JP6650412B2 - 熱伝導シート及びその製造方法 - Google Patents
熱伝導シート及びその製造方法 Download PDFInfo
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Description
下記の特許文献3には、配向したグラファイト構造体に金属化合物粒子が分散されている高熱伝導性部材が開示されている。
特許文献3の高熱伝導性部材は、グラファイトの配向性を維持しつつ熱伝導性の粒子を混合することにより高熱伝導性を得るものであるが、やはり厚み方向の熱伝導性が十分ではなかった。
本発明に係る熱伝導シートは、好ましくは、前記配向制御粒子の平均粒径が、0.2μm以上、1000μm以下である。
本発明に係る熱伝導シートは、膨張黒鉛と、配向制御粒子とを含む。上記膨張黒鉛の少なくとも一部は、上記配向制御粒子の存在により、シートの面方向とは異なる方向に配向している。そのため、本発明に係る熱伝導シートは、シートの厚み方向における熱伝導性に優れている。もっとも、膨張黒鉛の全てが、シートの面方向とは異なる方向に配向していない場合、本発明に係る熱伝導シートは、シートの面方向における熱伝導性にも優れている。
膨張黒鉛は、複数のグラフェン層の積層体である。膨張黒鉛は、例えば、天然黒鉛や人造黒鉛などの通常の黒鉛よりも、グラフェン層間が大きい黒鉛である。本明細書においては、少なくとも一部のグラフェン層間が通常の黒鉛より拡げられたものも膨張黒鉛に含まれるものとする。膨張黒鉛の大きさとしては、特に限定されないが、平均粒径で、100μm〜1000μmのものを用いることが好ましい。なお、本明細書において、「平均粒径」とは、レーザ回折/散乱式粒度分布計により測定された値である。
配向制御粒子とは、その存在により、少なくとも一部の膨張黒鉛を、シートの面方向とは異なる方向に配向させることが可能な粒子のことをいう。配向制御粒子は、上記の機能を有する限り、無機化合物であってもよく、有機化合物であってもよい。
本発明に係る熱伝導シートの製造方法は、膨張黒鉛と、配向制御粒子との混合物を用意する工程(工程1)と、上記混合物をシート成形することによって、上記膨張黒鉛の少なくとも一部をシートの面方向とは異なる方向に配向させる工程(工程2)とを備える。
まず、膨張黒鉛と、配向制御粒子とを混合し、混合物を用意する。膨張黒鉛と、配向制御粒子との混合は、乾燥状態で行ってもよいが、超臨界媒体の存在下で行うことが好ましい。超臨界媒体中で混合する場合、膨張黒鉛と、配向制御粒子とをより一層均一に混合することができる。そのため、後述するシート成形において、膨張黒鉛をシートの面方向とは異なる方向により一層配向させることができ、熱伝導シートの厚み方向の放熱性をより一層高めることができる。なお、超臨界媒体としては、例えば、超臨界状体にある水や二酸化炭素(超臨界二酸化炭素)を用いることができる。
次に、得られた混合物をプレスによりシート成形する。このとき、膨張黒鉛へのプレスは、上記配向制御粒子の存在下で行われる。そのため、上記膨張黒鉛の少なくとも一部がシートの面方向とは異なる方向に配向することとなる。
部分剥離型薄片化黒鉛の製造方法においては、まず樹脂が黒鉛もしくは一次薄片化黒鉛に固定されている組成物を用意する。樹脂の黒鉛もしくは薄片化黒鉛への固定は、グラフト又は吸着により行われる。なお、一次薄片化黒鉛とは、黒鉛を剥離することにより得られた薄片化黒鉛を多く含むものである。一次薄片化黒鉛は、黒鉛を剥離することにより得られるものであるため、その比表面積は、黒鉛よりも大きいものであればよい。
本発明では、上記のようにして用意された、固定化された樹脂の一部が残存している部分剥離型薄片化黒鉛と、配向制御粒子とを含む原料組成物を加熱し、それによって部分剥離型薄片化黒鉛内に配向制御粒子を包摂させることができる。
次に、本発明の具体的な実施例及び比較例を挙げることにより本発明を明らかにする。なお、本発明は以下の実施例に限定されるものではない。
膨張黒鉛(鈴裕化学社製、商品名「GREP−EG」、平均粒径100〜2000μm)71.4重量%と、配向制御粒子としてのAl2O3(和光純薬社製、商品名「酸化アルミ」、平均粒径:>75μm)28.6重量%とを、圧力容器に入れ(重量比;膨張黒鉛:配向制御粒子=10:4)、マグネチックスターラーにより、20〜100rpmの速度で撹拌した。しかる後、容器内に超臨界二酸化炭素を供給し、容器内の圧力を27.6MPaとして、50℃で6時間撹拌した。撹拌後、超臨界二酸化炭素を抜き取り、膨張黒鉛とAl2O3の混合物を取り出した。
膨張黒鉛及び配向制御粒子の添加量(重量比)、配向制御粒子の種類又は配向制御粒子の平均粒径をそれぞれ下記の表1に示すように設定したこと以外は実施例1と同様にして、熱伝導シートを得た。
