JP7379939B2 - thermally conductive composition - Google Patents
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- 239000000203 mixture Substances 0.000 title claims description 49
- 239000002199 base oil Substances 0.000 claims description 36
- 239000011231 conductive filler Substances 0.000 claims description 23
- 239000002270 dispersing agent Substances 0.000 claims description 16
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 11
- 229910052731 fluorine Inorganic materials 0.000 claims description 11
- 239000011737 fluorine Substances 0.000 claims description 11
- 239000004519 grease Substances 0.000 description 30
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 12
- 239000002562 thickening agent Substances 0.000 description 12
- 238000006116 polymerization reaction Methods 0.000 description 11
- 239000000843 powder Substances 0.000 description 8
- -1 alloys) Chemical class 0.000 description 7
- 239000003112 inhibitor Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 239000011787 zinc oxide Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 5
- 229910052582 BN Inorganic materials 0.000 description 4
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 229920002545 silicone oil Polymers 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000395 magnesium oxide Substances 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 125000005010 perfluoroalkyl group Chemical group 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 150000007942 carboxylates Chemical class 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical group 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000010292 electrical insulation Methods 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 230000020169 heat generation Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000003607 modifier Substances 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920013639 polyalphaolefin Polymers 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229920000089 Cyclic olefin copolymer Polymers 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 235000010724 Wisteria floribunda Nutrition 0.000 description 1
- TVIPECTUCRNDNZ-UHFFFAOYSA-M [Na+].NC(=O)C1=CC=C(C([O-])=O)C=C1 Chemical compound [Na+].NC(=O)C1=CC=C(C([O-])=O)C=C1 TVIPECTUCRNDNZ-UHFFFAOYSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 1
- 239000012964 benzotriazole Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012811 non-conductive material Substances 0.000 description 1
- JGTNAGYHADQMCM-UHFFFAOYSA-N perfluorobutanesulfonic acid Chemical class OS(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F JGTNAGYHADQMCM-UHFFFAOYSA-N 0.000 description 1
- 239000010702 perfluoropolyether Substances 0.000 description 1
- 239000012169 petroleum derived wax Substances 0.000 description 1
- 235000019381 petroleum wax Nutrition 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- 229920001083 polybutene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000193 polymethacrylate Polymers 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-L succinate(2-) Chemical compound [O-]C(=O)CCC([O-])=O KDYFGRWQOYBRFD-UHFFFAOYSA-L 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 150000004867 thiadiazoles Chemical class 0.000 description 1
- 150000003672 ureas Chemical class 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Description
本発明は、熱伝導性組成物、特に高い熱伝導率を有する熱伝導性組成物に関する。 The present invention relates to thermally conductive compositions, particularly thermally conductive compositions having high thermal conductivity.
例えば、電子機器に使用されている半導体部品の中には、コンピューターのＣＰＵ、ペルチェ素子、ＬＥＤ、インバーター等の電源制御用パワー半導体等使用中に発熱をともなう発熱部品がある。これらの発熱部品を熱から保護し、正常に機能させるために、熱伝導性グリースや熱伝導性シートを介して、発熱部品から発生した熱をヒートスプレッダーやヒートシンク等の放熱部品（冷却装置）へ伝導させ放熱させる方法がある。 For example, among semiconductor components used in electronic devices, there are heat-generating components that generate heat during use, such as computer CPUs, Peltier elements, LEDs, and power semiconductors for controlling power supplies such as inverters. In order to protect these heat-generating components from heat and allow them to function properly, the heat generated from the heat-generating components is transferred to heat dissipation components (cooling devices) such as heat spreaders and heat sinks through thermally conductive grease or thermally conductive sheets. There is a method to dissipate heat by conduction.
ここで、熱伝導性グリースとは、流動性又は半流動性を有する潤滑剤であって、発熱部品と放熱部品の間隔を狭くした状態で効果的に放熱部品（冷却装置）へ熱を伝導することが可能なグリースである。また、熱伝導性シートとは、基材に熱伝導性塗料を塗布した熱伝導性を有するシートであり、取り扱い性が非常に簡便で、繰り返し使用が可能なシートである。 Here, thermally conductive grease is a fluid or semi-fluid lubricant that effectively conducts heat to heat-radiating parts (cooling device) while keeping the distance between the heat-generating parts and the heat-radiating parts narrow. It is possible to use grease. Further, a thermally conductive sheet is a sheet that has thermal conductivity and has a base material coated with a thermally conductive paint, and is a sheet that is very easy to handle and can be used repeatedly.
ここで、本明細書では、熱伝導性組成物とは熱伝導性グリースや熱伝導性塗料等の熱伝導性を有する流動体または半流動体の総称を意味する。 Here, in this specification, the thermally conductive composition is a general term for fluids or semi-fluids having thermal conductivity, such as thermally conductive grease and thermally conductive paint.
