JP7237884B2 - 熱伝導性シリコーン組成物 - Google Patents
熱伝導性シリコーン組成物 Download PDFInfo
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- JP7237884B2 JP7237884B2 JP2020073777A JP2020073777A JP7237884B2 JP 7237884 B2 JP7237884 B2 JP 7237884B2 JP 2020073777 A JP2020073777 A JP 2020073777A JP 2020073777 A JP2020073777 A JP 2020073777A JP 7237884 B2 JP7237884 B2 JP 7237884B2
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- thermally conductive
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- silicone composition
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- conductive silicone
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- 229920001296 polysiloxane Polymers 0.000 title claims description 81
- 239000000203 mixture Substances 0.000 title claims description 60
- 239000002245 particle Substances 0.000 claims description 23
- 239000000843 powder Substances 0.000 claims description 23
- 238000002844 melting Methods 0.000 claims description 20
- 230000008018 melting Effects 0.000 claims description 20
- 125000004432 carbon atom Chemical group C* 0.000 claims description 19
- 125000003342 alkenyl group Chemical group 0.000 claims description 13
- 229910000807 Ga alloy Inorganic materials 0.000 claims description 11
- 239000011231 conductive filler Substances 0.000 claims description 11
- 125000001183 hydrocarbyl group Chemical group 0.000 claims description 11
- 125000000217 alkyl group Chemical group 0.000 claims description 8
- 229910045601 alloy Inorganic materials 0.000 claims description 6
- 239000000956 alloy Substances 0.000 claims description 6
- 229910001128 Sn alloy Inorganic materials 0.000 claims description 5
- 229910052582 BN Inorganic materials 0.000 claims description 4
- 229910016338 Bi—Sn Inorganic materials 0.000 claims description 4
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 4
- 229910000846 In alloy Inorganic materials 0.000 claims description 4
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 4
- 239000000395 magnesium oxide Substances 0.000 claims description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 4
- 229910020994 Sn-Zn Inorganic materials 0.000 claims description 3
- 229910009069 Sn—Zn Inorganic materials 0.000 claims description 3
- -1 2-methyl-2-phenylethyl Chemical group 0.000 description 8
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 239000004519 grease Substances 0.000 description 7
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 229910052733 gallium Inorganic materials 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000004020 conductor Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- 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 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 2
- 125000003710 aryl alkyl group Chemical group 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 2
- 229910052794 bromium Inorganic materials 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000001186 cumulative effect Effects 0.000 description 2
- 125000004093 cyano group Chemical group *C#N 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
- 125000001511 cyclopentyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C1([H])[H] 0.000 description 2
- 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 2
- 239000004205 dimethyl polysiloxane Substances 0.000 description 2
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 2
- 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 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 125000005843 halogen group Chemical group 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 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 2
- 239000007788 liquid Substances 0.000 description 2
- 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 2
- 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 2
- 125000003854 p-chlorophenyl group Chemical group [H]C1=C([H])C(*)=C([H])C([H])=C1Cl 0.000 description 2
- 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 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 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 2
