JP5169292B2 - 熱伝導性感圧接着剤組成物、及び、熱伝導性感圧接着性シート - Google Patents
熱伝導性感圧接着剤組成物、及び、熱伝導性感圧接着性シート Download PDFInfo
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- JP5169292B2 JP5169292B2 JP2008039336A JP2008039336A JP5169292B2 JP 5169292 B2 JP5169292 B2 JP 5169292B2 JP 2008039336 A JP2008039336 A JP 2008039336A JP 2008039336 A JP2008039336 A JP 2008039336A JP 5169292 B2 JP5169292 B2 JP 5169292B2
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- sensitive adhesive
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Description
本発明において、膨張化黒鉛粉の平均粒径及び粒径分布とは、レーザー式粒度測定機(株式会社セイシン企業製)を用い、マイクロソーティング制御方式(測定領域内にのみ測定対象粒子を通過させ、測定の信頼性を向上させる方式)により測定したものを意味する。この測定方法によると、セル中に測定対象の膨張化黒鉛粉0.01〜0.02gが流されることで、測定領域内に流れてくる膨張化黒鉛粉に波長670nmの半導体レーザー光が照射され、その際のレーザー光の散乱と回折が測定機にて測定されることにより、フランホーファの回折原理から、平均粒径及び粒径分布が計算され、その結果が表示される。
重合体(S)を構成するものとしては、ゴム、エラストマー、及び、樹脂の中から任意に選んだ少なくとも一種を挙げることができる。重合体(S)に、接着性及び/又は粘着性を備えさせるためには、ゴム、エラストマー、及び、樹脂は、接着性及び/又は粘着性を有するものの中から選ぶことが好ましい。しかしながら、接着性及び/又は粘着性を有しないゴム、エラストマー、及び、樹脂に、粘接着性付与剤を組み合わせ用いることもできる。
重合体(S)を構成するものとしては、(メタ)アクリル酸エステル重合体(A1)が好ましい。
本発明の熱伝導性感圧接着剤組成物(F)は、(メタ)アクリル酸エステル重合体(A1)に加えて、さらに、(メタ)アクリル酸エステル単量体(A2m)を含有することがより好ましい。本発明の熱伝導性感圧接着剤組成物(F)を成形して、熱伝導性感圧接着性シート(G)とする際に、熱伝導性感圧接着剤組成物(F)中の(メタ)アクリル酸エステル単量体(A2m)は、重合して(メタ)アクリル酸エステル重合体に変換する。
本発明の熱伝導性感圧接着剤組成物(F)には、膨張化黒鉛粉(E)が含有される。本発明に用いることができる膨張化黒鉛粉の例としては、酸処理した黒鉛を500℃〜1200℃にて熱処理して100ml/g〜300ml/gに膨張させ、次いで、粉砕することを含む工程を経て得られたものを挙げることができる。より好ましくは、黒鉛を強酸で処理した後アルカリ中で焼結し、その後再度強酸で処理したものを500℃〜1200℃にて熱処理して、酸を除去すると共に100ml/g〜300ml/gに膨張させ、次いで、粉砕することを含む工程を経て得られたものを挙げることができる。上記熱処理の温度は、特に好ましくは800℃〜1000℃である。
本発明の熱伝導性感圧接着剤組成物(F)には、難燃性熱伝導無機化合物(B)が含有されることが好ましい。本発明に用いることができる難燃性熱伝導無機化合物(B)は特に限定されることはなく、その具体例としては、水酸化アルミニウム、水酸化マグネシウム、水酸化カルシウム、2水和石膏、ホウ酸亜鉛、カオリンクレー、アルミン酸カルシウム、炭酸カルシウム、炭酸アルミニウム、ドーソナイトなどが挙げられる。難燃性熱伝導無機化合物(B)は、一種を単独で使用してもよく、二種以上を併用してもよい。