このような熱伝導組成物に関し、例えば熱伝導性グリースとしては、ポリαオレフィン油やシリコーン油等の基油に、銀、アルミニウム等の金属、或いは、酸化亜鉛又は酸化アルミニウム等の金属酸化物や、窒化ホウ素、窒化アルミニウム等の無機窒化物等の熱伝導性充填剤を分散させたもの等が知られている。 Regarding such a thermally conductive composition, for example, a thermally conductive grease may include a base oil such as poly-α-olefin oil or silicone oil, a metal such as silver or aluminum, or a metal oxide such as zinc oxide or aluminum oxide. , those in which thermally conductive fillers such as inorganic nitrides such as boron nitride and aluminum nitride are dispersed are known.
近年、電力制御機器の大電力動作や電子機器の高速動作の結果、発熱部品の発熱量は増大する傾向にある。それに対し、例えば、高い熱伝導性を有する熱伝導性グリースを提供することを目的として特定の表面改質剤を配合した技術（特許文献１参照）等が開示されている。 In recent years, as a result of high-power operation of power control devices and high-speed operation of electronic devices, the amount of heat generated by heat-generating components tends to increase. In contrast, for example, a technique has been disclosed in which a specific surface modifier is blended for the purpose of providing a thermally conductive grease having high thermal conductivity (see Patent Document 1).
一方で、部品の小型化と発熱部品の高密度実装化に伴い、発熱の密度もまた上昇する傾向にある。このような発熱の量的増大と高密度化に対応して機器の性能を長期に亘って安定に維持するため、発熱部品内での発熱を効率的に除去する必要性から、熱伝導性組成物は、高い耐熱性を有すると同時に、発熱部品と放熱部品の間に従来よりも優れた熱伝導性を有する層を形成することが求められている。 On the other hand, as components become smaller and heat-generating components are mounted in higher density, the density of heat generation also tends to increase. In order to maintain stable performance of equipment over a long period of time in response to such an increase in the quantity and density of heat generation, it is necessary to efficiently remove heat generated within heat-generating components, so thermally conductive compositions are being developed. Products are required to have high heat resistance and at the same time form a layer between a heat generating component and a heat dissipating component that has better thermal conductivity than before.
一般に熱伝導組成物の熱伝導性は、熱伝導性充填剤の含有量が支配的であるが、その特性を十分発揮するためには、熱伝導性充填剤間を橋渡しする基油が、放熱させる熱に耐えうる耐熱性が必要となる。そのため、例えば、高い耐熱性を有し、熱伝導性に優れた熱伝導組成物（熱伝導性グリース）を提供することを目的として、基油としてポリオルガノシロキサン等のシリコーン油を使用した技術（特許文献２参照）が開示されている。 Generally, the thermal conductivity of a thermally conductive composition is dominated by the content of the thermally conductive filler, but in order to fully demonstrate its properties, the base oil that bridges the thermally conductive fillers must be used for heat dissipation. Heat resistance is required to withstand the heat generated. Therefore, for example, with the aim of providing a thermally conductive composition (thermal conductive grease) that has high heat resistance and excellent thermal conductivity, we have developed a technology that uses silicone oil such as polyorganosiloxane as a base oil ( (see Patent Document 2) is disclosed.
しかしながら、基油としてシリコーン油を使用した熱伝導性グリースでは、加熱により発生するシロキサンガスによる接点障害発生の懸念から、シリコーン油を使用しない熱伝導性グリース等の熱伝導性組成物が求められている。 However, there is a need for thermally conductive compositions such as thermally conductive greases that do not use silicone oil due to concerns that thermally conductive greases that use silicone oil as a base oil may cause contact failure due to siloxane gas generated by heating. There is.
本発明は、高い耐熱性を有しつつ、優れた熱伝導性を有する熱伝導性組成物を提供することを目的とする。 An object of the present invention is to provide a thermally conductive composition that has high heat resistance and excellent thermal conductivity.
本発明者らは、上記課題を達成するために鋭意検討した結果、所定の重合平均分子量のパーフルオロポリオキセタンを基油として含有した熱伝導性組成物であれば上記課題を解決できることを見出し、本発明を完成するに至った。すなわち、本発明は以下のものを提供する。 As a result of intensive studies to achieve the above-mentioned problems, the present inventors found that the above-mentioned problems could be solved by a thermally conductive composition containing perfluoropolyoxetane with a predetermined polymerization average molecular weight as a base oil. The present invention has now been completed. That is, the present invention provides the following.
（１）本発明の第１は、少なくとも、熱伝導性充填剤と、基油と、を含有し、前記基油は重合平均分子量が３５００以上５０００未満のパーフルオロポリオキセタンである熱伝導性組成物である。 (1) The first aspect of the present invention is a thermally conductive composition containing at least a thermally conductive filler and a base oil, the base oil being a perfluoropolyoxetane having a polymerization average molecular weight of 3,500 or more and less than 5,000. It is a thing.
（２）本発明の第２は、第１の発明において、前記熱伝導性充填剤の含有量は、当該熱伝導性組成物１００質量％に対し８０質量％以上９７質量％以下の割合である熱伝導性グリースである。 (2) In the second aspect of the present invention, in the first aspect, the content of the thermally conductive filler is in a proportion of 80% by mass or more and 97% by mass or less based on 100% by mass of the thermally conductive composition. It is a thermally conductive grease.
