JP2005330426A - Heat-dissipating silicone grease composition - Google Patents
Heat-dissipating silicone grease composition Download PDFInfo
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- JP2005330426A JP2005330426A JP2004151706A JP2004151706A JP2005330426A JP 2005330426 A JP2005330426 A JP 2005330426A JP 2004151706 A JP2004151706 A JP 2004151706A JP 2004151706 A JP2004151706 A JP 2004151706A JP 2005330426 A JP2005330426 A JP 2005330426A
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- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 68
- 239000004519 grease Substances 0.000 title claims abstract description 67
- 239000000203 mixture Substances 0.000 title claims abstract description 65
- 239000000843 powder Substances 0.000 claims abstract description 22
- 239000002245 particle Substances 0.000 claims abstract description 19
- 229910052751 metal Inorganic materials 0.000 claims abstract description 6
- 239000002184 metal Substances 0.000 claims abstract description 6
- 239000000919 ceramic Substances 0.000 claims abstract description 5
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 5
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 5
- 125000001183 hydrocarbyl group Chemical group 0.000 claims abstract description 4
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 4
- 239000011362 coarse particle Substances 0.000 claims description 29
- 230000017525 heat dissipation Effects 0.000 claims description 25
- 125000004432 carbon atom Chemical group C* 0.000 claims description 3
- 239000000945 filler Substances 0.000 claims description 3
- 239000011231 conductive filler Substances 0.000 abstract description 23
- 230000000694 effects Effects 0.000 abstract description 9
- 230000000717 retained effect Effects 0.000 abstract 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 15
- 239000000463 material Substances 0.000 description 9
- 239000006185 dispersion Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- -1 2-methyl-2-phenylethyl group Chemical group 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 230000000191 radiation effect Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 125000000094 2-phenylethyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 125000003342 alkenyl group Chemical group 0.000 description 1
- 125000003710 aryl alkyl group Chemical group 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 125000001511 cyclopentyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C1([H])[H] 0.000 description 1
- 125000002704 decyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 125000005816 fluoropropyl group Chemical group [H]C([H])(F)C([H])([H])C([H])([H])* 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 150000008282 halocarbons Chemical group 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 125000001421 myristyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 125000003854 p-chlorophenyl group Chemical group [H]C1=C([H])C(*)=C([H])C([H])=C1Cl 0.000 description 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229930195734 saturated hydrocarbon Natural products 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- 229930195735 unsaturated hydrocarbon Natural products 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
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- Lubricants (AREA)
- Cooling Or The Like Of Semiconductors Or Solid State Devices (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
Description
本発明は、特に放熱特性に優れた放熱用シリコーングリース組成物に関する。 The present invention relates to a heat-dissipating silicone grease composition that is particularly excellent in heat dissipation characteristics.
電気部品の多くは使用中に熱が発生するので、その電気部品を適切に機能させるためには熱を取り除くことが必要である。この除熱のため、多くの熱伝導性材料が提案されている。熱伝導性材料の形態には、大きく分けて取り扱いが容易であるシート状のものと、ペースト状の一般的に放熱グリースと呼ばれるものの２種類がある。熱抵抗は、放熱材料の厚みに比例するため、一般的には、加圧することで容易に材料そのものが薄くなる放熱グリースの方が放熱特性はよい。 Many electrical components generate heat during use, and it is necessary to remove the heat in order for the electrical components to function properly. Many heat conductive materials have been proposed for this heat removal. There are two types of thermally conductive materials: a sheet-like material that is easy to handle and a paste-like material generally called heat dissipating grease. Since the thermal resistance is proportional to the thickness of the heat radiating material, in general, the heat radiating grease is better in heat radiating characteristics because the material itself is easily thinned by pressurization.
しかしながら、近年益々ＬＳＩ等の素子の発熱量が上がってくると、通常の放熱グリースでは十分な放熱効果が得られなくなってきた。放熱グリースの性能を上げるためには、ひとつには熱伝導性充填材を高度に充填する方法がある。しかしながら、熱伝導性充填材を高度に充填すると、放熱グリースの粘度が上がりすぎるため、使い勝手の面で限界がある。もう一つの手段としては、熱抵抗は放熱材料の厚みに比例するため、放熱グリースの塗り厚を薄くする方法がある。そのためには、一般的には平均粒径の小さいものを熱伝導性充填材として使用するが、それでも十分な放熱効果は得られなかった。それは、平均粒径の小さな熱伝導性充填材を使用しても、熱伝導性充填材に予期せぬ粗粒が混入しているため、塗布時放熱グリースが所望する薄さになっていないことが原因であった。 However, as the amount of heat generated by elements such as LSIs has increased in recent years, it has become impossible to obtain a sufficient heat radiation effect with ordinary heat radiation grease. In order to improve the performance of the heat dissipating grease, there is a method of highly filling the heat conductive filler. However, when the heat conductive filler is filled to a high degree, the viscosity of the heat dissipating grease increases too much, so that there is a limit in usability. As another means, since the thermal resistance is proportional to the thickness of the heat dissipating material, there is a method of reducing the coating thickness of the heat dissipating grease. For this purpose, a material having a small average particle diameter is generally used as the heat conductive filler, but still a sufficient heat dissipation effect was not obtained. That is, even if a heat conductive filler with a small average particle size is used, unexpectedly coarse particles are mixed in the heat conductive filler, so that the heat dissipation grease is not as thin as desired. Was the cause.
