JP6759322B2 - 黒鉛シートおよびその製造方法 - Google Patents
黒鉛シートおよびその製造方法 Download PDFInfo
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- JP6759322B2 JP6759322B2 JP2018239926A JP2018239926A JP6759322B2 JP 6759322 B2 JP6759322 B2 JP 6759322B2 JP 2018239926 A JP2018239926 A JP 2018239926A JP 2018239926 A JP2018239926 A JP 2018239926A JP 6759322 B2 JP6759322 B2 JP 6759322B2
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- graphite
- graphite sheet
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- coating
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Description
本願発明の目的は、垂直方向の熱拡散率を減少させ、水平方向の熱拡散率を増加させることにより、水平/垂直方向の熱拡散率の比率が高い黒鉛シート、およびその製造方法を提供することである。
本願発明は、300以上の水平/垂直方向の熱拡散率の比率を有する黒鉛シートを提供する。
本願発明の黒鉛シートは、垂直方向の熱拡散率が低く、水平方向の熱拡散率が高いために、水平/垂直方向の熱拡散率の比が高く、同時に、良好な耐屈曲性を有する。
[例]
例1
(1)基体の準備
セルロース系繊維で構成された基体として、平織の綿布(100su、150mm×100mm、中国製)が準備された。
液相ポリアミド酸(製造者:KOLON PI、商品名:PAA Varnish、重量平均分子量:250,000)を、基体の両面上に25℃での圧延プロセスにより175μmの厚さで被覆した。同一の被覆溶液を、第1の被覆層上に第2の被覆として150μmの厚さで被覆し、それにより基体フィルムを生産した。
ステップ(2)において調製された基体フィルムを、窒素雰囲気中に(約100Torrの圧力で)置き、温度を1℃/分の比率で上昇させた。基体フィルムを、約400℃で約10時間加熱し、厚さ140〜160μmのイミド化基体フィルムを生産した。
ステップ(3)において調製されたイミド化基体フィルムを、窒素ガスまたは不活性ガス雰囲気中に(約100Torrの圧力で)置き、温度を1℃/分の比率で上昇させた。イミド化基体フィルムを、その炭化のために約1,000℃で約3時間加熱した。それから、温度を5℃/分の比率で上昇させ、炭化基体フィルムを、その黒鉛化のために約2,600℃で約1時間加熱した。後処理として、黒鉛化基体シートを、圧延プレスを用いて10トンの負荷の下でプレスし、約40μmの厚さの黒鉛シートを生産した。
約40μmの厚さの黒鉛シートが、綿布の代わりにレーヨン布が用いられたことを除いて、例1に記載したと同様の方法により製造された。
約40μmの厚さの黒鉛シートが、基体フィルムとしてポリイミドフィルム(厚さ約75μm、製造者:KOLON PI、商品名:PIフィルム75μm)が、例1の基体フィルムとして用いられたことを除いて、例1に記載されたと同様の炭化、黒鉛化、および後処理により製造された。
<熱拡散率の測定>
例および比較例において製造された黒鉛シートの水平および垂直方向における熱拡散率を、熱拡散率測定装置(Netsch Co.製、 “LFA447 Nanoflash”)を用いて、光交流法により測定した。特に、黒鉛シートは、それぞれφ25.4mmおよびφ12.6mmのサイズに切断され、水平および垂直方向の熱拡散率は25℃で5回以上測定され、その平均値が算出された。
<耐屈曲性の測定>