（３）本発明の第３は、第１又は第２の発明において、前記基油の含有量は、当該熱伝導性組成物１００質量％に対し２質量％以上２０質量％以下の割合である熱伝導性組成物である。 (3) In the third aspect of the present invention, in the first or second aspect, the content of the base oil is in a proportion of 2% by mass or more and 20% by mass or less based on 100% by mass of the thermally conductive composition. It is a thermally conductive composition.
本発明に係る熱伝導性組成物によれば、高い耐熱性を有するとともに優れた熱伝導性を有する。 The thermally conductive composition according to the present invention has high heat resistance and excellent thermal conductivity.
以下、本発明の具体的な実施形態（以下、「本実施の形態」という）について詳細に説明する。なお、本発明は、以下の実施形態に何ら限定されるものではなく、本発明の目的の範囲内において、適宜変更を加えて実施することができる。 Hereinafter, a specific embodiment of the present invention (hereinafter referred to as "this embodiment") will be described in detail. Note that the present invention is not limited to the following embodiments, and can be implemented with appropriate modifications within the scope of the purpose of the present invention.
≪１．熱伝導性組成物≫
本実施の形態に係る熱伝導性組成物は、少なくとも、熱伝導性充填剤と、基油と、を含有する。以下、熱伝導性組成物に含まれる各成分について説明する。
≪1. Thermal conductive composition≫
The thermally conductive composition according to this embodiment contains at least a thermally conductive filler and a base oil. Each component contained in the thermally conductive composition will be explained below.
（１）基油
本実施の形態に係る熱伝導性組成物は、基油として、重合平均分子量が３５００以上５０００未満のパーフルオロポリオキセタンであることを特徴としている。本発明者らは、各種基油との組み合わせを鋭意研究した結果、フッ素系の基油のなかでも、パーフルオロポリオキセタンを用いることにより、高い耐熱性を維持できることを見出した。
(1) Base Oil The thermally conductive composition according to the present embodiment is characterized in that the base oil is perfluoropolyoxetane having a polymerization average molecular weight of 3,500 or more and less than 5,000. As a result of intensive research on combinations with various base oils, the present inventors found that among fluorine-based base oils, by using perfluoropolyoxetane, high heat resistance can be maintained.
そして、本発明者らは、フッ素系の基油のなかでも重合平均分子量が３５００以上５０００未満のパーフルオロポリオキセタンを選択することにより、熱伝導性充填剤を高密度に含有させることを可能となり、高い耐熱性に加えて、優れた熱伝導性を奏することを見出した。 The present inventors selected perfluoropolyoxetane with a polymerization average molecular weight of 3,500 or more and less than 5,000 among fluorine-based base oils, thereby making it possible to contain a thermally conductive filler in a high density. discovered that it exhibits excellent thermal conductivity in addition to high heat resistance.
また、パーフルオロポリオキセタンは、重合平均分子量は３８００以上４８００以下であることが好ましく、４２００以上４６００以下であることがより好ましい。 Further, the polymerization average molecular weight of the perfluoropolyoxetane is preferably 3,800 or more and 4,800 or less, more preferably 4,200 or more and 4,600 or less.
重合平均分子量が３５００以上５０００未満のパーフルオロポリオキセタンとしては、例えば、ダイキン社製のデルナムＳ６５等が市販されており、好適に用いることができる。 As perfluoropolyoxetane having a polymerization average molecular weight of 3,500 or more and less than 5,000, for example, Delnum S65 manufactured by Daikin Co., Ltd. is commercially available and can be suitably used.
（２）熱伝導性充填剤
熱伝導性充填剤は、熱伝導性組成物に高い熱伝導性を付与する成分である。熱伝導性充填剤としては、基油より高い熱伝導性を有するものであれば特に限定されないが、金属酸化物、無機窒化物、金属（合金も含む。）、ケイ素化合物、カーボン材料等の粉末を用いることが好ましい。熱伝導性充填剤の種類は１種類であってもよいし、また２種以上を組み合わせて用いることもできる。
(2) Thermal conductive filler The thermally conductive filler is a component that imparts high thermal conductivity to the thermally conductive composition. Thermal conductive fillers are not particularly limited as long as they have higher thermal conductivity than the base oil, but powders such as metal oxides, inorganic nitrides, metals (including alloys), silicon compounds, carbon materials, etc. It is preferable to use The number of types of thermally conductive fillers may be one, or two or more types may be used in combination.
