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WO2025166510A1 - Composition thermoconductrice et élément de dissipation de chaleur - Google Patents

Composition thermoconductrice et élément de dissipation de chaleur

Info

Publication number
WO2025166510A1
WO2025166510A1 PCT/CN2024/076121 CN2024076121W WO2025166510A1 WO 2025166510 A1 WO2025166510 A1 WO 2025166510A1 CN 2024076121 W CN2024076121 W CN 2024076121W WO 2025166510 A1 WO2025166510 A1 WO 2025166510A1
Authority
WO
WIPO (PCT)
Prior art keywords
thermal conductive
conductive composition
diamond particles
composition according
silicone resin
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
PCT/CN2024/076121
Other languages
English (en)
Inventor
Hengda YU
Dan XIE
Dan Li
Jianguo KANG
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Henkel China Co Ltd
Henkel AG and Co KGaA
Original Assignee
Henkel China Co Ltd
Henkel AG and Co KGaA
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Henkel China Co Ltd, Henkel AG and Co KGaA filed Critical Henkel China Co Ltd
Priority to PCT/CN2024/076121 priority Critical patent/WO2025166510A1/fr
Publication of WO2025166510A1 publication Critical patent/WO2025166510A1/fr
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C08K9/06—Ingredients treated with organic substances with 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
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • 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
    • H01L23/3737—Organic materials with or without a thermoconductive filler