なお、本発明に関連する公知文献としては、下記のものがある。
本発明は、上記事情に鑑みなされたもので、好適な放熱効果を発揮する放熱用シリコーングリース組成物を提供することを目的とする。 This invention is made | formed in view of the said situation, and it aims at providing the silicone grease composition for thermal radiation which exhibits a suitable thermal radiation effect.
本発明者は、上記目的を達成するため鋭意検討した結果、（Ａ）熱伝導率が１０Ｗ／ｍ℃以上、且つ平均粒径が０．１〜１５．０μｍである金属粉末、金属酸化物粉末及びセラミック粉末から選ばれる１種又は２種以上の熱伝導性充填材：６０〜９８質量％、（Ｂ）式（１）で表される２５℃における動粘度が５０〜５００，０００ｍｍ2／ｓのオルガノポリシロキサン：２〜４０質量％を含有してなる放熱用シリコーングリース組成物において、５００メッシュ（２５μｍ目開き）オンの粗粒質量が、該組成物中５０ｐｐｍ以下であり、且つ３２５メッシュ（４５μｍ目開き）オンの粗粒が実質的にゼロであるように熱伝導性充填材の粗粒を高度に取り除くことで、放熱用シリコーングリース組成物の塗布厚さを極めて薄くすることができ、好適な放熱効果を発揮することを見出し、本発明をなすに至ったものである。 As a result of intensive studies to achieve the above object, the present inventor has (A) a metal powder and a metal oxide powder having a thermal conductivity of 10 W / m ° C. or higher and an average particle size of 0.1 to 15.0 μm. And one or more heat conductive fillers selected from ceramic powders: 60 to 98% by mass, (B) kinematic viscosity at 25 ° C. represented by formula (1) is 50 to 500,000 mm 2 / s The heat-dissipating silicone grease composition containing 2 to 40% by mass of the organopolysiloxane of the present invention has a coarse particle mass of 500 mesh (25 μm aperture) on and not more than 50 ppm in the composition, and 325 mesh ( The coating thickness of the heat-dissipating silicone grease composition can be made extremely thin by removing the coarse particles of the thermally conductive filler so that the coarse particles of ON are substantially zero. Found to exhibit optimal heat dissipation effect are those able to complete the present invention.
従って、本発明は、下記の放熱用シリコーングリース組成物を提供する。
〔１〕（Ａ）熱伝導率が１０Ｗ／ｍ℃以上、且つ平均粒径が０．１〜１５．０μｍである金属粉末、金属酸化物粉末及びセラミック粉末から選ばれる１種又は２種以上の熱伝導性充填材 ６０〜９８質量％
（Ｂ）下記平均組成式（１）
Ｒ1 aＳｉＯ(4-a)/2 ・・・・・（１）
〔式中、Ｒ1は独立に炭素数１〜１８の飽和又は不飽和の１価炭化水素基であり、ａは１．８≦ａ≦２．２の正数である。〕
で表される２５℃における動粘度が５０〜５００，０００ｍｍ2／ｓのオルガノポリシロキサン ２〜４０質量％
を含有してなる放熱用シリコーングリース組成物において、５００メッシュ（２５μｍ目開き）オンの粗粒質量が、放熱用シリコーングリース組成物中５０ｐｐｍ以下であり、且つ３２５メッシュ（４５μｍ目開き）オンの粗粒が実質的にゼロであることを特徴とする放熱用シリコーングリース組成物。
〔２〕放熱用シリコーングリース組成物を０．１５ＭＰａの圧力で押しつぶした時の厚さが２５μｍ以下であることを特徴とする〔１〕記載の放熱用シリコーングリース組成物。
Accordingly, the present invention provides the following heat-dissipating silicone grease composition.
[1] (A) One or more kinds selected from metal powder, metal oxide powder and ceramic powder having a thermal conductivity of 10 W / m ° C. or more and an average particle diameter of 0.1 to 15.0 μm Thermally conductive filler 60-98% by mass
(B) The following average composition formula (1)
R 1 a SiO (4-a) / 2 (1)
[Wherein, R 1 is independently a saturated or unsaturated monovalent hydrocarbon group having 1 to 18 carbon atoms, and a is a positive number of 1.8 ≦ a ≦ 2.2. ]
2 to 40% by mass of an organopolysiloxane having a kinematic viscosity of 50 to 500,000 mm 2 / s at 25 ° C.