熱伝導性充填剤としては、電気絶縁性を求める場合には、酸化亜鉛、酸化マグネシウム、酸化アルミニウム、窒化アルミニウム、窒化ホウ素、炭化ケイ素、シリカ、ダイヤモンド等の、半導体やセラミック等の非導電性物質の粉末が好ましく、酸化亜鉛、酸化マグネシウム、酸化アルミニウム、窒化アルミニウム、窒化ホウ素、炭化ケイ素、シリカの粉末がより好ましく、酸化亜鉛、酸化アルミニウム、窒化アルミニウムの粉末が特に好ましい。 As a thermally conductive filler, when electrical insulation is required, non-conductive materials such as semiconductors and ceramics such as zinc oxide, magnesium oxide, aluminum oxide, aluminum nitride, boron nitride, silicon carbide, silica, and diamond are used. Powders of zinc oxide, magnesium oxide, aluminum oxide, aluminum nitride, boron nitride, silicon carbide, and silica are more preferable, and powders of zinc oxide, aluminum oxide, and aluminum nitride are particularly preferable.
また、上記の熱伝導性充填剤のなかでも高い熱伝導性を有するという観点からは、酸化亜鉛、酸化マグネシウム、酸化アルミニウム、窒化アルミニウム窒化ホウ素及び炭化ケイ素からなる群から選ばれる少なくとも１種以上であることが好ましい。 In addition, from the viewpoint of having high thermal conductivity among the above-mentioned thermally conductive fillers, at least one selected from the group consisting of zinc oxide, magnesium oxide, aluminum oxide, aluminum nitride, boron nitride, and silicon carbide is preferred. It is preferable that there be.
電気的な特性に対する要求が無く、電気絶縁性が求められない場合は、金属粉末や炭素材料粉末と非導電性物質の粉末とを組み合わせて用いることもできる。金属粉末を用いる場合は、高い熱伝導性を有するという観点から、銅、アルミニウム、及び銀の粉末からなる群から選ばれる少なくとも１種以上であることが好ましい。 If there is no requirement for electrical properties and electrical insulation is not required, a combination of metal powder or carbon material powder and non-conductive substance powder may be used. When using metal powder, from the viewpoint of having high thermal conductivity, it is preferably at least one selected from the group consisting of copper, aluminum, and silver powder.
熱伝導性充填剤の含有量は、熱伝導性組成物１００質量％に対し８０質量％以上９７質量％以下の割合であることが好ましく、９０質量％以上９６質量％以下の割合であることがより好ましい。熱伝導性充填剤の含有量が８０質量％以上の割合であることにより、熱伝導性組成物に高い熱伝導率を付与することができる。熱伝導性充填剤の含有量が９７質量％以下の割合であることにより、例えば、本実施の形態に係る熱伝導性組成物を熱伝導性グリースとする場合、ちょう度の低下を抑制して適切な粘度とし、十分な展性を付与することができる。 The content of the thermally conductive filler is preferably 80% by mass or more and 97% by mass or less, and preferably 90% by mass or more and 96% by mass or less, based on 100% by mass of the thermally conductive composition. More preferred. When the content of the thermally conductive filler is 80% by mass or more, high thermal conductivity can be imparted to the thermally conductive composition. By setting the content of the thermally conductive filler at a ratio of 97% by mass or less, for example, when the thermally conductive composition according to the present embodiment is used as a thermally conductive grease, a decrease in consistency can be suppressed. Appropriate viscosity and sufficient malleability can be imparted.
（３）分散剤
分散剤は、必要に応じて、本実施の形態に係る熱伝導性組成物に含有させてもよい。分散剤は、本実施の形態に係る熱伝導性組成物において必須の成分ではないが、熱伝導性組成物に含有される熱伝導性充填剤の表面に吸着し、熱伝導性充填剤と基油との親和性を向上させることができる。すなわち、分散剤は、熱伝導性充填剤の表面改質剤として機能し、熱伝導性充填剤と基油との親和性を向上させることによって、熱伝導性を向上させることができる。また、例えば本実施の形態に係る熱伝導性組成物を熱伝導性グリースとする場合、ちょう度を向上させ、適切な粘度とすることができる。
(3) Dispersant A dispersant may be included in the thermally conductive composition according to this embodiment, if necessary. Although the dispersant is not an essential component in the thermally conductive composition according to the present embodiment, it is adsorbed on the surface of the thermally conductive filler contained in the thermally conductive composition, and is combined with the thermally conductive filler and the base. Can improve affinity with oil. That is, the dispersant functions as a surface modifier for the thermally conductive filler, and can improve thermal conductivity by improving the affinity between the thermally conductive filler and the base oil. Further, for example, when the thermally conductive composition according to the present embodiment is used as a thermally conductive grease, the consistency can be improved and the viscosity can be made appropriate.