Definitions

  • heat-dissipating members can be installed inside or outside the devices, for example, between electronic devices and housings, heat sinks or the like.
  • the heat-dissipating members are usually formed of heat dissipating resin compositions, which are produced by dispersing and mixing thermal conductive fillers in a polymer matrix, for example, silicone resin.
  • thermal conductive fillers such as aluminum nitride, alumina, magnesium oxide, boron nitride, however, super high thermal conductivity can’ t be achieved, for example, of above 15W/m ⁇ K.
  • diamond powder is introduced in the field of heat dissipation of electronic devices due to its natural high conductivity of around 1000W/m ⁇ K, and electric insulativity at room temperature.
  • it due to its inert chemical property, it’s difficult for the diamond powder to be mixed and dispersed well with polymer matrix and other types of fillers such as aluminum nitride and alumina, and therefore, its thermal conductive effect and thus heat dissipation benefit can’t be utilized to a maximum extent.
  • the present inventor has found that by surface treating diamond particles having a controlled particle size with a particular surface treating agent, the diamond particles can be easily and homogenously dispersed in the polymer matrix, resulting in a thermal conductive composition having improved flowability and storage stability, and excellent thermal conductivity.
  • the present invention provides a thermal conductive composition, comprising a polymer matrix, and diamond particles having an average particle size D50 of about 20 to 150 ⁇ m which are surface treated with an alkylalkoxysilane compound having about 9 to 16 carbon atoms in the alkyl group in an amount of more than 0.03 wt. %and less than 0.7wt. %based on the weight of diamond particles.
  • the present invention provides a heat dissipating member obtained by curing the thermal conductive composition.
  • the thermal conductive composition according to the present invention comprises a polymer matrix and surface-treated diamond particles.
  • the thermal conductive composition exhibits improved flowability and thermal conductivity, and at the same time exhibits excellent storage stability and thixotropy, which are desirable for dispensing process in the manufacturing of electronic assembly.
  • the thermal conductive composition according to the present invention comprises a polymer matrix.
  • the polymer matrix suitable for use in the present invention can be of any type conventionally used in a thermal conductive polymer composition material.
  • suitable polymer matrix include, but are not limited to, resins, for example, silicone resins, epoxy resins and polyurethane resins, and silicone oil, for example, methylphenyl silicone oil, dimethylsilicone oil, and modified silicone oil.
  • epoxy resins mention may be made of epoxy compounds having at least one, preferably two or more epoxy groups, examples of which include bisphenol-type epoxy resin, novolac-type epoxy resin, diphenyl-type epoxy resin, and naphthalene-type epoxy resin etc.
  • the thermal conductive composition according to the present invention comprises a silicone resin.
  • the silicone resin may be condensation curable type silicone resin, or addition reaction-curable type silicone resin, with addition reaction-curable type silicone resin being more preferable.
  • the unsaturated group-containing polyorganosiloxane is preferably a polyorganosiloxane having alkenyl group, more preferably vinyl group, examples of which include vinyl-terminated polyorganosiloxane, for example, vinyl-terminated polydimethylsiloxane, vinyl-terminated polydimethylmethylvinylsiloxane, vinyl-terminated polydimethylmethylphenylsiloxane, vinyl-terminated polydimethyldiphenylsiloxane.
  • the thermal conductive composition according to the present invention comprises diamond particles as described below as a thermal conductive filler.
  • the diamond particles to be used have an average particle size D50 of about 20 to 150 ⁇ m, preferably about 25 to 130 ⁇ m. If the average particle size is lower than about 20 ⁇ m, generally synthetic diamond particles of below 20 ⁇ m have irregular shape which will affect thermal conductivity and viscosity of the composition. If the average particle size is larger than about 150 ⁇ m, the filler will affect the bondline thickness (BLT) and compression force of electronic assembly.
  • BLT bondline thickness
  • the diamond particles to be used in the thermal conductive composition according to the invention have been surface treated with an alkylalkoxy silane compound comprising about 9 to 16, preferably about 10 to 16, more preferably about 11 to 15 carbon atoms in the alkyl group.
  • alkylalkoxysilane compound examples include, but are not limited to, octyltrimethoxysilane, octyltriethoxysilane, decyltrimethoxysilane, decyltriethoxysilane, dodecyltrimethoxysilane, dodecyltriethoxysilane, tetradecyltrimethoxysilane, tetradecyltriethoxysilane, hexadecyltrimethoxysilane, hexadecyltriethoxysilane, methyl-octyldimethoxysilane, methyl-octyldiethoxysilane, methydecyldimethoxysilane, methyldodecyldimethoxysilane, methylhexadecyldimethoxysilane.
  • the amount of the silane compound to be used as a surface treating agent is greater than 0.03wt. %and smaller than 0.07wt. %, and preferably is about 0.04 to 0.55wt. %, relative to the weight of the diamond particles.
  • a method for surface treating the diamond particles with the silane compound is not especially limited, and as known in the art, there can be used, for example, a wet treatment method, a dry treatment method, or a combination thereof.
  • the wet treatment method comprises the steps of adding the diamond particles in a solution in which the silane compound is dispersed, mixing the mixture and then heat treating the mixture at a temperature of normally about 50 to 90 °C.
  • the thermal conductive composition may contain from 25 to 75 wt. %, preferably from 35 to 65 wt. %of the diamond particles, based on the total weight of the composition.
  • the thermal conductive composition may further preferably comprise other thermal conductive fillers conventionally used in the art than the diamond particles.
  • thermal conductive fillers include, but are not limited to, alumina, magnesium oxide, zinc oxide, boron nitride, aluminum nitride, etc. This other thermal conductive filler may be used in a single type or in combination of two or more types.
  • the thermal conductive fillers may have an average particle size D50 of 0.1 to 200 ⁇ m.
  • the thermal conductive composition according to the invention may further comprise other additives conventionally used for heat dissipating member, for example, reactor inhibitor, dispersant, antioxidant, thermal stabilizer, pigments, and flame retardant according to actual needs.