In the heat-dissipating silicone grease composition, the coarse particle mass of 500 mesh (25 μm openings) -on is 50 ppm or less in the heat-dissipating silicone grease composition and 325 mesh (45 μm openings) -on coarse A silicone grease composition for heat dissipation, characterized in that the number of grains is substantially zero.
[2] The heat-dissipating silicone grease composition according to [1], wherein the heat-dissipating silicone grease composition has a thickness of 25 μm or less when crushed with a pressure of 0.15 MPa.
本発明の放熱用シリコーングリース組成物は、好適な放熱効果を発揮する。 The silicone grease composition for heat dissipation of the present invention exhibits a suitable heat dissipation effect.
本発明の放熱用シリコーングリース組成物は、５００メッシュ（２５μｍ目開き）オンの粗粒質量が、放熱用シリコーングリース組成物に対して５０ｐｐｍより大きいと放熱用シリコーングリース組成物の膜厚さを十分に薄くすることができず、所望する放熱効果が得られないため、５０ｐｐｍ以下、好ましくは３０ｐｐｍ以下であることが必要である。また、５００メッシュ（２５μｍ目開き）オンの粗粒質量が仮に５０ｐｐｍ以下であっても、一粒大きな粗粒が放熱用シリコーングリース組成物中に存在している場合もあり、当然このケースでは放熱用シリコーングリース組成物が十分に薄くならず、所望する放熱効果が得られない。従って、所望の放熱効果を得るためには、同時に３２５メッシュ（４５μｍ目開き）オンの粗粒が、実質的にゼロであることが必要である。 The heat-dissipating silicone grease composition of the present invention has a sufficient film thickness of the heat-dissipating silicone grease composition when the coarse particle mass of 500 mesh (25 μm openings) is larger than 50 ppm with respect to the heat-dissipating silicone grease composition. Therefore, it is necessary to be 50 ppm or less, preferably 30 ppm or less because the desired heat dissipation effect cannot be obtained. Further, even if the coarse particle mass of 500 mesh (25 μm aperture) ON is 50 ppm or less, one large coarse particle may be present in the heat-dissipating silicone grease composition. The silicone grease composition for use is not sufficiently thin and the desired heat dissipation effect cannot be obtained. Therefore, in order to obtain a desired heat radiation effect, it is necessary that the number of coarse particles having 325 mesh (45 μm openings) on is substantially zero at the same time.
放熱用シリコーングリース組成物から粗粒を取り除くには、放熱用シリコーングリース組成物を直接５００メッシュ（目開き２５μｍ）で濾過する方法もあるが、放熱用シリコーングリース組成物のように高度に熱伝導性充填材が入っているような材料を濾過することは現実的には難しく、やはり熱伝導性充填材から粗粒を取り除くことが好ましい。 In order to remove coarse particles from the heat-dissipating silicone grease composition, there is a method of directly filtering the heat-dissipating silicone grease composition through a 500 mesh (aperture 25 μm), but it is highly heat conductive like the heat-dissipating silicone grease composition. It is practically difficult to filter a material containing a conductive filler, and it is also preferable to remove coarse particles from the thermally conductive filler.
本発明に用いられる（Ａ）成分の熱伝導性充填材は、その充填材のもつ熱伝導率が１０Ｗ／ｍ℃より小さいと、放熱用シリコーングリース組成物の熱伝導率そのものが小さくなるため、熱伝導性充填材の熱伝導率は１０Ｗ／ｍ℃以上であることが必要である。 When the thermal conductivity of the component (A) used in the present invention is less than 10 W / m ° C., the thermal conductivity of the silicone grease composition for heat dissipation itself becomes small. The thermal conductivity of the thermally conductive filler is required to be 10 W / m ° C. or higher.
熱伝導性充填材の形状は、不定形でも球形でも如何なる形状でも構わないが、球状であることが好ましい。熱伝導性充填材の平均粒径は、０．１μｍより小さいとグリース状にならず、伸展性に乏しいものとなるし、１５．０μｍより大きいとシリコーングリース組成物を塗布した際に十分に薄くならず、放熱効果が小さくなるので、０．１〜１５．０μｍの範囲であり、好ましくは０．３〜８．０μｍの範囲である。なお、本発明において、平均粒径は、Ｍｉｃｒｏｔｒａｃ社製ＭＴ３０００（型式）により測定した値である。 The shape of the heat conductive filler may be indefinite, spherical, or any shape, but is preferably spherical. If the average particle size of the thermally conductive filler is smaller than 0.1 μm, it does not become grease-like and has poor extensibility, and if it is larger than 15.0 μm, it is sufficiently thin when a silicone grease composition is applied. However, since the heat dissipation effect becomes small, it is in the range of 0.1 to 15.0 μm, preferably in the range of 0.3 to 8.0 μm. In the present invention, the average particle size is a value measured by MT3000 (model) manufactured by Microtrac.