熱伝導性感圧接着性シート(G)を成形する際に、熱伝導性感圧接着剤組成物(F)中の(メタ)アクリル酸エステル単量体(A2m)は重合する。その重合を促進するため、熱伝導性感圧接着剤組成物(F)は、(メタ)アクリル酸エステル重合体(Al)、及び、(メタ)アクリル酸エステル単量体(A2m)に加えて、さらに、重合開始剤(C2)を含有することが好ましい。
本発明の熱伝導性感圧接着剤組成物(F)には、それから得られる熱伝導性感圧接着性シート(G)を発泡させるために、発泡剤を添加することもできる。発泡剤としては、熱分解性有機発泡剤(D)が好ましい。さらに、熱分解性有機発泡剤(D)としては、80℃以上かつ200℃以下の分解開始温度を有するものが好ましい。
本発明の熱伝導性感圧接着剤組成物(F)には、感圧接着剤としての凝集力を高め、耐熱性などを向上させるために、外部架橋剤を添加して、(メタ)アクリル酸エステル重合体(A1)の存在下に(メタ)アクリル酸エステル単量体(A2m)を重合してなる重合体に架橋構造を導入することができる。
本発明の熱伝導性感圧接着剤組成物(F)には、さらに、必要により、顔料、その他の充填材、難燃剤、老化防止剤、増粘剤、などの公知の各種添加剤を、本発明の効果を損なわない範囲で含有することができる。
本発明の熱伝導性感圧接着性シート(G)は、熱伝導性感圧接着剤組成物(F)をシート状に成形してなる。
レーザー式粒度測定機(セイシン企業(株)社製)を用い、マイクロソーティング制御方式(測定領域内にのみ測定対象粒子を通過させ、測定の信頼性を向上させる方式)により測定する。セル中に測定対象の膨張化黒鉛粉0.01〜0.02gが流されることで、測定領域内に流れてくる膨張化黒鉛粉に波長670nmの半導体レーザー光が照射され、その際のレーザー光の散乱と回折が測定機にて測定されることにより、フランホーファの回折原理から、平均粒径及び粒径分布が計算され、その結果が表示される。
熱伝導性感圧接着剤組成物を容器に入れ、その容器を水平面に対して30度傾けた。その状態で3分間放置し、熱伝導性感圧接着剤組成物が移動した距離を測定した。
熱伝導性感圧接着性シートを幅50mm×長さ110mm×厚さ1mmの大きさに裁断し、23℃の恒温室に48時間以上静置して、状態調整を行ったものを試料とした。熱伝導率(単位:W/m・K)測定は、迅速熱伝導率計(QTM―500:京都電子工業社製)を用いて、非定常熱線比較法により行った。なお、熱伝導率既知の比較用標準板として、シリコンスポンジ(0.1W/m・K)、シリコーンゴム(0.2W/m・K)、石英(1.4W/m・K)、ジルコニア(3.4W/m・K)、ムライト(5.7W/m・K)を用いた。
<熱伝導性感圧接着剤組成物作成>
反応器に、アクリル酸2−エチルヘキシル94%とアクリル酸6%とからなる単量体混合物100部、2,2'−アゾビスイソブチロニトリル0.03部及び酢酸エチル700部を入れて均一に溶解し、窒素置換後、80℃で6時間重合反応を行った。重合転化率は97%であった。得られた重合体を減圧乾燥して酢酸エチルを蒸発させ、粘性のある固体状の(メタ)アクリル酸エステル重合体(A1)(1)を得た。(メタ)アクリル酸エステル重合体(A1)(1)の重量平均分子量(Mw)は270,000、重量平均分子量(Mw)/数平均分子量(Mn)は3.1であった。重量平均分子量(Mw)及び数平均分子量(Mn)は、テトラヒドロフランを溶離液とするゲルパーミエーションクロマトグラフィーにより、標準ポリスチレン換算で求めた。
熱伝導性感圧接着性シート作成方法を、図1を用いて説明する。図1は、熱伝導性感圧接着性シート作成工程の一部を概略的に示す図である。図1(a)は、熱伝導性感圧接着性シートの作成に用いる各部材を上から見た図である。図1(b)〜(d)は、図1(a)中に示した破線で示した箇所での断面を示す図である。