  • additives conventionally used for heat dissipating member for example, reactor inhibitor, dispersant, antioxidant, thermal stabilizer, pigments, and flame retardant according to actual needs.
  • the thermal conductive composition comprises a dispersant, to facilitate dispersion of the thermal conductive fillers in the polymer matrix of the composition.
  • a dispersant silicone-based or non-silicone based dispersant can be used, for example, polydimethylsiloxane, hydroxyl-functional polydimethylsiloxane, fatty acids, polyacrylates.
  • the amount of the dispersant to be used in the composition may be, based on the total weight of the composition, from about 0.1 to 5wt. %, preferably about 0.5 to 2wt. %.
  • the thermal conductive composition according to the invention can be prepared by mixing the polymer matrix, the diamond particles, and further optionally other thermal conductive fillers, and additives as described above.
  • a two-component curing type silicone resin is used as the polymer matrix, and in this case, as described above, the thermal conductive composition can be prepared by mixing a first component comprising the unsaturated group-containing polyorganosiloxane and a second component comprising the hydrogen group-containing polyorganosiloxane, which have been prepared separately.
  • the diamond particles, the other thermal conductive fillers and the optional additives can be comprised in either or both of the first component and the second component.
  • the first component can be prepared by mixing the unsaturated group-containing polyorganosiloxane, the platinum compound catalyst, the diamond particles, other thermal conductive fillers, and additives comprising for example a dispersant, a reaction inhibitor and a pigment
  • the second component can be prepared by mixing the hydrogen group-containing polyorganosiloxane, the diamond particles, other thermal conductive fillers, and an additive for example a pigment.
  • the mixing can be done by any known mixing apparatus, which can be selected by a skilled person according to practical requirement, at a temperature of normally from about 20°C to 140°C, preferably about 60°C to 120°C.
  • a planetary mixer, a kneader, a static mixer, or any combination thereof can be used.
  • the thermal conductive composition according to the present invention exhibits an excellent property portfolio of initial flow rate, aged flow rate, thixotropy, and storage stability.
  • the present invention provides a heat dissipating member, which is obtained by curing the above thermal conductive composition.
  • the thermal conductive composition can be cured by heating, or without being heated.
  • the composition can be cured at normal temperature, for example about 25°C after 24 to 48 hours, or the composition can be cured by heating at about 60-80°C for about 0.5 to 2 hours.
  • the obtained heat dissipating member according to the present invention has an excellent thermal conductivity of above 15.00 W/m ⁇ K.
  • the heat dissipating member according to the present invention is suitable for use in a wide variety of electronic devices and electronic components, for example, CPUs, chipsets, hard disk drives, power transistors, etc.
  • Raw Diamond particles-A average particle size of 115 ⁇ m, specific surface area of 0.050 m 2 /g, available from Guangzhou Fanya Jiarong Trading Co., Ltd.;
  • Raw Diamond particles-B average particle size of 45 ⁇ m, specific surface area of 0.140 m 2 /g, available from Guangzhou Fanya Jiarong Trading Co., Ltd.;
  • Raw Diamond particles-C average particle size of 25 ⁇ m, specific surface area of 0.25 m 2 /g, available from Guangzhou Fanya Jiarong Trading Co., Ltd.;
  • Vinyl-terminated polysiloxane trade name: RH-Vi321, available from Ningbo Runhe High-tech Material Co., Ltd.;
  • Hydride-terminated polydimethylsiloxane trade name: XL1-7501, available from Nusil Technology LLC.;
  • Trimethyl-terminated polymethyhydrogenlsiloxane trade name: RH-H33, available from Ningbo Runhe High-tech Material Co., Ltd.;
  • Polydimethylsiloxane trade name: KF-96-50CS, available from Shin-Etsu;
  • Platinum Catalyst Karstedt Catalyst, having a Pt content of 2%, trade name: CAT1-50, available from Nusil Technology LLC;
  • Inhibitor 1, 3, 5, 7-tetramethyl-1, 3, 5, 7-tetravinyl-cyclotetrasiloxane, trade name: XL-119, available from Nusil Technology LLC;
  • Filler dispersant trade name: LP-X-21879, available from BYK;
  • Pigment trade name: Sunfast Blue 15: 4 &Sunfast Green 7, available from Qingdao Sun Chemical Corporation;
  • Aluminum Nitride-1 average particle size of 120 ⁇ m, trade name: AN120, available from Suzhou Ginet New Material Technology Co., Ltd.;
  • Aluminum Nitride-2 average particle size of 25 ⁇ m, trade name: AN30, available from Suzhou Ginet New Material Technology Co., Ltd.;
  • Aluminum Nitride-3 average particle size of 5 ⁇ m, trade name: AN5, available from Suzhou Ginet New Material Technology Co., Ltd.;
  • Alumina average particle size of 0.3 ⁇ m, trade name: Y06-1, available from Suzhou Ginet New Material Technology Co., Ltd.
  • Part A (a first component) was prepared by first mixing the ingredients except for the inhibitor and platinum catalyst in a planetary mixer at a speed of 25 rpm and at normal temperature for 30 minutes, and then at a speed of 20rpm and at a temperature of 100 to 150°C for 1 hour, and cooling to 30°C, followed by adding the inhibitor and platinum catalyst and mixing for additional 30 minutes.
  • Part B was prepared by mixing the respective ingredients in a planetary mixer at a speed of 25 rpm and at normal temperature for 30 minutes, and then at a speed of 20rpm and at a temperature of 100 to 150°C for 1 hour, and cooling to 30°C.
  • the thermal conductive compositions were then applied on the test plate of LW-9389 Thermal Tester, with test condition being 80°C for 30 minutes and the compositions were online cured. The cured products were then subjected to a thermal conductivity test.
  • Viscosity was measured at 25°C on a Rheometer (Discovery HR-30, manufactured by TA instruments Inc. ) using a plate-plate geometry with a 25mm in diameter plate at a 1.0mm gap and at a shear rate of 0.1s -1 and 1.0s -1 .
  • the thixotropy was calculated by the following equation:
  • Example 7 using treated diamond particles having a greater average particle size in Example 6 further improves the combined properties of thixotropy, flow rate reliability and thermal conductivity to some extent. According to the present invention, therefore, the average particle size of the diamond particles should be controlled to be not lower than about 20 ⁇ m.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