このような熱伝導性充填材としては、金属粉末、金属酸化物粉末、セラミック粉末が用いられ、具体的には、アルミニウム粉末、銅粉末、銀粉末、ニッケル粉末、金粉末、酸化アルミニウム粉末、酸化亜鉛粉末、酸化マグネシウム粉末、窒化アルミニウム粉末、窒化ホウ素粉末、窒化珪素粉末、ダイヤモンド粉末、カーボン粉末などが挙げられるが、熱伝導率が１０Ｗ／ｍ℃以上且つ平均粒径が０．１〜１５．０μｍの間であれば如何なる充填材でもよく、これらは１種類単独であるいは２種類以上混ぜ合わせてもよい。 As such a heat conductive filler, metal powder, metal oxide powder and ceramic powder are used. Specifically, aluminum powder, copper powder, silver powder, nickel powder, gold powder, aluminum oxide powder, oxidation powder are used. Examples thereof include zinc powder, magnesium oxide powder, aluminum nitride powder, boron nitride powder, silicon nitride powder, diamond powder, and carbon powder. The thermal conductivity is 10 W / m ° C. or more and the average particle size is 0.1 to 15. Any filler may be used as long as it is between 0 μm, and these may be used alone or in combination of two or more.
なお、本発明の熱伝導性充填材は、上述したように、５００メッシュ（２５μｍ目開き）オンの粗粒が、得られるシリコーングリース組成物中の５０ｐｐｍ以下となる量、更に３２５メッシュ（４５μｍ目開き）オンの粗粒が、実質的に配合されていないことが必要である。 In addition, as described above, the thermally conductive filler of the present invention has an amount of coarse particles having a 500 mesh (25 μm mesh) ON coarseness of 50 ppm or less in the obtained silicone grease composition, and further 325 mesh (45 μm mesh). Open) It is necessary that the coarse particles of ON are not substantially blended.
熱伝導性充填材等のフィラーを製造するメーカーが、粒度分布を測定し、検査表などに値を載せているが、絶対量が少ない粗粒は一般的には粒度分布測定装置では検出できない。従って、同じ材料、同じ平均粒径のものを使っても粗粒を取り除いているかどうかで放熱特性に大きな差が生じる。素子の発熱が非常に大きくなっている現在、熱伝導性充填材の粗粒の量をコントロールすることは特に重要である。 A manufacturer that manufactures a filler such as a heat conductive filler measures the particle size distribution and puts a value on an inspection table or the like, but coarse particles with a small absolute amount cannot generally be detected by a particle size distribution measuring device. Therefore, even if the same material and the same average particle diameter are used, there is a large difference in heat dissipation characteristics depending on whether or not coarse particles are removed. It is particularly important to control the amount of coarse particles of the heat conductive filler at the time when the heat generation of the device is very large.
これら、熱伝導性充填材から粗粒を取り除くためには、いくつか方法がある。一般的には気流分級やメッシュ分級などがあり、高度に粗粒を取り除きさえすれば、熱伝導性充填材の分級は何でもよいが、本発明に用いられる熱伝導性充填材は、メッシュ分級を掛けることが好ましい。気流分級もかなりの確率で粗粒を取り除くことができるが、やはり高度に取り除くことは難しいし、メッシュ分級の方が、例えば５００メッシュ（目開き２５μｍ）パス品を使えば実質的に、最大粒径２５μｍの熱伝導性充填材が得られる。 There are several ways to remove coarse particles from these thermally conductive fillers. Generally, there are airflow classification, mesh classification, etc. As long as coarse particles are removed to a high degree, the classification of the thermally conductive filler is not limited, but the thermally conductive filler used in the present invention is classified into mesh classification. It is preferable to multiply. Coarse particles can be removed with a considerable probability by airflow classification, but it is still difficult to remove coarsely, and mesh classification is practically the largest particle when using a 500 mesh (opening 25 μm) pass product, for example. A thermally conductive filler with a diameter of 25 μm is obtained.
上記熱伝導性充填材の充填量は、シリコーングリース組成物中、６０質量％より少ないと所望する放熱効果が得られないし、９８質量％より大きいとグリース状にならず、伸展性の乏しいものとなるため、６０〜９８質量％の範囲、好ましくは８０〜９５質量％の範囲である。 When the amount of the heat conductive filler is less than 60% by mass in the silicone grease composition, the desired heat dissipation effect cannot be obtained, and when it is greater than 98% by mass, it does not become a grease and has poor extensibility. Therefore, it is in the range of 60 to 98% by mass, preferably in the range of 80 to 95% by mass.
（Ｂ）成分のオルガノポリシロキサンは、下記平均組成式（１）で示されるものである。
Ｒ1 aＳｉＯ(4-a)/2 ・・・・・（１）
The (B) component organopolysiloxane is represented by the following average composition formula (1).