膨張黒鉛(炭鈴裕化学社製、商品名「GREP−EG」、平均粒径100〜2000μm)50重量%と、配向制御粒子としてのAl2O3(和光純薬社製、商品名「酸化アルミ」、平均粒径0.236μm)50重量%とを、圧力容器に入れ(重量比;膨張黒鉛:配向制御粒子=10:10)、マグネチックスターラーにより、20〜100rpmの速度で撹拌した。しかる後、容器内に超臨界二酸化炭素を供給し、容器内の圧力を27.6MPaとして、50℃で6時間撹拌した。撹拌後、超臨界二酸化炭素を抜き取り、膨張黒鉛とAl2O3の混合物を取り出した。
部分剥離型薄片化黒鉛の調製;
膨張黒鉛(東洋炭素社製、商品名「PFパウダー8F」)2.5gと、熱分解性発泡剤として、式(1)に示した構造を有するADCA(永和化成社製、商品名「AC♯R−K」、熱分解温度210℃)5gと、ポリグリシジルメタクリレート(日本油脂社製、品番「G2050M」)50gとを、溶媒としてのテトラヒドラフラン450gと混合し、原料組成物を用意した。原料組成物に、超音波処理装置(本多電子社製)を用い、100W、発振周波数28kHzで5時間超音波を照射した。超音波処理により、ポリグリシジルメタクリレートを膨張黒鉛に吸着させた。このようにして、ポリグリシジルメタクリレートが膨張黒鉛に吸着されている組成物を用意した。
配向制御粒子の種類を下記の表1に示すように設定したこと以外は実施例9と同様にして、熱伝導シートを得た。
実施例9と同様の方法で作製した部分剥離型薄片化黒鉛71.4重量%と、配向制御粒子としてのMgO(和光純薬社製、商品名「酸化マグネシウム」、平均粒径40〜70μm))28.6重量%とを、圧力容器に入れ(重量比;膨張黒鉛:配向制御粒子=10:4)、マグネチックスターラーにより、20〜100rpmの速度で撹拌した。室温で6時間撹拌した後、膨張黒鉛とMgOの混合物を取り出した。その他の点は、実施例1と同様にして、熱伝導シートを得た。
膨張黒鉛(東洋炭素社製、商品名「PFパウダー8F」、平均粒径10〜300μm)100重量%を、シリンダー(大きさ:直径25mm、高さ250mm)内に充填し、10〜20MPaの圧力を加えて、15分間プレスした。しかる後、混合物を500℃で2時間加熱した。加熱後、混合物を再度シリンダー内で、30〜40MPaの圧力を加えて、15分間プレスした。それによって、熱伝導シートを得た。
(SEM写真による断面観察)
熱伝導シートを、ダイヤモンドワイヤーソーにより切り出し、その断面を走査型電子顕微鏡(日立ハイテクノロジーズ社製、型番「S−3400N」)を用いて観察した。また、EDX(日立ハイテクノロジーズ社製、型番「S−3400N」)を用いて、得られた走査型電子顕微鏡写真(SEM写真)の元素マッピング像を得た。
NETZSCH社製、品番「LFA447 ナノフラッシュ」を使用して、1cm角の熱伝導シートの熱伝導率を測定した。
熱伝導測定を行う1cm角の熱伝導シートの厚み(d)cmと重量(W)gを測定した。比重は、W/(1×1×d)により算出した。
Claims (10)
- 熱伝導シートであって、
膨張黒鉛と、配向制御粒子とを含み、
前記膨張黒鉛の少なくとも一部が、前記配向制御粒子の存在により、シートの面方向とは異なる方向に配向しており、
前記膨張黒鉛の前記配向制御粒子に対する重量比(膨張黒鉛/配向制御粒子)が、1/4以上、5以下の範囲にあり、
前記配向制御粒子の平均粒径が、0.2μm以上、1000μm以下である、熱伝導シート。 - 前記膨張黒鉛の少なくとも一部が、前記配向制御粒子の存在により、シートの厚み方向に配向している、請求項1に記載の熱伝導シート。
- 厚み方向の熱伝導率が、5W/m・K以上である、請求項1又は2に記載の熱伝導シート。
- 比重が、1.5g/cm3以上、5g/cm3以下の範囲内にある、請求項1〜3のいずれか1項に記載の熱伝導シート。
- 前記膨張黒鉛が、部分的にグラフェンが剥離している構造を有する部分剥離型薄片化黒鉛である、請求項1〜4のいずれか1項に記載の熱伝導シート。
- 前記部分剥離型薄片化黒鉛内に、前記配向制御粒子が包摂されている、請求項5に記載の熱伝導シート。
- 前記配向制御粒子が、無機化合物である、請求項1〜6のいずれか1項に記載の熱伝導シート。
- 熱伝導シートの製造方法であって、
膨張黒鉛と、配向制御粒子との混合物を用意する工程と、
前記混合物をプレスによりシート成形することによって、前記膨張黒鉛の少なくとも一部をシートの面方向とは異なる方向に配向させる工程とを備える、熱伝導シートの製造方法。 - 前記混合物を用意する工程において、前記膨張黒鉛と、前記配向制御粒子とを、超臨界媒体の存在下で混合する、請求項8に記載の熱伝導シートの製造方法。
- 前記シート成形が、前記混合物をシリンダー内に充填して、プレスすることにより行われる、請求項8又は9に記載の熱伝導シートの製造方法。
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