JP5005538B2 - バルク熱伝導率を増大させるためのナノ材料含有有機マトリックス - Google Patents
バルク熱伝導率を増大させるためのナノ材料含有有機マトリックス Download PDFInfo
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- JP5005538B2 JP5005538B2 JP2007527154A JP2007527154A JP5005538B2 JP 5005538 B2 JP5005538 B2 JP 5005538B2 JP 2007527154 A JP2007527154 A JP 2007527154A JP 2007527154 A JP2007527154 A JP 2007527154A JP 5005538 B2 JP5005538 B2 JP 5005538B2
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- colloidal silica
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- H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
- H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
- H01L23/3737—Organic materials with or without a thermoconductive filler
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- General Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
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- Compositions Of Macromolecular Compounds (AREA)
- Cooling Or The Like Of Semiconductors Or Solid State Devices (AREA)
Description
"Thermally Conductive Polymer Compositions," D.M. Bigg., Polymer Composites, June 1986, Vol.7, No.3
式中、R1は各々独立にC1−18一価炭化水素基又はC6−14アリール基であり、C1−18一価炭化水素基は適宜アルキルアクリレート、アルキルメタクリレート、エポキシド、ビニル、アリル、スチレン系、シリル又はシロキシル基でさらに官能化されていてもよく、R2は各々独立にC1−18一価炭化水素基又は水素基であり、「a」は1〜3の整数である。好ましくは、本発明の技術的範囲に属するオルガノアルコキシシランは、2−(3,4−エポキシシクロヘキシル)エチルトリメトキシシラン、3−グリシドキシプロピルトリメトキシシラン、フェニルトリメトキシシラン、メタクリルオキシプロピルトリメトキシシラン(MAPTMS)、1−ヘキセニルトリエトキシシラン、n−オクチルトリエトキシシラン、n−ドデシルトリエトキシシラン及び2−(3−ビニル−テトラメチルジシロキシル)−エチルトリメトキシシランである。複数の官能基の組合せも可能である。通例、オルガノアルコキシシランは、コロイダルシリカに含まれる二酸化ケイ素の重量を基準にして約2〜約60重量%存在する。得られたオルガノ官能化コロイダルシリカはpHを中和するため酸又は塩基で処理してもよい。酸又は塩基並びにシラノールとアルコキシシラン基の縮合を促進するその他の触媒も、官能化プロセスの促進に使用できる。かかる触媒としては、有機チタン及び有機スズ化合物、例えば、テトラブチルチタネート、チタンイソプロポキシビス(アセチルアセトナト)、ジブチルスズジラウレート、ジブチルスズジアセテート又はこれらの組合せが挙げられる。
4.95gの分散体組成物は、31wt%(wt%は未官能化コロイダルSiO2を基準)のメタクリルオキシプロピルトリメトキシシラン(「MAPTMS」)官能化コロイダルSiO2(20nm)とアクリルオキシ末端ポリジメチルシロキサン(Gelest社製DMSU22、MW約1000〜1200)からなるものであった。さらに、2gのMAPTMS、0.13gのヨードニウム塩(GE Silicones社製UV9380c)及び45.6gのアルミナ(昭和電工(株)製AS10)を分散体組成物にブレンドした。アルミナの添加量は配合物全体の86.5wt%であった。分散体組成物を120℃で硬化させた。分散体組成物の熱伝導率を測定したところ、室温で2.6W/m−K±0.05、100℃で2.55W/m−Kであった。比較として、アクリレート単独の熱伝導率は86.5wt%のアルミナ(平均粒径=38ミクロン)を充填したとき100℃で約1.4〜1.9w/m−Kである。表1参照。