分散剤としては、例えば、含フッ素基・親水性含有オリゴマー、含フッ素基・親油性基含有オリゴマー、含フッ素基・親水性基・親油性基含有オリゴマー、含フッ素基・親水性基・親油性基・カルボキシル基含有オリゴマー、パーフルオロブタンスルホン酸塩、パーフルオロアルキル基含有カルボン酸塩、パーフルオロアルキル基・リン酸基含有リン酸エステル等のフッ素系分散剤や、ポリグリセリンモノアルキルエーテル化合物、カルボン酸構造を有する化合物、ポリカルボン酸系化合物等を挙げることができる。これらは単独で使用してもよいが、２種以上を組み合わせて使用してもよい。基油との親和性との観点からフッ素系分散剤を使用することが好ましく、含フッ素基・親水性含有オリゴマーを使用することが特に好ましい。 Examples of dispersants include oligomers containing fluorine-containing groups and hydrophilicity, oligomers containing fluorine-containing groups and lipophilic groups, oligomers containing fluorine-containing groups and hydrophilic groups and lipophilic groups, and oligomers containing fluorine-containing groups and hydrophilic groups and lipophilic groups. Fluorine-based dispersants such as group/carboxyl group-containing oligomers, perfluorobutane sulfonates, perfluoroalkyl group-containing carboxylates, phosphate esters containing perfluoroalkyl groups/phosphoric acid groups, polyglycerin monoalkyl ether compounds, Examples include compounds having a carboxylic acid structure and polycarboxylic acid compounds. These may be used alone or in combination of two or more. From the viewpoint of affinity with the base oil, it is preferable to use a fluorine-based dispersant, and it is particularly preferable to use a fluorine-containing group/hydrophilicity-containing oligomer.
分散剤の含有量は、熱伝導性組成物１００質量％に対して０．００１質量％以上３質量％以下であることが好ましい。より好ましくは０．０５質量％以上２質量％以下であり、さらに好ましくは０．１５質量％以上１質量％以下であり、最も好ましくは０．２質量％以上０．５質量％以下である。 The content of the dispersant is preferably 0.001% by mass or more and 3% by mass or less based on 100% by mass of the thermally conductive composition. The content is more preferably 0.05% by mass or more and 2% by mass or less, further preferably 0.15% by mass or more and 1% by mass or less, and most preferably 0.2% by mass or more and 0.5% by mass or less.
分散剤の含有量が０．００１質量％以上であることにより、熱伝導性組成物に含有される無機粉末充填剤と基油との親和性をより向上させる効果が得られ、熱伝導性組成物を熱伝導性グリースとする場合に、ちょう度を効果的に高めることができ、適切な粘度の熱伝導性組成物とすることができるため好ましい。 When the content of the dispersant is 0.001% by mass or more, the effect of further improving the affinity between the inorganic powder filler contained in the thermally conductive composition and the base oil can be obtained, and the thermally conductive composition When used as a thermally conductive grease, it is preferable because the consistency can be effectively increased and the thermally conductive composition can have an appropriate viscosity.
一方、分散剤の含有量が３質量％を超えても、分散剤含有による効果が飽和して熱伝導性組成物の特性は大きく変化しない。本実施の形態に係る熱伝導性組成物に好適に用いることのできる分散剤は、高い耐熱性等を有する必要があり、一般的に価格の高い物が多い。そのため、分散剤の含有量を３質量％以下にすることにより、余計なコストの発生を抑制することができるため好ましい。 On the other hand, even if the content of the dispersant exceeds 3% by mass, the effect of containing the dispersant is saturated and the properties of the thermally conductive composition do not change significantly. A dispersant that can be suitably used in the thermally conductive composition according to the present embodiment needs to have high heat resistance, etc., and is generally expensive. Therefore, it is preferable to set the content of the dispersant to 3% by mass or less because it is possible to suppress the generation of unnecessary costs.
（４）増ちょう剤
増ちょう剤も、必要に応じて、本実施の形態に係る熱伝導性組成物に含有させてもよい。増ちょう剤は、本実施の形態に係る熱伝導性組成物において必須の成分ではないが、例えば、熱伝導性組成物を熱伝導性グリースとする場合、増ちょう剤を含有させることにより、熱伝導性グリースのちょう度を制御して、熱伝導性グリースの塗布性を向上させることができる。
(4) Thickener A thickener may also be included in the thermally conductive composition according to the present embodiment, if necessary. Although the thickener is not an essential component in the thermally conductive composition according to the present embodiment, for example, when the thermally conductive composition is used as a thermally conductive grease, by including the thickener, it is possible to The consistency of the conductive grease can be controlled to improve the applicability of the thermally conductive grease.
増ちょう剤としては、例えば、ウレア化合物、ナトリウムテレフタラメート、ポリテトラフルオロエチレン、有機化ベントナイト、シリカゲル、石油ワックス、ポリエチレンワックス等を挙げることができる。特に、基油との親和性との観点からポリテトラフルオロエチレンを使用することが好ましい。 Examples of the thickener include urea compounds, sodium terephthalamate, polytetrafluoroethylene, organized bentonite, silica gel, petroleum wax, and polyethylene wax. In particular, it is preferable to use polytetrafluoroethylene from the viewpoint of affinity with the base oil.
