JP2007182369A - 機能強化窒化ホウ素組成物及びこれで作られた組成物 - Google Patents
機能強化窒化ホウ素組成物及びこれで作られた組成物 Download PDFInfo
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- JP2007182369A JP2007182369A JP2006323729A JP2006323729A JP2007182369A JP 2007182369 A JP2007182369 A JP 2007182369A JP 2006323729 A JP2006323729 A JP 2006323729A JP 2006323729 A JP2006323729 A JP 2006323729A JP 2007182369 A JP2007182369 A JP 2007182369A
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Abstract
【解決手段】表面が、シラン、シロキサン、カルボン酸誘導体、及びその混合物の少なくとも1つを含むコーティング層で処理された窒化ホウ素組成物であって、コーティング層が、窒化ホウ素の表面の少なくとも10%に付着する。窒化ホウ素粉末表面は、最初に、焼成工程により、或いは表面が最終的なコーティング層の少なくとも1つの官能基に反応する少なくとも官能基を含む複数の反応部位を有するように少なくとも無機化合物でコーティングすることにより処理される。
【選択図】 図1
Description
出発材料として、非コーティングBN成分は、当技術分野で公知のプロセスにより作られた結晶性又は部分結晶性窒化ホウ素粒子を含む。これらには、特許文献4に開示されているようなプラズマガスを用いるプロセスで生成されたミクロンサイズの範囲の球状BN粒子、特許文献5に開示されているような結合剤により互いに結合されて、その後スプレー乾燥された不規則な非球状BN粒子で形成された球状窒化ホウ素凝集塊を含むhBN粉末、特許文献6及び特許文献7に開示されているような加圧成形により生成されたBN粉末、特許文献8に開示されているようなBN凝集粉末、特許文献9に開示されているような高拡散係数のBN粉末、及び特許文献10に開示されているような高度デラミネートBN粉末が含まれる。
ることが見出されている。
1つの実施形態では、非コーティングBN粉末粒子は、BN中の酸素濃度を少なくとも100%ほど増大させるのに十分に高温で十分な時間期間焼成される。1つの実施形態では、BN粉末粒子は、酸素濃度が少なくとも1重量%になるのに十分な時間期間焼成される。別の実施形態では、BN粉末粒子は、BN酸素濃度が少なくとも3重量%になるのに十分な温度で十分な時間焼成される。
BN表面上の反応部位を増加させるための第1の段階には種々の実施形態が存在し、乾燥法及び湿潤法が含まれる。乾燥法の1つの実施形態では、BN粒子は、200〜1100°Cの間の温度で焼成される。第2の実施形態では、300〜900°Cの間の温度で焼成される。第3の実施形態では、500〜900°Cの間の温度である。1つの実施形態では、BN粒子は、少なくとも2%の酸素濃度にするのに十分な量の時間及び十分な温度で焼成される。第2の実施形態では、BN粒子は、少なくとも3重量%の酸素濃度にするのに約1〜5時間焼成して、BN粒子の表面層を酸化する。加熱による焼成手段として、酸化環境(例えば空気)が確実に確保される限り、電気炉、ガス炉、回転窯及び連続炉のような種々の手段を用いることができる。
表面機能化BNは、粉末の形態で用いることもでき、IPA、メタノール、エタノール及び同様のものの水性又は非水性媒体内に約60〜80重量%の固体BNをペーストの形態で組み入れることもできる。
1つの実施形態では、本発明の表面機能化BNにより、非処理BNが充填される同じ複合体に比較して、複合体の粘性が殆ど増大しない状態でBNの充填濃度を上昇させることができ、これによって、熱伝導性を向上させて粘性を低下させるか、又は、単に充填ポリマー複合体の粘性を低下させて加工性を向上させる。1つの実施形態では、表面処理BN組成物がポリマー複合体にブレンドされると、ポリマー複合体の粘性は、ジルコネートカップリング剤で処理されていない同量の窒化ホウ素粉末を含むポリマー組成物の粘性に対して少なくとも20%低下する。別の実施形態では、粘性は、特に表面処理BNが(BN充填剤を含むポリマー複合体の総重量に基づき)20重量%を超える量で加えられたときに少なくとも50%低下する。
本明細書では本発明を説明する実施例を示すが、本明細書の範囲を限定するものではない。