R 1 a SiO (4-a) / 2 (1)
上記式（１）において、Ｒ1は炭素数１〜１８の飽和又は不飽和の１価炭化水素基から選択される１種もしくは２種以上の基である。このような基としては、例えば、メチル基、エチル基、プロピル基、ヘキシル基、オクチル基、デシル基、ドデシル基、テトラデシル基、ヘキサデシル基、オクタデシル基等のアルキル基、シクロペンチル基、シクロヘキシル基等のシクロヘキシル基、ビニル基、アリル基等のアルケニル基、フェニル基、トリル基等のアリール基、２−フェニルエチル基、２−メチル−２−フェニルエチル基等のアラルキル基、３，３，３−トリフロロプロピル基、２−（パーフロロブチル）エチル基、２−（パーフロロオクチル）エチル基、ｐ−クロロフェニル基等のハロゲン化炭化水素基などが挙げられるが、特にメチル基、フェニル基、及び炭素数６〜１４のアルキル基が好ましい。ａはシリコーングリース組成物として要求される粘度の観点から、１．８〜２．２の範囲の正数がよく、特に１．９〜２．２の範囲の正数が好ましい。 In the above formula (1), R 1 is one or more groups selected from monovalent saturated or unsaturated hydrocarbon group having 1 to 18 carbon atoms. Such groups include, for example, methyl groups, ethyl groups, propyl groups, hexyl groups, octyl groups, decyl groups, alkyl groups such as dodecyl groups, tetradecyl groups, hexadecyl groups, octadecyl groups, cyclopentyl groups, cyclohexyl groups, etc. An alkenyl group such as a cyclohexyl group, a vinyl group and an allyl group; an aryl group such as a phenyl group and a tolyl group; an aralkyl group such as a 2-phenylethyl group and a 2-methyl-2-phenylethyl group; Examples include halogenated hydrocarbon groups such as a fluoropropyl group, 2- (perfluorobutyl) ethyl group, 2- (perfluorooctyl) ethyl group, and p-chlorophenyl group. Particularly, methyl group, phenyl group, and carbon The alkyl group of several 6-14 is preferable. From the viewpoint of the viscosity required for the silicone grease composition, a is preferably a positive number in the range of 1.8 to 2.2, and particularly preferably a positive number in the range of 1.9 to 2.2.
また、本発明で使用するオルガノポリシロキサンの２５℃における動粘度は、５０ｍｍ2／ｓより低いとシリコーングリース組成物にした時にオイルブリードが出やすくなるし、５００，０００ｍｍ2／ｓより大きくなるとシリコーングリース組成物にしたときの伸展性が乏しくなることから、２５℃における動粘度が５０〜５００，０００ｍｍ2／ｓであることが必要であり、特に１００〜１０，０００ｍｍ2／ｓであることが好ましい。なお、動粘度はオストワルド粘度計により測定することができる。 Moreover, kinematic viscosity at 25 ° C. of the organopolysiloxane used in the present invention, oil bleeding to easily appear when lower than 50 mm 2 / s to the silicone grease composition, greater than 500,000 2 / s when silicone since the extensibility when the grease composition becomes poor, that kinematic viscosity at 25 ° C. is required to be 50~500,000mm 2 / s, in particular 100~10,000mm 2 / s preferable. The kinematic viscosity can be measured with an Ostwald viscometer.
また、本発明のシリコーングリース組成物中、このオルガノポリシロキサンの配合量が２質量％より少ないとグリース状にならず、伸展性に乏しいものとなり、４０質量％より多いと放熱効果が乏しいものとなるため、２〜４０質量％の範囲、好ましくは３〜１５質量％の範囲である。 Further, in the silicone grease composition of the present invention, when the blending amount of the organopolysiloxane is less than 2% by mass, it does not become a grease and has poor extensibility, and when it exceeds 40% by mass, the heat dissipation effect is poor. Therefore, it is in the range of 2 to 40% by mass, preferably in the range of 3 to 15% by mass.
本発明の放熱用シリコーングリース組成物を製造するには、（Ａ）及び（Ｂ）成分をプラネタリーミキサーなど高粘度材料を混練りできる装置を用い、室温下あるいは加熱下で攪拌混合することにより得ることができる。ここで、攪拌混合条件としては、室温〜１５０℃、特に５０〜１００℃で３０分〜３時間、特に１時間〜２時間とすることが好ましい。
なお、本発明の放熱用シリコーングリース組成物には、上記成分以外の各種添加剤を、本発明の目的を損なわない範囲で適宜配合してもよい。
In order to produce the silicone grease composition for heat dissipation of the present invention, the components (A) and (B) are stirred and mixed at room temperature or under heating using a device capable of kneading a high viscosity material such as a planetary mixer. Can be obtained. Here, as stirring and mixing conditions, room temperature to 150 ° C., particularly 50 to 100 ° C., 30 minutes to 3 hours, particularly 1 hour to 2 hours are preferable.
In addition, you may mix | blend suitably various additives other than the said component in the silicone grease composition for thermal radiation of this invention in the range which does not impair the objective of this invention.