1.82gのオクタキス(ジメチルシロキシ−T8−シルセキオキサン)(T8 OSiMe2H、Gelest社製)、0.73gの1,5−ヘキサメチル−トリシロキサン(MHDMH GE Silicones社製)、1.53gの1,3−ジビニルテトラメチルジシロキサン(GE Silicones社製)、1.04gのビニル末端ポリジメチルシロキサン(Gelest社製、MW9400)DMSV22、適当な触媒及び20gのアルミナ(昭和電工(株)製AS−40及び住友化学(株)製AA04)の分散体組成物をブレンドした。アルミナの添加量は配合物全体の約80wt%であった。分散体組成物を80℃で硬化させた。分散体組成物の熱伝導率を測定したところ、室温で1.99W/m−K±0.15、100℃で1.70W/m−K±0.10であった。比較として、ポリジメチルシロキサン(「PDMS」)の熱伝導率は80wt%のアルミナ(平均粒径はAS40では10μm、AA04では0.4μm)を充填したとき約1.00W/m−Kである。表1参照。
7gのGE Silicones社製FCS100(1,6−ヘキサンジオールジアクリレート中に40wt%のMAPTMS官能化コロイダルSiO2を含む)、0.14gのヨードニウム塩(GE Silicones社製UV9380c)及び43gのアルミナ(昭和電工(株)製AS50及び住友化学(株)製AA04)を含む分散体組成物をブレンドした。アルミナの添加量は配合物全体の86wt%であった。分散体の熱伝導率を測定したところ、室温で3.35W/m−K±0.20W/m−K、100℃で3.25W/m−K±0.15であった。比較として、アクリレートの熱伝導率は86.5wt%のアルミナ(平均粒径はAS50では10μm、住友化学(株)製では0.4μm)を充填したとき100℃で約1.4〜1.9w/m−Kである。表1参照。
最終分散体は、脂環式エポキシ樹脂(Dow社製UVR6105)中に、56wt%のフェニルトリメトキシシラン官能化コロイダルシリカ(SiO2含量及び官能基を基準)、触媒として1wt%のヨードニウム塩(GE Silicones社製UV9392c)及び0.5wt%のベンゾイルピナコール(Aldrich社製)からなるものであった。分散体を156℃で5分間硬化させ、測定したところ熱伝導率は25℃で0.37W/m−Kであった。ナノ粒子を含まない典型的なエポキシの熱伝導率は25℃で0.2〜0.25W/m−Kである。
最終分散体は、ビニル末端ポリジメチル−コ−ジフェニル−シロキサン(Gelest社製PDV1625)中の、フェニルトリメトキシシランで官能化してさらにヘキサメチルジシラジン(HMDZ)で末端封鎖した22wt%のコロイダルシリカからなるものであった。コロイダルシリカ及び縮合官能基のwt%は約27%である。最終分散体5.33gを、0.04gの白金触媒パッケージ(最終配合物中の[Pt]=7.5ppm)及び0.14gのポリジメチル−コ−メチルヒドリド−シロキサン(GE Silicones社製88466)と混合した。最終配合物は流動性の材料であった。上記組成物を150℃で1時間硬化させてバルク熱伝導率0.17W/m−Kの材料を得た。
10.06gのビニル末端ポリジメチル−コ−ジフェニル−シロキサン(Gelest社製PDV1625)、0.38gのポリジメチル−コ−メチルヒドリド−シロキサン(GE Silicones社製88466)、1.10gのフェニルトリメトキシシラン及び0.10gの触媒パッケージ(最終配合物中の目標[Pt]=7.5ppm)からなるストック溶液を調製した。このストック溶液2.76gを、0.44gの溶融シリカ(電気化学工業(株)製、平均粒径=5ミクロン)及び0.35gの二重処理ヒュームドシリカ(GE Silicones社製88318)と混合した。この混合物は非流動性の高粘度ペーストであった。
実施例5に記載の適量の最終分散体をシリンジから、8×8mmアルミニウムクーポンの上に手作業でX字形に形成した。その上に第2のアルミニウムクーポンを載置して、得られたサンドイッチ構造体を150℃のオーブンに1時間入れて硬化を完了させた。このTIM層の接合面(ボンドライン)厚さは16.8ミクロンである。TIM層の有効熱伝導率は25℃で0.18W/m−Kである。TIM層を通しての総熱抵抗は94mm2−K/Wであった。
Claims (7)
- オルガノ官能化ナノ粒子と硬化性ポリマーマトリックスとのブレンドを含んでなる熱伝導組成物であって、
前記オルガノ官能化ナノ粒子は、オルガノ官能化コロイダルシリカであり、オルガノ官能化コロイダルシリカはコロイダルシリカを下記式
(R1)aSi(OR2)4−a
(上記式中、R1は各々独立にC1―18一価炭化水素基であり、該一価炭化水素基は、アルキルアクリレート、アルキルメタクリレート、エポキシド、ビニル、アリル、スチレン系、シリル又はシロキシル基でさらに官能化されている。R2は各々独立にC1―18一価炭化水素基又は水素基であり、aは1〜3の整数である。)
