JP2017132672A - 窒化ホウ素構造体、樹脂材料、熱硬化性材料及び積層体 - Google Patents
窒化ホウ素構造体、樹脂材料、熱硬化性材料及び積層体 Download PDFInfo
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- JP2017132672A JP2017132672A JP2016016024A JP2016016024A JP2017132672A JP 2017132672 A JP2017132672 A JP 2017132672A JP 2016016024 A JP2016016024 A JP 2016016024A JP 2016016024 A JP2016016024 A JP 2016016024A JP 2017132672 A JP2017132672 A JP 2017132672A
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- Prior art keywords
- boron nitride
- thermosetting
- resin
- skeleton
- filler
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- 239000000463 material Substances 0.000 title claims abstract description 133
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- 229920005989 resin Polymers 0.000 title claims description 69
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- 229910052582 BN Inorganic materials 0.000 claims abstract description 74
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- 239000000945 filler Substances 0.000 claims description 64
- 239000003795 chemical substances by application Substances 0.000 claims description 36
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- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 230000017525 heat dissipation Effects 0.000 abstract description 29
- 150000008065 acid anhydrides Chemical class 0.000 description 33
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- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical group C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 21
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- 239000011787 zinc oxide Substances 0.000 description 3
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- KFUSXMDYOPXKKT-UHFFFAOYSA-N 2-[(2-methylphenoxy)methyl]oxirane Chemical group CC1=CC=CC=C1OCC1OC1 KFUSXMDYOPXKKT-UHFFFAOYSA-N 0.000 description 2
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 description 2
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical compound C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 description 2
- FVCSARBUZVPSQF-UHFFFAOYSA-N 5-(2,4-dioxooxolan-3-yl)-7-methyl-3a,4,5,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1C(C(OC2=O)=O)C2C(C)=CC1C1C(=O)COC1=O FVCSARBUZVPSQF-UHFFFAOYSA-N 0.000 description 2
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Images
Abstract
Description
(C)窒化ホウ素構造体は、窒化ホウ素材料から構成されるハニカム状多孔質構造を有することが好ましい。ここで、ハニカム状多孔質構造とは、側壁で囲まれた複数の空間(孔)が分布した構造である。ハニカム状多孔質構造とは、側壁で囲まれた複数の空間(孔)が厚み方向に分布した構造であることが好ましい。複数の空間をまたがるように側壁は連続していることが好ましい。例えば、隣り合う3以上の孔の側壁が連続していることが好ましく、隣り合う4以上の孔の側壁が連続していることがより好ましく、隣り合う5以上の孔の側壁が連続していることが更に好ましい。
上記窒化ホウ素材料としては、窒化ホウ素フィラー及び窒化ホウ素ナノチューブ等が挙げられる。(A)樹脂及び(A2)熱硬化性化合物を容易に含浸させることができるので、上記窒化ホウ素材料は、繊維状の窒化ホウ素を含むことが好ましい。なお、窒化ホウ素ナノチューブは、繊維状の窒化ホウ素に相当する。上記窒化ホウ素フィラー及び窒化ホウ素ナノチューブの材質は、窒化ホウ素である。上記窒化ホウ素材料は、窒化ホウ素ナノチューブであることが好ましい。上記窒化ホウ素材料として、窒化ホウ素ナノチューブと、窒化ホウ素フィラーとを組み合わせてもよい。