本発明の放熱用シリコーングリース組成物は、上述したように、５００メッシュ（２５μｍ目開き）オンの粗粒質量が、該組成物中５０ｐｐｍ以下であることが必要である。また、同時に３２５メッシュ（４５μｍ目開き）オンの粗粒が、実質的にゼロであることが必要である。 As described above, the heat-dissipating silicone grease composition of the present invention needs to have a coarse particle mass of 500 mesh (25 μm aperture) ON of 50 ppm or less in the composition. At the same time, 325 mesh (45 μm openings) coarse particles must be substantially zero.
本発明において、放熱用シリコーングリース組成物中の粗粒質量を測定するには、その放熱用シリコーングリース組成物のシリコーン分を溶解させることができる溶剤ならば何でもいいが、例えばトルエンなどに溶解させ、その溶解液を３２５メッシュ（目開き４５μｍ）及び５００メッシュ（目開き２５μｍ）に通過させ、よく洗浄後、３２５メッシュ（目開き４５μｍ）オンは目視で観察し、５００メッシュ（目開き２５μｍ）オンは、オンした粗粒を乾燥させ、薬包紙などに集めてその質量を測定すればよい。 In the present invention, the mass of coarse particles in the heat-dissipating silicone grease composition may be measured by any solvent that can dissolve the silicone content of the heat-dissipating silicone grease composition. For example, it can be dissolved in toluene or the like. The solution was passed through 325 mesh (aperture 45 μm) and 500 mesh (aperture 25 μm), washed well, and 325 mesh (aperture 45 μm) on was visually observed and 500 mesh (aperture 25 μm) on The dried coarse particles may be dried and collected on a medicine wrapping paper and the mass thereof may be measured.
本発明の放熱用シリコーングリース組成物は、これを７５μｍの厚さで金属板等の硬質基材間に塗工し、０．１５ＭＰａの圧力で１５分かけて押しつぶした場合、容易に厚さ２５μｍ以下、特に２０μｍ以下となるものである。通常、発熱する素子とヒートシンク等の間に放熱用シリコーングリース組成物を塗布し、クリップなどでヒートシンクを素子に押しつけるような構造をとるが、現在の機器の小型化、軽量化傾向においては、ヒートシンクを素子に十分に加圧するような構造は取れなくなってきている。従って、低い圧力においても放熱用シリコーングリース組成物が十分薄くならないと、所望な放熱特性が得られない。 The heat-dissipating silicone grease composition of the present invention is easily applied to a hard substrate such as a metal plate at a thickness of 75 μm and crushed for 15 minutes at a pressure of 0.15 MPa. In particular, it is 20 μm or less. Normally, a heat-dissipating silicone grease composition is applied between the heat-generating element and the heat sink, and the heat sink is pressed against the element with a clip or the like. It has become impossible to take a structure that sufficiently pressurizes the element. Therefore, if the silicone grease composition for heat dissipation is not sufficiently thin even at a low pressure, desired heat dissipation characteristics cannot be obtained.
このような放熱用シリコーングリース組成物の回転粘度計により測定した２５℃における粘度は、１０〜１，０００Ｐａ・ｓ、特に１００〜５００Ｐａ・ｓであることが好ましい。 The viscosity at 25 ° C. of the silicone grease composition for heat dissipation measured with a rotational viscometer is preferably 10 to 1,000 Pa · s, particularly preferably 100 to 500 Pa · s.
以下、実施例及び比較例を示し、本発明を更に詳述するが、本発明は下記の実施例に制限されるものではない。なお、下記例において、平均粒径はＭｉｃｒｏｔｒａｃ社製のＭＴ３０００（型式）により測定した値であり、動粘度はオストワルド粘度計により測定した２５℃における値である。 EXAMPLES Hereinafter, although an Example and a comparative example are shown and this invention is further explained in full detail, this invention is not restrict | limited to the following Example. In the following examples, the average particle diameter is a value measured with MT3000 (model) manufactured by Microtrac, and the kinematic viscosity is a value at 25 ° C. measured with an Ostwald viscometer.
［実施例１〜５、比較例１〜５］
表１及び表２に示す成分及び配合量を５リットルプラネタリーミキサー（井上製作所（株）製混合機の登録商標）に投入し、室温にて１時間攪拌し、放熱用シリコーングリース組成物を製造した。得られた放熱用シリコーングリース組成物の特性を下記に示す方法により測定し、これらの結果を表１及び表２に併記した。
[Examples 1-5, Comparative Examples 1-5]
The components and blending amounts shown in Table 1 and Table 2 are put into a 5-liter planetary mixer (registered trademark of a mixer manufactured by Inoue Seisakusho Co., Ltd.) and stirred at room temperature for 1 hour to produce a heat-dissipating silicone grease composition. did. The properties of the obtained heat-dissipating silicone grease composition were measured by the methods shown below, and the results are also shown in Tables 1 and 2.
