27% by volume of scaly boron nitride (D50 of 10 ⁇ m) having a hexagonal crystal shape, 20% by volume of aluminum nitride (D50 of 1.2 ⁇ m), and spherical A thermally conductive sheet was obtained in the same manner as in Example 1, except that a thermally conductive composition was prepared by uniformly mixing 20% by volume of alumina particles (D50: 2 ⁇ m).
  • ⁇ Bulk thermal conductivity> For bulk thermal conductivity, the thermal resistance of each thermal conductive sheet is measured by a method in accordance with ASTM-D5470, the horizontal axis is the thickness (mm) of the thermal conductive sheet at the time of measurement, and the vertical axis is the thermal resistance of the thermal conductive sheet ( °C ⁇ cm 2 /W) was plotted, and the bulk thermal conductivity (W/m ⁇ K) of the thermal conductive sheet was calculated from the slope of the plot.
  • the thermal resistance of the thermally conductive sheet was measured by preparing three types of thermally conductive sheets with different thicknesses and measuring the thermally conductive sheets with different thicknesses. Table 1 shows the results. In Table 1, "-" indicates that the bulk thermal conductivity could not be measured because the thermally conductive sheet could not be produced.
  • thermally conductive sheets obtained in Examples 1 to 4 consist of cured products of compositions containing binder resins, anisotropic thermally conductive fillers, and other thermally conductive fillers, and meet the conditions 1 to 3 described above. It was found that the thermal conductivity is high by satisfying
  • the quality of the manufactured heat conductive sheet can be determined, for example, the heat conductive sheet containing a predetermined amount of heat conductive filler having a predetermined particle size. It becomes possible to easily determine whether the sheet has a predetermined thermal conductivity.
  • Comparative Example 5 a heat conductive sheet could not be produced due to its high hardness.
  • the thermally conductive composition used in Comparative Example 5 had a total content of the anisotropic thermally conductive filler and other thermally conductive fillers of 75% by volume, which is considered to be because the above condition 3 was not satisfied.
  • thermally conductive sheet 1A surface, 2 binder resin, 3 anisotropic thermally conductive filler, 4 other thermally conductive filler, 5 virtual perpendicular line, 6 light beam, 51 electronic component, 52 heat spreader, 53 heat sink, 52a main surface, 52b side wall

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Abstract

L'invention concerne une feuille thermoconductrice ayant une conductivité thermique élevée, et pour laquelle une évaluation de réussite/échec d'une feuille thermoconductrice souhaitée peut facilement être réalisée.　La feuille thermoconductrice 1 comprend un produit durci d'une composition contenant une résine liante 2, une charge thermoconductrice anisotrope 3, et une autre charge thermiquement conductrice 4 autre que la charge thermoconductrice anisotrope 3, et satisfait les conditions 1-3 ci-dessous. [Condition 1] Une valeur de brillant mesurée selon un rayon lumineux 6 qui est incident à une position 60° par rapport à une ligne perpendiculaire virtuelle par rapport à la surface supérieure de la feuille thermoconductrice 1 est inférieure à 10. [Condition 2] La taille moyenne des particules de la charge thermoconductrice anisotrope 3 est de 15 µm à 45 µm. [Condition 3] Dans la feuille thermoconductrice 1, la teneur totale de la charge thermoconductrice anisotrope 3, et l'autre charge thermoconductrice 4 dépasse de 60 % en volume mais est inférieure à 75 % en volume.
PCT/JP2022/021880 2021-06-16 2022-05-30 Feuille thermoconductrice et procédé de production de feuille thermoconductrice WO2022264790A1 (fr)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014010521A1 (fr) * 2012-07-07 2014-01-16 デクセリアルズ株式会社 Procédé de fabrication de feuille thermo-conductrice
JP2015003953A (ja) * 2013-06-19 2015-01-08 デクセリアルズ株式会社 熱伝導性シート及び熱伝導性シートの製造方法
WO2016104169A1 (fr) * 2014-12-25 2016-06-30 デクセリアルズ株式会社 Procédé de fabrication de feuille thermoconductrice, feuille thermoconductrice et dispositif à semi-conducteur
JP2017115042A (ja) * 2015-12-24 2017-06-29 日東電工株式会社 グラファイトシート用粘着シート
WO2020050334A1 (fr) * 2018-09-07 2020-03-12 積水ポリマテック株式会社 Feuille thermoconductrice
JP6960554B1 (ja) * 2021-06-16 2021-11-05 デクセリアルズ株式会社 熱伝導シート及び熱伝導シートの製造方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014010521A1 (fr) * 2012-07-07 2014-01-16 デクセリアルズ株式会社 Procédé de fabrication de feuille thermo-conductrice
JP2015003953A (ja) * 2013-06-19 2015-01-08 デクセリアルズ株式会社 熱伝導性シート及び熱伝導性シートの製造方法
WO2016104169A1 (fr) * 2014-12-25 2016-06-30 デクセリアルズ株式会社 Procédé de fabrication de feuille thermoconductrice, feuille thermoconductrice et dispositif à semi-conducteur
JP2017115042A (ja) * 2015-12-24 2017-06-29 日東電工株式会社 グラファイトシート用粘着シート
WO2020050334A1 (fr) * 2018-09-07 2020-03-12 積水ポリマテック株式会社 Feuille thermoconductrice
JP6960554B1 (ja) * 2021-06-16 2021-11-05 デクセリアルズ株式会社 熱伝導シート及び熱伝導シートの製造方法

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