実施例では、BN粉末は、オハイオ州クリーブランドに所在のGeneral Electric CompanyのQuartz businessからPTX60(平均粒径が60ミクロンの六方晶系小板BNの球状凝集塊)、PT120(平均粒径が12ミクロンの六方晶系小板BN)、及びPT110(平均粒径が45ミクロンの六方晶系小板BN)として市販されている。出発BN粉末の酸素レベルは、0.4%未満であり、BN表面上の利用可能な反応部位を示す。
表1
表3
実施例4の表面機能化BN粉末試料を室温、35重量%の充填でポリジメチルシリコーン(PDMS)又はシクロヘキシルエポキシ(UVR6105)の何れかと混合する。混合は、FlackTekスピードミキサを用いてほぼ3500rpmで約20秒間行う。充填グリースの粘性測定は、Rheometric Scientific(型番RDA3)を用いて行い、結果は以下の表4の通りである。
表4
粘性測定
実施例1の球状BN充填剤PTX60及びPTX60Sは、1000cPケイ素流体と共に配合され、異なる充填剤の充填量で熱グリースを形成する。図2に示すように、表面修正PTX60Sでの配合は、同様の充填レベルでは非修正PTX60での配合よりも粘性が小さいことが示されている。
表5
表9
Claims (17)
- 窒化ホウ素粉末を含む窒化ホウ素組成物であって、前記窒化ホウ素粉末の表面が、シラン、シロキサン、カルボン酸誘導体、及びその混合物の少なくとも1つを含む少なくともオーバーコーティング層で処理されており、前記オーバーコーティング層が、少なくとも反応性のある1つの官能基を有し、前記オーバーコーティングコーティング層が、前記窒化ホウ素の表面の少なくとも2%に付着することを特徴とする窒化ホウ素組成物。
- 前記窒化ホウ素粉末が、オーバーコーティング層で処理される前に焼成工程で処理され、前記窒化ホウ素粉末が、200から1000°Cの間の温度で酸化環境で0.5〜24時間焼成されることを特徴とする請求項1に記載の窒化ホウ素組成物。
- 前記窒化ホウ素粉末が、オーバーコーティング層で処理される前に少なくとも2%の酸素濃度で焼成されることを特徴とする請求項1〜請求項2の何れかに記載の窒化ホウ素組成物。
- 前記窒化ホウ素粉末は、オーバーコーティング層で処理される前に、前記オーバーコーティング層の少なくとも1つの官能基と反応する少なくとも1つの官能基を含む複数の反応部位を前記窒化ホウ素表面が有するように処理されることを特徴とする請求項1〜請求項3の何れかに記載の窒化ホウ素組成物。
- 前記窒化ホウ素粉末は、オーバーコーティング層で処理される前に、前記最終コーティン層の官能基に反応する少なくとも1つに反応する官能基を含む複数の反応部位を前記表面が有するように、前記窒化ホウ素粉末を少なくとも1つの無機又は有機金属化合物でコーティングすることにより処理されることを特徴とする請求項1〜請求項4の何れかに記載の窒化ホウ素組成物。
- 前記窒化ホウ素粉末が、オーバーコーティング層で処理される前に、耐火金属酸化物及び水酸化物の群から選択される無機化合物の0.5〜約10重量%でコーティングすることにより処理されることを特徴とする請求項1〜請求項5の何れかに記載の窒化ホウ素組成物。
- 前記窒化ホウ素粉末が、オーバーコーティング層で処理される前に、少なくとも有機金属化合物又は金属化合物でコーティングされることにより処理され、前記有機金属又は前記金属化合物をアルミナ、シリカ、ジルコニア、ボリア、チタニア、セリア、ゲルマニア、酸化タンタル、セシア、イットリア、マグネシア、トリア、及びその混合物の少なくとも1つに変換するのに十分な温度まで加熱されることを特徴とする請求項1〜請求項6の何れかに記載の窒化ホウ素組成物。
- 前記窒化ホウ素粉末が、オーバーコーティング層で処理される前に、酢酸ニッケル、硫酸ニッケル、硝酸ニッケル、酢酸銅、硫酸銅、硝酸銅、酢酸亜鉛、硫酸亜鉛、硝酸亜鉛、酢酸ストロンチウム、硫酸ストロンチウム、硝酸ストロンチウム、硫酸アルミニウム、アルミニウムプロポキシド、ケイ酸アルミニウム、アルミン酸ナトリウム、酢酸アルミニウム及びその混合物の少なくとも1つでコーティングすることにより処理されることを特徴とする請求項1〜請求項7の何れかに記載の窒化ホウ素組成物。
- 前記窒化ホウ素粉末が、オーバーコーティング層で処理される前に、20〜100μmの範囲の平均粒径を有するコロイド状シリカを含む組成物でコーティングすることにより処理されることを特徴とする請求項1〜請求項8の何れかに記載の窒化ホウ素組成物。
- 前記窒化ホウ素粉末が、オーバーコーティング層で処理される前に、ソルビタンモノステアレート、ソルビタンモノラウレート、ソルビタンモノオレエート(monoleate)、ソルビタンモノパルミテート(monopalmate)、ポリオキシエチレンソルビタンモノラウレート、ポリオキシエチレンソルビタンモノステアレート、ポリオキシエチレンソルビタンモノオレエート、ポリオキシエチレンソルビタンモノパルミテート(monopalmate)、ポリオキシエチレンソルビタントリステアレート、及びその混合物の少なくとも1つを含む組成物でコーティングすることにより処理されることを特徴とする請求項1〜請求項9の何れかに記載の窒化ホウ素組成物。
