JP7047199B1 - 熱伝導性グリース組成物 - Google Patents
熱伝導性グリース組成物 Download PDFInfo
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- JP7047199B1 JP7047199B1 JP2022503964A JP2022503964A JP7047199B1 JP 7047199 B1 JP7047199 B1 JP 7047199B1 JP 2022503964 A JP2022503964 A JP 2022503964A JP 2022503964 A JP2022503964 A JP 2022503964A JP 7047199 B1 JP7047199 B1 JP 7047199B1
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- Prior art keywords
- grease composition
- heat conductive
- mass
- conductive grease
- parts
- 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.)
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- 239000004519 grease Substances 0.000 title claims abstract description 55
- 239000000203 mixture Substances 0.000 title claims abstract description 41
- 239000002245 particle Substances 0.000 claims abstract description 38
- 229910052582 BN Inorganic materials 0.000 claims abstract description 12
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000005484 gravity Effects 0.000 claims abstract description 12
- 229920000089 Cyclic olefin copolymer Polymers 0.000 claims abstract description 11
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000005977 Ethylene Substances 0.000 claims abstract description 11
- 239000004711 α-olefin Substances 0.000 claims abstract description 11
- 125000004432 carbon atom Chemical group C* 0.000 claims description 11
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 8
- 125000000217 alkyl group Chemical group 0.000 claims description 6
- 125000000962 organic group Chemical group 0.000 claims description 6
- 229920001577 copolymer Polymers 0.000 claims description 5
- 230000035939 shock Effects 0.000 claims description 4
- 239000004034 viscosity adjusting agent Substances 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- -1 silane compound Chemical class 0.000 abstract description 7
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 abstract description 5
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 abstract description 5
- 125000003545 alkoxy group Chemical group 0.000 abstract description 2
- 229910000077 silane Inorganic materials 0.000 abstract description 2
- 239000011347 resin Substances 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 238000004381 surface treatment Methods 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 5
- 229920001296 polysiloxane Polymers 0.000 description 5
- KQAHMVLQCSALSX-UHFFFAOYSA-N decyl(trimethoxy)silane Chemical compound CCCCCCCCCC[Si](OC)(OC)OC KQAHMVLQCSALSX-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000011231 conductive filler Substances 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229920002545 silicone oil Polymers 0.000 description 2