〔テストピース作製〕
直径１２．６ｍｍ円形、厚み１ｍｍのＡｌ板２枚で厚さ７５μｍの放熱用シリコーングリース組成物を挟み込み、０．１５ＭＰａの圧力を１５分間掛けてテストピースを作製した。
[Test piece production]
A heat dissipation silicone grease composition having a thickness of 75 μm was sandwiched between two Al plates having a diameter of 12.6 mm and a thickness of 1 mm, and a test piece was produced by applying a pressure of 0.15 MPa for 15 minutes.
〔放熱用シリコーングリース組成物の厚み測定〕
テストピースの厚さをマイクロメータ（株式会社ミツトヨ製）で測定し、予め測定してあったＡｌ板２枚分の厚さを差し引いて放熱用シリコーングリース組成物の厚みを算出した。
[Measurement of thickness of silicone grease composition for heat dissipation]
The thickness of the test piece was measured with a micrometer (manufactured by Mitutoyo Corporation), and the thickness of the heat-dissipating silicone grease composition was calculated by subtracting the thickness measured in advance for two Al plates.
〔熱抵抗測定〕
放熱用シリコーングリース組成物の厚みを測定した後、そのテストピースを用いて放熱用シリコーングリース組成物の熱抵抗の測定を行った。使用機器は、Ｈｏｌｏｍｅｔｒｉｘ ｍｉｃｒｏｍｅｔ社の型式Ｍｉｃｒｏ ｆｌａｓｈ ３００を使用した。
(Thermal resistance measurement)
After measuring the thickness of the silicone grease composition for heat dissipation, the thermal resistance of the silicone grease composition for heat dissipation was measured using the test piece. The equipment used was a model Micro flash 300 manufactured by Holometrix micromet.
〔５００メッシュ（目開き２５μｍ）オン質量測定〕
放熱用シリコーングリース組成物５０ｇをトルエン１００ｇと共に２００ｍｌのプラスチック瓶に入れ、栓をして放熱用シリコーングリース組成物が分散しきるまで振とうした。分散した後、５００メッシュ（目開き２５μｍ）にその分散液を流し込み、洗浄用トルエンなどでよく洗い流し、乾燥機にそのメッシュを入れて乾燥させた。乾燥後、薬包紙に５００メッシュオンの粗粒を移してその質量を計り、放熱用シリコーングリース組成物に対し、５００メッシュオンの粗粒が何ｐｐｍかを計算した。
[Measurement of 500 mesh (aperture 25 μm) on mass]
50 g of the heat-dissipating silicone grease composition was placed in a 200 ml plastic bottle together with 100 g of toluene, capped and shaken until the heat-dissipating silicone grease composition was completely dispersed. After the dispersion, the dispersion was poured into a 500 mesh (aperture 25 μm), washed thoroughly with washing toluene, etc., and the mesh was put into a dryer and dried. After drying, 500 mesh-on coarse particles were transferred to a medicine wrapping paper, and the mass thereof was measured to calculate how many ppm of 500 mesh-on coarse particles were calculated for the silicone grease composition for heat dissipation.
〔３２５メッシュ（目開き４５μｍ）オン目視観察〕
放熱用シリコーングリース組成物５０ｇをトルエン１００ｇと共に２００ｍｌのプラスチック瓶に入れ、栓をして放熱用シリコーングリース組成物が分散しきるまで振とうした。分散した後、３２５メッシュ（目開き４５μｍ）にその分散液を流し込み、洗浄用トルエンなどでよく洗い流し、乾燥機にそのメッシュを入れて乾燥させた。乾燥後、薬包紙に３２５メッシュオンの粗粒を移して目視観察し、下記判定基準により評価した。
＜判定基準＞
○：３２５メッシュ（目開き４５μｍ）オンの粗粒が目視にて見つけられない。
×：３２５メッシュ（目開き４５μｍ）オンの粗粒が目視にて一粒でも確認できる。
[Visual observation on 325 mesh (aperture 45 μm)]
50 g of the heat-dissipating silicone grease composition was placed in a 200 ml plastic bottle together with 100 g of toluene, capped and shaken until the heat-dissipating silicone grease composition was completely dispersed. After the dispersion, the dispersion was poured into a 325 mesh (aperture 45 μm), washed thoroughly with toluene for washing, and the mesh was put into a dryer and dried. After drying, 325 mesh-on coarse particles were transferred to the medicine wrapping paper, visually observed, and evaluated according to the following criteria.
<Criteria>
◯: Coarse particles with 325 mesh (aperture 45 μm) are not found visually.
X: 325 mesh (aperture 45 μm) ON coarse particles can be confirmed by visual observation.
〔粘度評価〕
放熱用シリコーングリース組成物の粘度は、２５℃における値を示し、その測定はマルコム粘度計（タイプＰＣ−１Ｔ）を用いた。
[Viscosity evaluation]
The viscosity of the silicone grease composition for heat dissipation showed the value in 25 degreeC, and the measurement used the Malcolm viscometer (type PC-1T).