膨張化黒鉛粉(E)の内訳を変更した以外は実施例1と同様にして、実施例2及び実施例3にかかる熱伝導性感圧接着性シートを得た。具体的には、実施例2では、EC−50を9部、及び、EC−100を36部用いた。実施例3では、EC−50を9部、及び、EC−500(平均粒径30μm、伊藤黒鉛工業株式会社製)を36部用いた。
膨張化黒鉛粉(E)にかえて球状黒鉛(平均粒径30μm、伊藤黒鉛工業株式会社製)45部を用いた以外は実施例1と同様にして、比較例1にかかる熱伝導性感圧接着性シートを得た。
膨張化黒鉛粉(E)にかえて人造黒鉛(平均粒径0.5mm、伊藤黒鉛工業株式会社製)45部を用いた以外は実施例1と同様にして、比較例2にかかる熱伝導性感圧接着性シートを得た。
膨張化黒鉛粉(E)の内訳を変更した以外は実施例1と同様にして、比較例3及び比較例4にかかる熱伝導性感圧接着性シートを得た。具体的には、比較例3では、EC−50を45部用いた。比較例4では、EC−500を45部用いた。
上記で作製した熱伝導性感圧接着剤組成物、及び、熱伝導性感圧接着性シートを評価した。結果を表2に示す。
2 厚み調整用の枠
3 ポリエチレンテレフタレート製のフィルム
4 熱伝導性感圧接着剤組成物
5 ポリエチレンテレフタレート製のフィルム
Claims (12)
- ゴム、エラストマー、及び、樹脂よりなる群から選ばれる少なくとも一種の重合体(S)と、粒径分布に複数のピークを有する膨張化黒鉛粉(E)と、を含有し、
前記膨張化黒鉛粉(E)の粒径分布の複数のピークのうち、少なくとも1つは150μm以上500μm以下にあり、かつ、少なくとも1つは1μm以上150μm未満にあり、
前記膨張化黒鉛粉(E)の粒径分布の複数のピークのうち、1つのピークと他のピークとの間が50μm以上であることを特徴とする、熱伝導性感圧接着剤組成物(F)。 - 前記膨張化黒鉛粉(E)が、平均粒径が異なる、複数の膨張化黒鉛粉を混合したものであることを特徴とする、請求項1に記載の熱伝導性感圧接着剤組成物(F)。
- 前記複数の膨張化黒鉛粉のうち最も平均粒径が大きい膨張化黒鉛粉の含有率が、前記膨張化黒鉛粉(E)全体量に対して、5質量%以上30質量%以下であることを特徴とする、
請求項2に記載の熱伝導性感圧接着剤組成物(F)。 - さらに、難燃性熱伝導無機化合物(B)を含むことを特徴とする、請求項1〜3のいずれか一項に記載の熱伝導性感圧接着剤組成物(F)。
- 前記難燃性熱伝導無機化合物(B)が水酸化アルミニウムであることを特徴とする、請求項4に記載の熱伝導性感圧接着剤組成物(F)。
- 前記重合体(S)が(メタ)アクリル酸エステル重合体(A1)であることを特徴とする、請求項1〜5のいずれか一項に記載の熱伝導性感圧接着剤組成物(F)。
- 前記(メタ)アクリル酸エステル重合体(A1)が有機酸基をもつことを特徴とする、請求項6に記載の熱伝導性感圧接着剤組成物(F)。
- さらに、(メタ)アクリル酸エステル単量体(A2m)を含有することを特徴とする、請求項6又は7に記載の熱伝導性感圧接着剤組成物(F)。
- 前記(メタ)アクリル酸エステル重合体(A1)100質量部に対して、前記膨張化黒鉛粉(E)の含有量が10質量部以上100質量部以下であることを特徴とする、請求項6〜8のいずれか一項に記載の熱伝導性感圧接着剤組成物(F)。
- 難燃性熱伝導無機化合物(B)を50質量部以上350質量部以下含有することを特徴とする、請求項9に記載の熱伝導性感圧接着剤組成物(F)。
- シート状に成形された、請求項1〜10のいずれか一項に記載の熱伝導性感圧接着剤組成物(F)である熱伝導性感圧接着性シート(G)。
- 請求項8〜10のいずれか一項に記載の熱伝導性感圧接着剤組成物(F)をシート状に成形しながら、またはシート状に成形した後、該熱伝導性感圧接着剤組成物(F)中の(メタ)アクリル酸エステル重合体(A1)の存在下に該熱伝導性感圧接着剤組成物(F)中の(メタ)アクリル酸エステル単量体(A2m)を重合することにより得られる、該熱伝導性感圧接着剤組成物(F)の固化物(F’)のシート状成形体である、熱伝導性感圧接着性シート(G)。
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