増ちょう剤の含有量は、熱伝導性グリースの所望とするちょう度に基づいて適宜設定することができるが、熱伝導性グリース１００質量％に対して０．００５質量％以上１質量％以下の割合で含有させることが好ましい。増ちょう剤の含有量を０．００５質量％以上とすることにより、基油に対するちょう度の調整効果が発揮され始め、熱伝導性グリースを使用目的に適した粘度にグリース化させることができるため好ましい。増ちょう剤の含有量が１質量％を超えると、ちょう度が低くなり過ぎ、グリース状を維持できなくなったりするため好ましくない。 The content of the thickener can be appropriately set based on the desired consistency of the thermally conductive grease, but it should be 0.005% by mass or more and 1% by mass or less based on 100% by mass of the thermally conductive grease. It is preferable to contain it in a proportion. By setting the content of the thickener to 0.005% by mass or more, the effect of adjusting the consistency of the base oil begins to be exerted, and the thermally conductive grease can be made into a grease with a viscosity suitable for the purpose of use. preferable. If the content of the thickener exceeds 1% by mass, the consistency becomes too low and it becomes impossible to maintain a grease-like state, which is not preferable.
なお、グリースの特性を有する観点からすると、熱伝導性グリースの塗布性、拡がり性、付着性の観点から、熱伝導性グリースに適した粘度となるように、増ちょう剤の含有量を適宜選択することが好ましい。熱伝導性グリースの粘度は付着性の観点では高粘度とするのが好ましいものの、塗布のしやすさから１０００Ｐａ・ｓ以下とすることが好ましく、良好な濡れ拡がり性も維持するには６００Ｐａ.ｓ以下とすることがより好ましい。 In addition, from the viewpoint of the characteristics of the grease, the content of the thickener should be selected appropriately so that the viscosity is suitable for the thermal conductive grease from the viewpoint of the spreadability, spreadability, and adhesion of the thermal conductive grease. It is preferable to do so. Although the viscosity of the thermally conductive grease is preferably high from the viewpoint of adhesion, it is preferably 1000 Pa.s or less for ease of application, and 600 Pa.s to maintain good wetting and spreading properties. It is more preferable to set it as below.
（５）その他の成分
本実施の形態に係る熱伝導性組成物においては、必要に応じて、上記の各成分以外の他の成分（その他の成分）をさらに含有することができる。その他の成分としては、例えば、酸化防止剤、基油拡散防止剤、防錆剤、腐食防止剤、増粘剤等を挙げることができる。
(5) Other components The thermally conductive composition according to the present embodiment may further contain components other than the above-mentioned components (other components), if necessary. Examples of other components include antioxidants, base oil diffusion inhibitors, rust inhibitors, corrosion inhibitors, thickeners, and the like.
例えば、基油拡散防止剤は、熱伝導性組成物に含まれる基油が、塗布面に拡散するのを防止する効果のある成分である。基油拡散防止剤としては、パーフルオロアルキル基を含有する拡散防止剤を用いることができる。 For example, the base oil diffusion inhibitor is a component that is effective in preventing the base oil contained in the thermally conductive composition from diffusing onto the coated surface. As the base oil diffusion inhibitor, a diffusion inhibitor containing a perfluoroalkyl group can be used.
また、防錆剤としては、スルホン酸塩、カルボン酸、カルボン酸塩、コハク酸エステル等が挙げられる。腐食防止剤としては、ベンゾトリアゾール及びその誘導体等の化合物、チアジアゾール系化合物等を挙げることができる。増粘剤としては、ポリブテン、ポリメタクリレート、オレフィンコポリマー、高粘度のポリアルファオレフィン等を挙げることができる。 Further, examples of the rust preventive include sulfonate, carboxylic acid, carboxylate, succinate, and the like. Examples of the corrosion inhibitor include compounds such as benzotriazole and its derivatives, thiadiazole compounds, and the like. Examples of thickeners include polybutenes, polymethacrylates, olefin copolymers, high viscosity polyalphaolefins, and the like.
これらの添加剤の含有量は、熱伝導性組成物の特性を損なわない範囲であれば、特に限定されない。すなわち、一般的な熱伝導性グリースに通常用いている含有量と同程度の量を含ませることができる。 The content of these additives is not particularly limited as long as it does not impair the properties of the thermally conductive composition. That is, it can be contained in an amount comparable to that normally used in general thermally conductive grease.
≪２．熱伝導性組成物の製造方法>>
本実施の形態に係る熱伝導性組成物は、各成分を混合することにより製造することができる。製造方法としては、均一に成分を混合できる方法であれば特に限定されず、例えば、一般的なグリースの製造方法等を採用することができる。
≪2. Manufacturing method of thermally conductive composition>>
The thermally conductive composition according to this embodiment can be manufactured by mixing each component. The manufacturing method is not particularly limited as long as the components can be mixed uniformly, and for example, a general grease manufacturing method can be adopted.
具体的な製造方法としては、プラネタリーミキサー、自転公転ミキサー等により混練りを行い、グリース状にした後、さらに三本ロールにてより均一に混練りする方法を用いることができる。 As a specific manufacturing method, a method can be used in which the mixture is kneaded using a planetary mixer, an autorotation-revolution mixer, etc. to form a grease, and then kneaded more uniformly using three rolls.