上記樹脂材料、(A)樹脂及び上記熱硬化性材料は、熱可塑性成分又は熱硬化性成分を含むことが好ましい。上記樹脂材料、(A)樹脂及び上記熱硬化性材料は、(A1)熱可塑性化合物又は(A2)熱硬化性化合物を含むことが好ましい。上記樹脂材料、(A)樹脂及び上記熱硬化性材料は、(A1)熱可塑性化合物を含んでいてもよく、(A2)熱硬化性化合物を含んでいてもよい。(A)樹脂は、(A2)熱硬化性化合物を含むことが好ましい。上記(A)樹脂は、(A2)熱硬化性化合物と(B)熱硬化剤とを含むことが好ましい。
上記樹脂材料は、(A1)熱可塑性化合物を含んでいてもよい。
上記樹脂材料及び上記熱硬化性材料は、(A2)熱硬化性化合物を含んでいてもよい。なお、上記熱硬化性材料が(A2)熱硬化性化合物を含む場合に、(A2)熱硬化性化合物は樹脂でなくてもよい。
(A2−1)熱硬化性化合物としては、環状エーテル基を有する熱硬化性化合物が挙げられる。上記環状エーテル基としては、エポキシ基及びオキセタニル基等が挙げられる。上記環状エーテル基を有する熱硬化性化合物は、エポキシ基又はオキセタニル基を有する熱硬化性化合物であることが好ましい。(A2−1)熱硬化性化合物は、1種のみが用いられてもよく、2種以上が併用されてもよい。
(A2−2)熱硬化性化合物は、分子量が10000以上である熱硬化性化合物である。(A2−2)熱硬化性化合物の分子量は10000以上であるので、(A2−2)熱硬化性化合物は一般にポリマーであり、上記分子量は、一般に重量平均分子量を意味する。
(B)熱硬化剤は特に限定されない。(B)熱硬化剤として、(A2)熱硬化性化合物を硬化させることができる適宜の熱硬化剤を用いることができる。また、本明細書において、(B)熱硬化剤には、硬化触媒が含まれる。(B)熱硬化剤は、1種のみが用いられてもよく、2種以上が併用されてもよい。
(D)フィラーは、窒化ホウ素材料ではなく、(D)フィラーの材質は、窒化ホウ素ではない。
上記樹脂材料及び熱硬化性材料は、上述した成分の他に、分散剤、キレート剤、酸化防止剤等の熱硬化性材料及び熱硬化性シートに一般に用いられる他の成分を含んでいてもよい。
上記樹脂材料は、樹脂シートであってもよい。上記熱硬化性材料は、熱硬化性シートであってもよい。
(窒化ホウ素構造体の作製)
窒化ホウ素ナノチューブの被覆:
平均直径が50nm、平均長さが100μmである窒化ホウ素ナノチューブ(BNNT)を用意した。この窒化ホウ素ナノチューブをステンレス容器に入れて、メタンと酸素を充填した後、300Wの出力でプラズマ処理を5分間行い、表面にカルボキシル基が導入されたBNNTを得た。得られたBNNTを水中に超音波分散させ、両親媒性ポリマーであるアミノ基を有するヒドロキシルポリエチレングリコールを添加した。2時間静置させた後、水洗し、乾燥し、両親媒性ポリマーにより表面が被覆されたBNNTを得た。
上記両親媒性ポリマーにより表面が被覆されたBNNTをクロロホルムに分散させた分散液(BNNT濃度:2mg/ml)を用いて、離型PETシート上に深さが50μmである金型を置き、上記分散液を塗布した。湿度80%の環境下でクロロホルムを蒸発させて、窒化ホウ素構造体を作製した。
マトリックス樹脂の作製:
熱可塑性化合物としてビスフェノールA型フェノキシ樹脂50重量部と、熱硬化性化合物としてビスフェノールA型エポキシ化合物30重量部と、硬化剤として脂環式骨格酸無水物(新日本理化社製「MH−700」)及びジシアンジアミドを合計で15重量部と、添加剤としてエポキシシランカップリング剤5重量部とを配合して、マトリックス樹脂を作製した。
上記マトリックス樹脂を上記窒化ホウ素構造体に含浸させ、厚みが20μmとなるように塗工した。その後、90℃のオーブン内で30分間乾燥することで、厚みが20μmの熱硬化性シート(シート状の熱硬化性材料)を得た。含浸させたマトリックス樹脂の体積量から、得られた熱硬化性シートに占める窒化ホウ素構造体の含有量は25体積%であった。
上記熱硬化性シートを3枚重ねて、厚みが100μmの銅基板で挟み、5MPa、200℃で1時間熱圧着硬化させ、放熱銅基板を得た。
実施例1の両親媒性ポリマーにより表面が被覆されたBNNTを用意した。
熱硬化性シートの作製の際、マトリックス樹脂を窒化ホウ素構造体に含浸させる代わりに、マトリックス樹脂とBNNTを配合比(単位は体積%)が40:60となるように添加し、ホモディスパー型攪拌機で混練して、ペースト(熱硬化性材料)を作製し、離型PETシート上に厚みが60μmとなるように塗工したこと以外は、実施例1と同様にして、熱硬化性シート(シート状の熱硬化性材料)を得た。
熱伝導率の測定:
放熱銅基板の熱伝導率を、京都電子工業社製熱伝導率計「迅速熱伝導率計QTM−500」を用いて測定した。また、比較例1の放熱銅基板の熱伝導率を同様にして測定した。比較例1の熱伝導率を1.0として、その他の実施例の熱伝導率を比較した。各実施例における熱伝導率の比較例1における熱伝導率に対する比(熱伝導率比)を求めた。
11…硬化物部(熱硬化性成分の硬化物部)
12…窒化ホウ素構造体及び硬化物
21…金属体
Claims (9)
- 窒化ホウ素材料から構成されるハニカム状多孔質構造を有する、窒化ホウ素構造体。
- 前記窒化ホウ素材料が、繊維状の窒化ホウ素を含む、請求項1に記載の窒化ホウ素構造体。
- 窒化ホウ素材料ではないフィラーを含む、請求項1又は2に記載の窒化ホウ素構造体。
- 前記窒化ホウ素材料ではないフィラーが、2nm以上、200nm以下の平均粒子径を有する、請求項3に記載の窒化ホウ素構造体。
- 樹脂と、
請求項1〜4のいずれか1項に記載の窒化ホウ素構造体とを有する、樹脂材料。 - 熱硬化性化合物と、
熱硬化剤と、
請求項1〜4のいずれか1項に記載の窒化ホウ素構造体とを有する、熱硬化性材料。 - 熱硬化性材料100体積%中、前記窒化ホウ素構造体の含有量が、20体積%以上、80体積%以下である、請求項6に記載の熱硬化性材料。
- 熱硬化性シートである、請求項6又は7に記載の熱硬化性材料。
- 金属体と、
請求項6〜8のいずれか1項に記載の熱硬化性材料の硬化物とを備える、積層体。
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