（Ａ）
Ａ−１ アルミニウム粉末（熱伝導率２３７Ｗ／ｍ℃、平均粒径１．９μｍ、５００
メッシュパス品）
Ａ−２ 酸化亜鉛粉末（熱伝導率５４Ｗ／ｍ℃、平均粒径：０．３μｍ、気流分級
品）
Ａ−３ 銅粉末（熱伝導率３９８Ｗ／ｍ℃、平均粒径６．９μｍ、気流分級品）
Ａ−４ アルミニウム粉末（熱伝導率２３７Ｗ／ｍ℃、平均粒径６．５μｍ、分級無
し）
Ａ−５ 銅粉末（熱伝導率３９８Ｗ／ｍ℃、平均粒径７．２μｍ、分級無し）
(A)
A-1 Aluminum powder (thermal conductivity 237 W / m ° C., average particle size 1.9 μm, 500
Mesh pass product)
A-2 Zinc oxide powder (thermal conductivity 54 W / m ° C, average particle size: 0.3 μm, airflow classification product)
A-3 Copper powder (thermal conductivity 398 W / m ° C., average particle size 6.9 μm, airflow classification product)
A-4 Aluminum powder (thermal conductivity 237 W / m ° C., average particle size 6.5 μm, no classification)
A-5 Copper powder (thermal conductivity 398 W / m ° C., average particle size 7.2 μm, no classification)
（Ｂ）
Ｂ−１ 下記式で示される動粘度：３９０ｍｍ2／ｓのオルガノポリシロキサン
B-1 Kinematic viscosity represented by the following formula: 390 mm 2 / s organopolysiloxane
Ｂ−２ 下記式で示される動粘度：５００ｍｍ2／ｓのオルガノポリシロキサン
Claims (2)
（Ｂ）下記平均組成式（１）
Ｒ1 aＳｉＯ(4-a)/2 ・・・・・（１）
〔式中、Ｒ1は独立に炭素数１〜１８の飽和又は不飽和の１価炭化水素基であり、ａは１．８≦ａ≦２．２の正数である。〕
で表される２５℃における動粘度が５０〜５００，０００ｍｍ2／ｓのオルガノポリシロキサン ２〜４０質量％
を含有してなる放熱用シリコーングリース組成物において、５００メッシュ（２５μｍ目開き）オンの粗粒質量が、放熱用シリコーングリース組成物中５０ｐｐｍ以下であり、且つ３２５メッシュ（４５μｍ目開き）オンの粗粒が実質的にゼロであることを特徴とする放熱用シリコーングリース組成物。 (A) One or more thermal conductivity selected from metal powder, metal oxide powder and ceramic powder having a thermal conductivity of 10 W / m ° C. or higher and an average particle size of 0.1 to 15.0 μm. Filler 60-98% by mass
(B) The following average composition formula (1)
R 1 a SiO (4-a) / 2 (1)
[Wherein, R 1 is independently a saturated or unsaturated monovalent hydrocarbon group having 1 to 18 carbon atoms, and a is a positive number of 1.8 ≦ a ≦ 2.2. ]
2 to 40% by mass of an organopolysiloxane having a kinematic viscosity of 50 to 500,000 mm 2 / s at 25 ° C.
In the heat-dissipating silicone grease composition, the coarse particle mass of 500 mesh (25 μm openings) -on is 50 ppm or less in the heat-dissipating silicone grease composition and 325 mesh (45 μm openings) -on coarse A silicone grease composition for heat dissipation, characterized in that the number of grains is substantially zero.
The heat-dissipating silicone grease composition according to claim 1, wherein the heat-dissipating silicone grease composition has a thickness of 25 μm or less when crushed by a pressure of 0.15 MPa.
Priority Applications (6)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2004151706A JP2005330426A (en) | 2004-05-21 | 2004-05-21 | Heat-dissipating silicone grease composition |
| TW094116167A TWI385246B (en) | 2004-05-21 | 2005-05-18 | Silicone grease compositions |
| CNB2005100980744A CN100569858C (en) | 2004-05-21 | 2005-05-20 | Silicone grease composition |
| US11/133,339 US7510998B2 (en) | 2004-05-21 | 2005-05-20 | Silicon grease compositions |
| EP05253144.9A EP1600494B1 (en) | 2004-05-21 | 2005-05-20 | Silicone grease compositions |
| KR1020050042314A KR101125811B1 (en) | 2004-05-21 | 2005-05-20 | Silicone grease compositions |
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| JP2004151706A JP2005330426A (en) | 2004-05-21 | 2004-05-21 | Heat-dissipating silicone grease composition |
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| JP2005330426A true JP2005330426A (en) | 2005-12-02 |
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| JP2004151706A Pending JP2005330426A (en) | 2004-05-21 | 2004-05-21 | Heat-dissipating silicone grease composition |
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| CN (1) | CN100569858C (en) |
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