La présente invention concerne une composition thermoconductrice, et un élément de dissipation de chaleur comprenant la composition thermoconductrice.
PCT/CN2024/076121 2024-02-05 2024-02-05 Composition thermoconductrice et élément de dissipation de chaleur Pending WO2025166510A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/CN2024/076121 WO2025166510A1 (fr) 2024-02-05 2024-02-05 Composition thermoconductrice et élément de dissipation de chaleur

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/CN2024/076121 WO2025166510A1 (fr) 2024-02-05 2024-02-05 Composition thermoconductrice et élément de dissipation de chaleur

Publications (1)

Publication Number Publication Date
WO2025166510A1 true WO2025166510A1 (fr) 2025-08-14

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ID=96698923

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2024/076121 Pending WO2025166510A1 (fr) 2024-02-05 2024-02-05 Composition thermoconductrice et élément de dissipation de chaleur

Country Status (1)

Country Link
WO (1) WO2025166510A1 (fr)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030234074A1 (en) * 2002-06-25 2003-12-25 Bhagwagar Dorab Edul Thermal interface materials and methods for their preparation and use
US20060292840A1 (en) * 2003-11-05 2006-12-28 Dow Corning Corporation Thermally conductive grease and methods and devices in which said grease is used
CN111032665A (zh) * 2017-08-10 2020-04-17 信越化学工业株式会社 有机硅化合物及固化性导热性硅酮组合物
CN112204106A (zh) * 2018-05-31 2021-01-08 积水化学工业株式会社 散热组合物、散热构件及散热构件用填料集合体
CN113508460A (zh) * 2019-03-29 2021-10-15 陶氏东丽株式会社 多成分型固化性聚有机硅氧烷组合物、导热性构件以及散热结构体
US20210332280A1 (en) * 2018-11-07 2021-10-28 Dow Global Technologies Llc Thermally conductive composition and methods and devices in which said composition is used

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030234074A1 (en) * 2002-06-25 2003-12-25 Bhagwagar Dorab Edul Thermal interface materials and methods for their preparation and use
US20060292840A1 (en) * 2003-11-05 2006-12-28 Dow Corning Corporation Thermally conductive grease and methods and devices in which said grease is used
CN111032665A (zh) * 2017-08-10 2020-04-17 信越化学工业株式会社 有机硅化合物及固化性导热性硅酮组合物
CN112204106A (zh) * 2018-05-31 2021-01-08 积水化学工业株式会社 散热组合物、散热构件及散热构件用填料集合体
US20210332280A1 (en) * 2018-11-07 2021-10-28 Dow Global Technologies Llc Thermally conductive composition and methods and devices in which said composition is used
CN113508460A (zh) * 2019-03-29 2021-10-15 陶氏东丽株式会社 多成分型固化性聚有机硅氧烷组合物、导热性构件以及散热结构体

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