- 125000006850 spacer group Chemical group 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- NMEPHPOFYLLFTK-UHFFFAOYSA-N trimethoxy(octyl)silane Chemical compound CCCCCCCC[Si](OC)(OC)OC NMEPHPOFYLLFTK-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 125000005370 alkoxysilyl group Chemical group 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 229920005601 base polymer Polymers 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- BAAAEEDPKUHLID-UHFFFAOYSA-N decyl(triethoxy)silane Chemical compound CCCCCCCCCC[Si](OCC)(OCC)OCC BAAAEEDPKUHLID-UHFFFAOYSA-N 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- YGUFXEJWPRRAEK-UHFFFAOYSA-N dodecyl(triethoxy)silane Chemical compound CCCCCCCCCCCC[Si](OCC)(OCC)OCC YGUFXEJWPRRAEK-UHFFFAOYSA-N 0.000 description 1
- SCPWMSBAGXEGPW-UHFFFAOYSA-N dodecyl(trimethoxy)silane Chemical compound CCCCCCCCCCCC[Si](OC)(OC)OC SCPWMSBAGXEGPW-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- MSRJTTSHWYDFIU-UHFFFAOYSA-N octyltriethoxysilane Chemical compound CCCCCCCC[Si](OCC)(OCC)OCC MSRJTTSHWYDFIU-UHFFFAOYSA-N 0.000 description 1
- 229960003493 octyltriethoxysilane Drugs 0.000 description 1
- 239000011146 organic particle Substances 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000012756 surface treatment agent Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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- C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
- C10N2020/01—Physico-chemical properties
- C10N2020/055—Particles related characteristics
- C10N2020/061—Coated particles
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/02—Pour-point; Viscosity index
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/28—Anti-static
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2050/00—Form in which the lubricant is applied to the material being lubricated
- C10N2050/10—Semi-solids; greasy
Abstract
Description
A 40℃における動粘度が10,000mm2/s以下のエチレン・α-オレフィン共重合体を100質量部と、
B 熱伝導性粒子を、A成分100質量部に対して115~580質量部を含み、
前記熱伝導性粒子は、
B1 中心粒子径が0.1~1μmの不定形アルミナであり、一部または全部がRaSi(OR’)4-a(但し、Rは炭素数8~12の非置換または置換有機基、R’は炭素数1~4のアルキル基、aは0もしくは1)で示されるアルコキシシラン化合物又はその部分加水分解物で表面処理されているもの55~350質量部と、
B2 中心粒子径が0.1~10μmの板状窒化ホウ素を5~60質量部と、
B3 中心粒子径が20~70μmの凝集窒化ホウ素を55~170質量部を含み、
B3成分/B2成分=2~20となる質量割合で配合されていることを特徴とする。
A 40℃における動粘度が10,000mm2/s以下のエチレン・α-オレフィン共重合体を100質量部と、
B 熱伝導性粒子を、A成分100質量部に対して115~580質量部を含む。B成分は130~550質量部が好ましく、より好ましくは160~500質量部である。
B1 中心粒子径が0.1~1μmの不定形アルミナであり、一部または全部がRaSi(OR’)4-a(但し、Rは炭素数8~12の非置換または置換有機基、R’は炭素数1~4のアルキル基、aは0もしくは1)で示されるアルコキシシラン化合物又はその部分加水分解物で表面処理されているもの55~350質量部と、
B2 中心粒子径が0.1~10μmの板状窒化ホウ素を5~60質量部と、
B3 中心粒子径が20~70μmの凝集窒化ホウ素を55~170質量部を含み、
B3成分/B2成分=2~20となる割合で配合されている。
前記において「一部」とは50質量%以上をいう。
アルコキシシラン化合物は予め熱伝導性粒子と混合して前処理しておくのが好ましい。熱伝導性粒子100質量部に対し、アルコキシシラン化合物は0.01~10質量部添加するのが好ましい。表面処理することでマトリックス樹脂に充填されやすくなる効果がある。