以下、本発明の実施例及び比較例を示して、本発明についてより具体的に説明する。なお、本発明は以下の実施例によって何ら限定されるものではない。 EXAMPLES Hereinafter, the present invention will be explained in more detail by showing examples and comparative examples of the present invention. Note that the present invention is not limited in any way by the following examples.
≪実施例、比較例≫
下記（Ａ）～（Ｄ）に示す各材料を用い、下記表１に示す組成の熱伝導性グリースを作製した。
≪Example, comparative example≫
A thermally conductive grease having a composition shown in Table 1 below was prepared using each material shown in (A) to (D) below.
（構成材料）
（Ａ）熱伝導性充填剤：酸化亜鉛
・Ａ１：平均粒径１１μｍ
・Ａ２：平均粒径０．６μｍ
（Ｂ）基油
・Ｂ１：パーフルオロポリオキセタン
（ダイキン社製 デムナムＳ６５ 重合平均分子量：４５００）
・Ｂ２：パーフルオロポリエーテル
（ソルベイソレクシス社製 Ｆｏｍｂｌｉｎ ＹＵ７００ 重合平均分子量：５０００）
・Ｂ３：パーフルオロアルキルエーテル
（Ｄｙｐｏｎｔ社製 Ｋｒｙｔｏｘ ＧＰＬ１０７ 重合平均分子量：７５００）
（Ｃ）分散剤
・Ｃ１：含フッ素基・親水性含有オリゴマー（ＤＩＣ社製 メガファックＦ４３０）
（Ｄ）増ちょう剤
・Ｄ１：ポリテトラフルオロエチレン（ＰＴＦＥ）（喜多村社製 ＫＴＬ１００）
(Constituent material)
(A) Thermal conductive filler: Zinc oxide・A1: Average particle size 11 μm
・A2: Average particle size 0.6 μm
(B) Base oil/B1: Perfluoropolyoxetane (Daikin Demnum S65 polymerization average molecular weight: 4500)
・B2: Perfluoropolyether (Fomblin YU700, manufactured by Solvay Solexis, polymerization average molecular weight: 5000)
・B3: Perfluoroalkyl ether (Krytox GPL107 manufactured by Dypont, polymerization average molecular weight: 7500)
(C) Dispersant・C1: Fluorine-containing group・hydrophilic-containing oligomer (Megafac F430 manufactured by DIC Corporation)
(D) Thickener/D1: Polytetrafluoroethylene (PTFE) (KTL100 manufactured by Kitamura Co., Ltd.)
下記表１に示すように各材料（Ａ）～（Ｄ）をプラネタリーミキサーにて混合しグリース状とした。その後、三本ロールによる混練を行うことにより各材料を十分に分散させて、実施例及び比較例の熱伝導性グリースを製造した。 As shown in Table 1 below, each of the materials (A) to (D) was mixed in a planetary mixer to form a grease. Thereafter, each material was sufficiently dispersed by kneading with three rolls to produce thermally conductive greases of Examples and Comparative Examples.
［熱伝導性グリースの評価］
（粘度評価）
粘度評価には、レオメーターを用いて室温下でせん断速度が６Ｓ－１のときの粘度を測定した。測定結果を表１に示す。
[Evaluation of thermally conductive grease]
(Viscosity evaluation)
For viscosity evaluation, the viscosity was measured at room temperature using a rheometer at a shear rate of 6S -1 . The measurement results are shown in Table 1.
（熱伝導率測定）
実施例及び比較例の熱伝導性グリースついて、熱伝導率を測定した。具体的には、京都電子工業社製迅速熱伝導率計ＱＴＭ－５００により室温にて熱伝導率を測定した。なお、熱伝導率は高いほど熱伝導性グリースとしては好ましい。
(Thermal conductivity measurement)
Thermal conductivity was measured for the thermally conductive greases of Examples and Comparative Examples. Specifically, the thermal conductivity was measured at room temperature using a rapid thermal conductivity meter QTM-500 manufactured by Kyoto Electronics Industry Co., Ltd. Note that the higher the thermal conductivity, the more preferable the thermally conductive grease is.
（耐熱性評価）
耐熱性はＥＩＡＪ ＥＤ－４７０１／１０６に準じたパワーサイクル試験において、熱抵抗増加率が１０％以内を示す限界回数（耐久サイクル数）により評価した。パワーサイクル試験は、富士電機株式会社製パワーモジュール２ ＭＢ１３００ＶＮ－１２０－５０を用い、Ｔｊ（ジャンクション温度）１６５℃を到達温度に、ΔＴｊ１００℃として、昇温時間６０秒、降温時間１２０秒を１サイクルとした。測定結果を表１に示す。なお、耐久サイクル数は１０００以上あれば十分に耐熱性を有すると評価できる。
(Heat resistance evaluation)
Heat resistance was evaluated in a power cycle test according to EIAJ ED-4701/106 based on the limit number of times (endurance cycle number) showing a thermal resistance increase rate of 10% or less. The power cycle test was conducted using Fuji Electric Co., Ltd.'s power module 2 MB1300VN-120-50, with Tj (junction temperature) of 165°C as the final temperature, ΔTj of 100°C, and one cycle of heating time of 60 seconds and cooling time of 120 seconds. And so. The measurement results are shown in Table 1. It should be noted that if the durability cycle number is 1000 or more, it can be evaluated as having sufficient heat resistance.