- 前記オーバーコーティング層が、ポリパラヒドロキシ安息香酸;ウンデシルオキシ安息香酸;機能化シラン、ジシラン、トリシラン、オリゴマーシラン、ポリマーシラン、及びその組み合わせの群から選択された化合物の1つを含むことを特徴とする請求項1〜請求項10の何れかに記載の窒化ホウ素組成物。
- 前記機能化シランが、アミン、カルボン酸、無水物、リン酸、ピリジニル、ヒドロキシル、エポキシ、チオイソシアネート、ブロックポリチオイソシアネート、アミド、カルバメート、マレイミド、フマレート、オニウム塩、ヒドロキシアルキルアミド、半エステル酸基及び塩、及びその組み合わせから選択される少なくとも1つの官能基を含むことを特徴とする請求項1〜請求項11の何れかに記載の窒化ホウ素組成物。
- 前記窒化ホウ素粉末が、少なくとも10μmの平均粒径の小板を含むことを特徴とする請求項1〜請求項12の何れかに記載の窒化ホウ素組成物。
- 前記窒化ホウ素粉末が、結合剤により互いに結合された後スプレー乾燥された不規則な非球状粒子の球形凝集塊を含むことを特徴とする請求項1〜請求項13の何れかに記載の窒化ホウ素組成物。
- 前記窒化ホウ素粉末が、約50〜約300のアスペクト比の六方晶系窒化ホウ素小板を含むことを特徴とする請求項1〜請求項14の何れかに記載の窒化ホウ素組成物。
- 溶融加工可能ポリマー、ポリエステル、フェノール、シリコーンポリマー、アクリル、ワックス、熱可塑ポリマー、低分子量流体、及びエポキシ成形化合物、並びにその混合物の群から選択されるポリマーマトリクスと、窒化ホウ素の粒子を含む充填剤材料とを含むポリマー複合体であって、前記窒化ホウ素の表面が、シラン、シロキサン、カルボン酸誘導体、及びその混合物の少なくとも1つを含むコーティング化合物で少なくとも処理され、前記コーティング化合物が、前記窒化ホウ素の表面の少なくとも10%に付着することを特徴とするポリマー複合体。
- 窒化ホウ素粉末を生成するための方法であって、
複数の反応部位を前記窒化ホウ素表面の少なくとも一部に導入する段階と、
シラン、シロキサン、カルボン酸誘導体、及びその混合物の少なくとも1つから選択される少なくとも反応性官能基を有する化合物を含むコーティング層で前記窒化ホウ素をコーティングする段階と、
を含み、
前記コーティング層が、前記窒化ホウ素表面の少なくとも10%に付着し、
前記反応部位が、
a)前記窒化ホウ素を200から1000°Cの間の温度の酸化環境で0.5〜24時間焼成する段階、
b)前記窒化ホウ素粉末の酸素濃度が少なくとも2%になるのに十分な温度で十分な時間前記窒化ホウ素を焼成する段階、及び、
c)前記窒化ホウ素粉末を少なくとも無機化合物、有機金属化合物、又は金属化合物でコーティングし、このコーティングホウ素粉末を前記無機化合物、前記有機金属又は前記金属化合物が、アルミナ、シリカ、ジルコニア、ボリア、チタニア、セリア、ゲルマニア、酸化タンタル、セシア、イットリア、マグネシア、トリア、及びその混合物の少なくとも1つに変換するのに十分な温度まで加熱する段階、
の少なくとも1つにより前記窒化ホウ素表面の少なくとも一部に導入されることを特徴とする方法。
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US11/327,709 US20060121068A1 (en) | 1999-08-31 | 2006-01-06 | Boron nitride particles of spherical geometry and process for making thereof |
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US60/777,850 | 2006-03-01 | ||
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EP1806384B1 (en) | 2017-10-25 |
CN101003696B (zh) | 2012-11-07 |
KR101361396B1 (ko) | 2014-02-21 |
JP5086619B2 (ja) | 2012-11-28 |
EP1806384A1 (en) | 2007-07-11 |
US20070054122A1 (en) | 2007-03-08 |
KR20070074457A (ko) | 2007-07-12 |
CN101003696A (zh) | 2007-07-25 |
US7524560B2 (en) | 2009-04-28 |
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