で表されるオルガノアルコキシシランで官能化し、さらにシリル化剤で官能化したものであり、前記シリル化剤は、ヘキサメチルジシラザン、テトラメチルジシラザン、ジビニルテトラメチルジシラザン、ジフェニルテトラメチルジシラザン、N−(トリメチルシリル)ジエチルアミン、1−(トリメチルシリル)イミダゾール、トリメチルクロロシラン、ペンタメチルクロロジシロキサン、ペンタメチルジシロキサン及びこれらの組合せから選ばれる少なくとも1つである、熱伝導組成物。 - 前記硬化性ポリマーマトリックスがアクリレート樹脂であり、
前記R1がアルキルアクリレート又はアルキルメタクリレートで官能化されたC1―18一価炭化水素基である請求項1記載の熱伝導組成物。 - さらにミクロン粒度の充填材を含む、請求項1又は請求項2記載の熱伝導組成物。
- 発熱部品(3)を、硬化性ポリマーマトリックスとオルガノ官能化ナノ粒子とのブレンドを含んでなる熱伝導組成物(2)と接触させて配置する段階、及び
ヒートシンク(1)を熱伝導組成物(2)と接触させて配置する段階
を含んでなる、熱伝達性を増大させる方法であって、
前記オルガノ官能化ナノ粒子は、オルガノ官能化コロイダルシリカであり、オルガノ官能化コロイダルシリカはコロイダルシリカを下記式
(R1)aSi(OR2)4−a
(上記式中、R1は各々独立にC1―18一価炭化水素基であり、該一価炭化水素基は、アルキルアクリレート、アルキルメタクリレート、エポキシド、ビニル、アリル、スチレン系、シリル又はシロキシル基でさらに官能化されている。R2は各々独立にC1―18一価炭化水素基又は水素基であり、aは1〜3の整数である。)
で表されるオルガノアルコキシシランで官能化し、さらにシリル化剤で官能化したものであり、前記シリル化剤は、ヘキサメチルジシラザン、テトラメチルジシラザン、ジビニルテトラメチルジシラザン、ジフェニルテトラメチルジシラザン、N−(トリメチルシリル)ジエチルアミン、1−(トリメチルシリル)イミダゾール、トリメチルクロロシラン、ペンタメチルクロロジシロキサン、ペンタメチルジシロキサン及びこれらの組合せから選ばれる少なくとも1つである、方法。 - 発熱部分(3)、
ヒートシンク(1)、及び
発熱部分(3)と前記ヒートシンク(1)との間に介在する熱伝導組成物(2)
を備える電子部品であって、前記熱伝導組成物(2)が硬化性ポリマーマトリックスとオルガノ官能化ナノ粒子とのブレンドを含んでなり、
前記オルガノ官能化ナノ粒子は、オルガノ官能化コロイダルシリカであり、オルガノ官能化コロイダルシリカはコロイダルシリカを下記式
(R1)aSi(OR2)4−a
(上記式中、R1は各々独立にC1―18一価炭化水素基であり、該一価炭化水素基は、アルキルアクリレート、アルキルメタクリレート、エポキシド、ビニル、アリル、スチレン系、シリル又はシロキシル基でさらに官能化されている。R2は各々独立にC1―18一価炭化水素基又は水素基であり、aは1〜3の整数である。)
で表されるオルガノアルコキシシランで官能化し、さらにシリル化剤で官能化したものであり、前記シリル化剤は、ヘキサメチルジシラザン、テトラメチルジシラザン、ジビニルテトラメチルジシラザン、ジフェニルテトラメチルジシラザン、N−(トリメチルシリル)ジエチルアミン、1−(トリメチルシリル)イミダゾール、トリメチルクロロシラン、ペンタメチルクロロジシロキサン、ペンタメチルジシロキサン及びこれらの組合せから選ばれる少なくとも1つである、電子部品。 - 熱伝導組成物(2)が予め形成されたパッドからなる、請求項5記載の電子部品。
- ミクロン粒度の充填剤を充填したポリマー組成物の相分離を遅延させる方法であって、オルガノ官能化ナノ粒子を硬化性ポリマー組成物にブレンドすることを含んでなり、
前記オルガノ官能化ナノ粒子は、オルガノ官能化コロイダルシリカであり、オルガノ官能化コロイダルシリカはコロイダルシリカを下記式
(R1)aSi(OR2)4−a
(上記式中、R1は各々独立にC1―18一価炭化水素基であり、該一価炭化水素基は、アルキルアクリレート、アルキルメタクリレート、エポキシド、ビニル、アリル、スチレン系、シリル又はシロキシル基でさらに官能化されている。R2は各々独立にC1―18一価炭化水素基又は水素基であり、aは1〜3の整数である。)
で表されるオルガノアルコキシシランで官能化し、さらにシリル化剤で官能化したものであり、前記シリル化剤は、ヘキサメチルジシラザン、テトラメチルジシラザン、ジビニルテトラメチルジシラザン、ジフェニルテトラメチルジシラザン、N−(トリメチルシリル)ジエチルアミン、1−(トリメチルシリル)イミダゾール、トリメチルクロロシラン、ペンタメチルクロロジシロキサン、ペンタメチルジシロキサン及びこれらの組合せから選ばれる少なくとも1つである、方法。
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