（基油残存率評価）
上記の実施例及び比較例の熱伝導性グリースついて、基油残存率を測定した。具体的には、２５０℃８時間保持後の基油の残存量を求め、初期投入量に対する基油残存率を算出した。算出結果を表１に示す。なお、基油残存率は高いほど熱伝導性グリースとして好ましい。具体的には、８０％以上であることが好ましい。
(Base oil residual rate evaluation)
Base oil residual rates were measured for the thermally conductive greases of the above Examples and Comparative Examples. Specifically, the residual amount of the base oil after being held at 250° C. for 8 hours was determined, and the base oil residual rate with respect to the initial input amount was calculated. The calculation results are shown in Table 1. Note that the higher the base oil residual rate, the more preferable it is as a thermally conductive grease. Specifically, it is preferably 80% or more.
表１より、重合平均分子量が４５００のパーフルオロポリオキセタンである基油を含有した実施例１、２の熱伝導性グリースは、高い熱伝導率を有するとともに優れた耐熱性を有する熱伝導性グリースであることが分かる。 From Table 1, the thermally conductive greases of Examples 1 and 2 containing the base oil of perfluoropolyoxetane with a polymerization average molecular weight of 4500 are thermally conductive greases that have high thermal conductivity and excellent heat resistance. It turns out that it is.
一方、パーフルオロポリオキセタンではない基油を含有した比較例１、２の熱伝導性グリースは耐熱性の低い熱伝導性グリースであることが分かる。 On the other hand, it can be seen that the thermally conductive greases of Comparative Examples 1 and 2 containing base oils other than perfluoropolyoxetane are thermally conductive greases with low heat resistance.
以上より、重合平均分子量が３５００以上５０００未満のパーフルオロポリオキセタンである基油を含有した本発明の熱伝導性組成物であれば、高い耐熱性を有するとともに優れた熱伝導性を有することが確認された。 From the above, the thermally conductive composition of the present invention containing a base oil that is a perfluoropolyoxetane with a polymerization average molecular weight of 3,500 or more and less than 5,000 has high heat resistance and excellent thermal conductivity. confirmed.
Claims (3)
さらにフッ素系分散剤を含有する分散剤を含有し、
前記基油は重量平均分子量が３５００以上５０００未満のパーフルオロポリオキセタンであり、
前記熱伝導性充填剤の含有量は、当該熱伝導性組成物１００質量％に対し９０質量％以上９７質量％以下の割合である
熱伝導性組成物。 Contains at least a thermally conductive filler and a base oil,
Furthermore, it contains a dispersant containing a fluorine-based dispersant,
The base oil is a perfluoropolyoxetane with a weight average molecular weight of 3500 or more and less than 5000,
The content of the thermally conductive filler is in a proportion of 90% by mass or more and 97% by mass or less based on 100% by mass of the thermally conductive composition.
請求項１に記載の熱伝導性組成物。 The thermally conductive composition according to claim 1, which has a viscosity of 1000 Pa·s or less when measured at room temperature using a rheometer at a shear rate of 6S −1 .
請求項１又は２に記載の熱伝導性組成物。 The thermally conductive composition according to claim 1 or 2, wherein the content of the base oil is in a proportion of 2% by mass or more and 4.5 % by mass or less based on 100% by mass of the thermally conductive composition.
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| JP2002201483A (en) | 2001-01-04 | 2002-07-19 | Hitachi Ltd | High thermal conductive grease composition and cooling apparatus using the same |
| WO2014034508A1 (en) | 2012-08-27 | 2014-03-06 | 日本バルカー工業株式会社 | Molded body suppressed in bleeding and method for producing same |
| JP2017082090A (en) | 2015-10-28 | 2017-05-18 | 信越化学工業株式会社 | Heat-conductive fluorine-containing curable composition, cured product of the same, and electric and electronic component |
| JP2017115099A (en) | 2015-12-25 | 2017-06-29 | 住鉱潤滑剤株式会社 | Solvent dilution type fluorine-based lubricant composition |
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| JP2002201483A (en) | 2001-01-04 | 2002-07-19 | Hitachi Ltd | High thermal conductive grease composition and cooling apparatus using the same |
| WO2014034508A1 (en) | 2012-08-27 | 2014-03-06 | 日本バルカー工業株式会社 | Molded body suppressed in bleeding and method for producing same |
| JP2017082090A (en) | 2015-10-28 | 2017-05-18 | 信越化学工業株式会社 | Heat-conductive fluorine-containing curable composition, cured product of the same, and electric and electronic component |
| JP2017115099A (en) | 2015-12-25 | 2017-06-29 | 住鉱潤滑剤株式会社 | Solvent dilution type fluorine-based lubricant composition |
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