なお、不定形アルミナは、粉砕ないしは破砕によって製造され、市販品を使用できる。
熱伝導性グリースの熱伝導率は、ホットディスク(ISO/CD 22007-2準拠)により測定した。この熱伝導率測定装置1は図1Aに示すように、ポリイミドフィルム製センサ2を2個の試料3a,3bで挟み、センサ2に定電力をかけ、一定発熱させてセンサ2の温度上昇値から熱特性を解析する。センサ2は先端4が直径7mmであり、図1Bに示すように、電極の2重スパイラル構造となっており、下部に印加電流用電極5と抵抗値用電極(温度測定用電極)6が配置されている。熱伝導率は以下の式(数1)で算出する。
グリースの絶対粘度はB型粘度計(ブルックフィールド社製HBDV2T)で測定した。スピンドルはT-Eスピンドルを使用し、回転速度5rpm、23℃における絶対粘度を測定した。
<落下試験>
図2A-Dに示す落下試験により測定した。
タテ40 mm、ヨコ100mm、厚さ5mmのアルミプレート12と、タテ40mm、ヨコ100mm、厚さ5mmのガラスプレート11の間に0.4gの熱伝導性グリース4を塗付し(図2A)、スペーサー13を介在させて厚さ0.5mmとなるように圧縮挟持した(図2B)。15は厚さ0.5mmまで圧縮された熱伝導性グリースである。次に、アルミプレート12とガラスプレート11の隙間が垂直になるようにヒートサイクル試験機に設置した(図2C)。16は試験前の試験片である。この状態で、-40℃と125℃で30分ずつ保持するヒートサイクル試験を行った。100サイクル経過した段階で試験片を取り出し、熱伝導性グリース15が落下していないか観察した。17は試験後の試験片(図2D)、18は落下距離である。熱伝導性グリースの落下が5mm以内であればA、5mmを超えた場合はBと判定した。
1.原料成分
(1)A成分:エチレン・プロピレン共重合体
・40℃における動粘度が400mm2/sのエチレン・プロピレン共重合体:三井化学社製、商品名"ルーカントLX004"
・40℃における動粘度が110mm2/sの非硬化性のシリコーンオイル(ジメチルポリシロキサン)
を表1に示す割合で使用した。
(2)B成分:熱伝導性粒子
・中心粒径0.3μm(D50=0.3μm)の不定形アルミナ:オクチルトリメトキシシラン前処理品(アルミナ100gに対してオクチルトリメトキシシラン2.4gを吸着させたもの)
・中心粒径5μm(D50=5μm)の板状窒化ホウ素(表面処理無し)
・中心粒径60μm(D50=60μm)の球状凝集窒化ホウ素(表面処理無し)
・中心粒径2.3μm(D50=2.3μm)の不定形アルミナ:デシルトリメトキシシラン前処理品(アルミナ100gに対してデシルトリメトキシシラン1.1gを吸着させたもの)
・中心粒径20μm(D50=20μm)の球状アルミナ(表面処理無し)
配合量は表1に示す。
(3)C成分:粘度調整剤
・デシルトリメトキシシラン
2.混合方法
上記A成分に熱伝導性粒子と粘度調整剤を混合し、熱伝導性グリース組成物とした。
以上のようにして得たグリースを評価した。条件と結果を次の表1にまとめて示す。
これに対し、比較例1はマトリックス樹脂としてシリコーンオイルを使用したため、実施例1~2に比べて低分子シロキサン発生の問題があり、耐落下性、比重も好ましくなかった。比較例2はB2,B3成分を使用しなかったため、実施例1~2に比べて耐落下性、比重は好ましくなかった。
2 センサ
3a,3b 試料
4 センサの先端
5 印加電流用電極
6 抵抗値用電極(温度測定用電極)
11 ガラスプレート
12 アルミプレート
13 スペーサー
14 熱伝導性グリース
15 圧縮された熱伝導性グリース
16 試験前の試験片
17 試験後の試験片
18 落下距離
Claims (8)
- 非硬化性の熱伝導性グリース組成物であって、
A 40℃における動粘度が10,000mm2/s以下のエチレン・α-オレフィン共重合体を100質量部と、
B 熱伝導性粒子を、A成分100質量部に対して115~580質量部を含み、
前記熱伝導性粒子は、
B1 中心粒子径が0.1~1μmの不定形アルミナであり、一部または全部がRaSi(OR’)4-a(但し、Rは炭素数8~12の非置換または置換有機基、R’は炭素数1~4のアルキル基、aは0もしくは1)で示されるアルコキシシラン化合物又はその部分加水分解物で表面処理されているもの55~350質量部と、
B2 中心粒子径が0.1~10μmの板状窒化ホウ素を5~60質量部と、
B3 中心粒子径が20~70μmの凝集窒化ホウ素を55~170質量部を含み、
B3成分/B2成分=2~20となる質量割合で配合されていることを特徴とする熱伝導性グリース組成物。 - 前記熱伝導性グリース組成物は、さらに粘度調整剤:C成分として、RaSi(OR’)4-a(但し、Rは炭素数8~12の非置換または置換有機基、R’は炭素数1~4のアルキル基、aは0もしくは1)で示されるアルコキシシラン化合物を0.1~2質量部含む請求項1に記載の熱伝導性グリース組成物。
- 前記熱伝導性グリース組成物の熱伝導率は、2.0W/m・K以上8.0W/m・K以下である請求項1又は2に記載の熱伝導性グリース組成物。
- 前記エチレン・α-オレフィン共重合体は比重が0.83~0.85である請求項1~3のいずれか1項に記載の熱伝導性グリース組成物。
- 前記熱伝導性グリース組成物は比重が1.0以上2.4以下である請求項1~4のいずれか1項に記載の熱伝導性グリース組成物。
- 前記熱伝導性グリース組成物は、B型粘度計で測定した絶対粘度が1,000~20,000Pasである請求項1~5のいずれか1項に記載の熱伝導性グリース組成物。
- 前記熱伝導性グリース組成物は、2枚のプレート間に0.4gを配置し、厚さ0.5mmに圧縮挟持し、前記2枚のプレートを垂直に保持してヒートショック試験機内に設置し、-40℃と125℃で30分ずつ保持し、100サイクル経過させるヒートショック試験において、グリースの落下が5mm以内である請求項1~6のいずれか1項に記載の熱伝導性グリース組成物。
- 前記エチレン・α-オレフィン共重合体はエチレン・プロピレン共重合体である請求項1~7のいずれか1項に記載の熱伝導性グリース組成物。
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