例および比較例において製造された黒鉛シートの耐屈曲性は、MIT耐屈曲性試験により評価された。MIT耐屈曲性試験においては、20mmの幅を有する正方形の試験片が、5mmの曲率半径(R)、180度の折り曲げ角、0.98Nの荷重、および90回/分の折り曲げ速度の条件下で、破壊まで繰り返し折り曲げられる。耐屈曲性は、MIT耐屈曲性試験における破壊までの往復動の数により評価された。
以下に、本願の出願当初の特許請求の範囲に記載された発明を付記する。
[1] 300以上の水平/垂直方向の熱拡散率の比率を有する黒鉛シート。
[2] 水平/垂直方向の熱拡散率の比率が500以上である[1]に記載の黒鉛シート。
[3] 黒鉛シートの破壊までの往復折り曲げ回数が、5mmの曲率半径(R)、180度の折り曲げ角、0.98Nの荷重、90回/分の折り曲げ速度の条件下でのMIT試験により試験したときに10,000以上である、[1]に記載の黒鉛シート。
[4] 2.0mm 2 /s以下の垂直方向の熱拡散率を有する黒鉛シート。
[5] 垂直方向の熱拡散率が1.0mm 2 /s以下である、[4]に記載の黒鉛シート。
[6] 黒鉛シートの製造方法であって、以下を含む方法:
(1)天然繊維、合成繊維、または紙を含む基体を提供すること;
(2)前記基体の一面または両面に、ポリマー、炭化ポリマー、および黒鉛からなる群から選択される少なくとも1種を含む被覆溶液で第1の被覆を行うこと;および
(3)前記の被覆された基体を、その熱処理により黒鉛化すること。
[7] さらに前記第1の被覆の後に、前記第1の被覆層の上に前記被覆溶液で第2の被覆を行うことを含む、[6]に記載の黒鉛シートの製造方法。
[8] さらに前記第1の被覆の後に、前記の被覆された基体を圧延することを含む、[6]に記載の黒鉛シートの製造方法。
[9] 前記被覆溶液がポリアミド酸を含み、前記方法はさらに前記第1の被覆の後に、前記の被覆された基体をイミド化することを含む、[6]に記載の黒鉛シートの製造方法。
[10] 前記基体は、綿、麻、羊毛、および絹からなる群から選択される少なくとも1種の天然繊維で構成されている、[6]に記載の黒鉛シートの製造方法。
[11] 前記基体は、レーヨン、アセテート、およびトリアセテートからなる群から選択される少なくとも1種のセルロース系繊維で構成されている、[6]に記載の黒鉛シートの製造方法。
[12] 前記基体は、ナイロン、ポリエステル、ポリウレタン、ポリエチレン、ポリ塩化ビニル、ポリフルオロエチレン、ポリビニルアルコール、アクリル、およびポリプロピレンからなる群から選択される少なくとも1種の合成繊維で構成されている、[6]に記載の黒鉛シートの製造方法。
[13] 黒鉛繊維を含む内層と、前記内層の片面または両面を覆う黒鉛外層とを備える黒鉛シート。
[14] 前記内層は、複数の黒鉛繊維を含む繊維束で構成される、[13]に記載の黒鉛シート。
[15] 前記繊維束は、複数の黒鉛繊維間に形成された空隙を含む、[14]に記載の黒鉛シート。
[16] 前記黒鉛外層は、前記内層の片面を覆う第1の黒鉛外層と、前記黒鉛内層の他の面を覆う第2の黒鉛外層を備え、前記第1の黒鉛外層および前記第2の黒鉛外層は互いに部分的に接続されている、[13]に記載の黒鉛シート。
[17] 前記内層は、黒鉛繊維または黒鉛繊維束で構成される横糸および縦糸が織られた布を備えている、[13]に記載の黒鉛シート。
104:黒鉛内層(基体層黒鉛)
114:黒鉛繊維を含む繊維束
116:走査型電子顕微鏡(SEM)画像を得るために用いられる成型材
Claims (2)
- 300以上の水平/垂直方向の熱拡散率の比率を有する黒鉛シートであって、
黒鉛シートの破壊までの往復折り曲げ回数が、5mmの曲率半径(R)、180度の折り曲げ角、0.98Nの荷重、90回/分の折り曲げ速度の条件下でのMIT試験により試験したときに10,000以上であり、垂直方向の熱拡散率が1.0mm 2 /s以下である、黒鉛シート。 - 水平/垂直方向の熱拡散率の比率が500以上である請求項1に記載の黒鉛シート。
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