- 125000003944 tolyl group Chemical group 0.000 description 2
- 125000000026 trimethylsilyl group Chemical group [H]C([H])([H])[Si]([*])(C([H])([H])[H])C([H])([H])[H] 0.000 description 2
- 229910001297 Zn alloy Inorganic materials 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 125000000753 cycloalkyl group Chemical group 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- ZKVLEFBKBNUQHK-UHFFFAOYSA-N helium;molecular nitrogen;molecular oxygen Chemical compound [He].N#N.O=O ZKVLEFBKBNUQHK-UHFFFAOYSA-N 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 150000004812 organic fluorine compounds Chemical class 0.000 description 1
- 150000001282 organosilanes Chemical class 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- GZCWPZJOEIAXRU-UHFFFAOYSA-N tin zinc Chemical compound [Zn].[Sn] GZCWPZJOEIAXRU-UHFFFAOYSA-N 0.000 description 1
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- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
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Description
(A)25℃での動粘度が10~500,000mm2/sであるオルガノポリシロキサン:100質量部
(B)平均粒径が0.01~100μmの熱伝導性充填剤:10~2,000質量部
(C)融点が-20~100℃である、ガリウム又はガリウム合金:1,000~10,000質量部
R1 aSiO(4-a)/2 (1)
(式中、R1は、アルケニル基を含まない、互いに独立に、炭素数1~18の、非置換または置換の一価炭化水素基であり、1.8≦a≦2.2である)
で表されるオルガノポリシロキサンである熱伝導性シリコーン組成物であることが好ましい。
で表される加水分解性基含有オルガノポリシロキサンを、前記(A)成分の全質量に対して10~100質量%の量で含む熱伝導性シリコーン組成物であることが好ましい。
(A)25℃での動粘度が10~500,000mm2/sであるオルガノポリシロキサン:100質量部
(B)平均粒径が0.01~100μmの熱伝導性充填剤:10~2,000質量部
(C)融点が-20~100℃である、ガリウム又はガリウム合金:1,000~10,000質量部
(A)成分は、25℃での動粘度が10~500,000mm2/s、好ましくは30~100,000mm2/s、更に好ましくは30~10,000mm2/sであるオルガノポリシロキサンである。オルガノポリシロキサンの動粘度が上記下限値より低いとグリースにした時にオイルブリードが出やすくなる。また、上記上限値より大きいと、シリコーン組成物の伸展性が乏しくなるため好ましくない。なお、本発明において、オルガノポリシロキサンの動粘度はオストワルド粘度計で測定した25℃の値である。
R1 aSiO(4-a)/2 (1)
(B)成分は、熱伝導性充填剤である。熱伝導性充填剤の種類は特に制限されず、従来放熱用(熱伝導性)グリースに使用されている粉末を使用できる。特には、熱伝導率の高いものがよく、酸化亜鉛粉末、アルミナ粉末、窒化ホウ素粉末、窒化アルミニウム粉末、水酸化アルミニウム粉末、酸化マグネシウム粉末の中から選択される少なくとも1種又は2種以上が好ましい。これら無機化合物粉体は、必要に応じてオルガノシラン、オルガノシラザン、オルガノポリシロキサン、有機フッ素化合物等により、その表面に疎水化処理を施したものを使用しても良い。疎水化処理は上記式(2)で示されるオルガノポリシロキサンで行うこともできる。
本発明の(C)成分はガリウム又はガリウム合金であって、その融点は、-20~100℃の範囲とすることが必要である。-20℃を下回るものは作製が難しいため経済的に好ましくなく、100℃を超えると組成物調製工程において速やかに融解しないため作業性に劣る結果となるし、製造中に析出して不均一になる。よって、融点が-20~100℃の範囲であるガリウム又はガリウム合金であることが、経済的にも、取り扱い上必要な条件であるとともに適切な範囲である。特に、-20~50℃の範囲内のものが好ましい。
また、本発明のシリコーン組成物は、必要に応じて、従来公知の酸化防止剤、染料、顔料、難燃剤、沈降防止剤、又はチクソ性向上剤等を、目的に応じた量で配合することができる。
(A-1)両末端がトリメチルシリル基で封鎖され、25℃における動粘度が1,000mm2/sのジメチルポリシロキサン。
(A-2)両末端がトリメチルシリル基で封鎖され、25℃における動粘度が5,000mm2/sのジメチルポリシロキサン。
(A-3)25℃における動粘度が35mm2/sの下記式(4)で示されるオルガノポリシロキサン
(B-1)酸化亜鉛粉末:平均粒径1.0μm
(B-2)アルミナ粉末:平均粒径8.9μm
(B-3)窒化ホウ素粉末:平均粒径2.0μm
(B-4)窒化アルミニウム粉末:平均粒径6.8μm
(B-5)水酸化アルミニウム粉末:平均粒径25μm
(B-6)酸化マグネシウム粉末:平均粒径45μm
(C-1)金属ガリウム〔融点=29.8℃〕
(C-2)Ga-In合金〔質量比=75.4:24.6、融点=15.7℃〕
(C-3)Ga-In-Bi-Sn合金〔質量比=9.4:47.3:24.7:18.6、融点=48.0℃〕
(C-4)Ga-In-Sn合金〔質量比=68.5:21.5:10、融点=-19℃〕
(C-5)金属インジウム〔融点=156.2℃〕<比較用>
シリコーン組成物の調製
上記(A)~(C)成分を、下記表1、2に示す組成及び配合量に従い、容量5リットルのプラネタリーミキサー(井上製作所(株)製、登録商標)に投入し、室温にて1時間撹拌してシリコーン組成物を調製した。
尚、融点が室温より高い(C-1)、(C-3)、(C-5)はオーブンであらかじめ溶解させておいてから投入した。
組成物の25℃における絶対粘度の測定は、株式会社マルコム社製の型番PC-1TL(10rpm)にて行った。
熱伝導率は、京都電子工業株式会社製のTPS-2500Sにより、いずれも25℃において測定した。
熱伝導性充填剤((B)成分)の粒径測定は、日機装株式会社製の粒度分析計であるマイクロトラックMT3300EXにより測定した体積基準の累積平均径である。
Claims (6)
- 下記(A)~(C)成分を含むものであることを特徴とする熱伝導性シリコーン組成物。
(A)25℃での動粘度が10~500,000mm2/sであり、下記一般式(2)で表される加水分解性基を有するオルガノポリシロキサンと、下記式(3)で表される直鎖状オルガノポリシロキサンとを含むオルガノポリシロキサン:100質量部
(B)平均粒径が0.01~100μmの熱伝導性充填剤:10~2,000質量部
(C)融点が-20~100℃である、ガリウム又はガリウム合金:1,000~10,000質量部
- 前記(A)成分がアルケニル基を含まないことを特徴とする請求項1に記載の熱伝導性シリコーン組成物。
- 前記(B)成分が、酸化亜鉛粉末、アルミナ粉末、窒化ホウ素粉末、窒化アルミニウム粉末、水酸化アルミニウム粉末、酸化マグネシウム粉末の中から選択される1種以上であることを特徴とする請求項1又は請求項2に記載の熱伝導性シリコーン組成物。
- 前記(A)成分が下記平均組成式(1)
R1 aSiO(4-a)/2 (1)
(式中、R1は、アルケニル基を含まない、互いに独立に、炭素数1~18の、非置換または置換の一価炭化水素基であり、1.8≦a≦2.2である)
で表されるオルガノポリシロキサンであることを特徴とする請求項1から請求項3のいずれか1項に記載の熱伝導性シリコーン組成物。 - 前記(C)成分のガリウム合金が、Ga-In合金、Ga-Sn-Zn合金、Ga-In-Sn合金、Ga-In-Bi-Sn合金の中から選択される1種以上であることを特徴とする請求項1から請求項5のいずれか1項に記載の熱伝導性シリコーン組成物。
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