JP6960474B2 - 高熱伝導のポリイミド系複合炭素膜およびその製造方法 - Google Patents
高熱伝導のポリイミド系複合炭素膜およびその製造方法 Download PDFInfo
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- JP6960474B2 JP6960474B2 JP2019565894A JP2019565894A JP6960474B2 JP 6960474 B2 JP6960474 B2 JP 6960474B2 JP 2019565894 A JP2019565894 A JP 2019565894A JP 2019565894 A JP2019565894 A JP 2019565894A JP 6960474 B2 JP6960474 B2 JP 6960474B2
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Description
圧力20MPaを1時間維持し、圧力を0MPaまで徐々に放出し、ホットプレスキャビティを真空度が−100〜10KPaになるまで5分間真空引きするというホットプレスプロセスを1〜5回繰り返し、
次いで、0.1〜5℃/分の速度で300℃まで昇温し、0.5時間保温した後、
圧力60MPaを1時間維持し、圧力を0MPaまで徐々に放出し、ホットプレスキャビティを真空度が−100〜10KPaになるまで5分間真空引きするというホットプレスプロセスを1〜5回繰り返し、
ホットプレスプロセス終了後に自然冷却させるステップと、
(1)平均寸法が50μmを超える酸化グラフェンで濃度4mg/mLの酸化グラフェン水溶液を調製した。
圧力20MPaを1時間維持し、圧力を0MPaまで徐々に放出し、ホットプレスキャビティを真空度が−100KPaになるまで5分間真空引きするというホットプレスプロセスを1回繰り返し、
次いで、0.1℃/分の速度で300℃まで昇温し、0.5時間保温した後、
圧力60MPaを1時間維持し、圧力を0MPaまで徐々に放出し、ホットプレスキャビティを真空度が−100KPaになるまで5分間真空引きするというホットプレスプロセスを1回繰り返し、
ホットプレスプロセス終了後に自然冷却させる。
(1)平均寸法が50μmを超える酸化グラフェンで濃度4mg/mLの酸化グラフェン水溶液を調製した。
(1)平均寸法が50μmを超える酸化グラフェンで濃度1mg/mLの酸化グラフェン水溶液を調製した。
圧力20MPaを1時間維持し、圧力を0MPaまで徐々に放出し、ホットプレスキャビティを真空度が−50KPaになるまで5分間真空引きするというホットプレスプロセスを5回繰り返し、
次いで、2℃/分の速度で300℃まで昇温し、0.5時間保温した後、
圧力60MPaを1時間維持し、圧力を0MPaまで徐々に放出し、ホットプレスキャビティを真空度が−50KPaになるまで5分間真空引きするというホットプレスプロセスを5回繰り返し、
ホットプレスプロセス終了後に自然冷却させた。
(1)平均寸法が50μmを超える酸化グラフェンで濃度10mg/mLの酸化グラフェン水溶液を調製した。
圧力20MPaを1時間維持し、圧力を0MPaまで徐々に放出し、ホットプレスキャビティを真空度が−50KPaになるまで5分間真空引きするというホットプレスプロセスを5回繰り返し、
次いで、2℃/分の速度で300℃まで昇温し、0.5時間保温した後、
圧力60MPaを1時間維持し、圧力を0MPaまで徐々に放出し、ホットプレスキャビティを真空度が−50KPaになるまで5分間真空引きするというホットプレスプロセスを5回繰り返した。
ホットプレスプロセス終了後に自然冷却させた。
(1)平均寸法が50μmを超える酸化グラフェンで濃度4mg/mLの酸化グラフェン水溶液を調製した。
圧力20MPaを1時間維持し、圧力を0MPaまで徐々に放出し、ホットプレスキャビティを真空度が−50KPaになるまで5分間真空引きするというホットプレスプロセスを5回繰り返し、
次いで、2℃/分の速度で300℃まで昇温し、0.5時間保温した後、
圧力60MPaを1時間維持し、圧力を0MPaまで徐々に放出し、ホットプレスキャビティを真空度が−50KPaになるまで5分間真空引きするというホットプレスプロセスを5回繰り返し、
ホットプレスプロセス終了後に自然冷却させた。
(1)平均寸法が50μmを超える酸化グラフェンで濃度4mg/mLの酸化グラフェン水溶液を調製した。
(1)平均寸法が50μmを超える酸化グラフェンで濃度4mg/mLの酸化グラフェン水溶液を調製した。
Claims (6)
- 厚みが100μmを超え、空孔率が10〜40%であり、任意の2つの隣接するグラファイトシート層の間隔が20nm未満であることを特徴とする高熱伝導のポリイミド系複合炭素膜。
- 請求項1に記載された高熱伝導のポリイミド系複合炭素膜の製造方法であって、
(ステップ1)平均寸法が50μmを超える酸化グラフェンで濃度1〜10mg/mLの酸化グラフェン水溶液を調製するステップ1と、
(ステップ2)ポリイミド系炭素膜に対して酸素プラズマ処理を行い、親水性をもたせるステップ2と、
(ステップ3)ステップ2で処理した複数のポリイミド系炭素膜を複合化するステップであって、ステップ1における酸化グラフェン溶液をポリイミド系炭素膜表面に均等に塗布した後、複数のポリイミド系炭素膜を厚み方向に接着するステップ3と、
(ステップ4)接着後のポリイミド系複合炭素膜をオーブンに置いて乾燥させ、オーブンの温度を40℃以下とするステップ4と、
(ステップ5)乾燥させたポリイミド系複合炭素膜をホットプレス機のホットプレスキャビティの中に置き、0.1〜5℃/分の速度で200℃まで昇温した後、
圧力20MPaを1時間維持し、圧力を0MPaまで徐々に放出し、ホットプレスキャビティを真空度が−100〜10KPaになるまで5分間真空引きするというホットプレスプロセスを1〜5回繰り返し、
次いで、0.1〜5℃/分の速度で300℃まで昇温し、0.5時間保温した後、
圧力60MPaを1時間維持し、圧力を0MPaまで徐々に放出し、ホットプレスキャビティを真空度が−100〜10KPaになるまで5分間真空引きするというホットプレスプロセスを1〜5回繰り返し、
ホットプレスプロセス終了後に自然冷却させるステップ5と、
(ステップ6)ステップ5でホットプレスしたポリイミド系複合炭素膜を、不活性ガス雰囲気において1〜20℃/分の速度で2400〜3000℃まで昇温し、さらなるホットプレスを行い、0.5〜8時間保温保圧し、圧力を60MPaとし、冷却プレス後に、高熱伝導のポリイミド系複合炭素膜を得るステップ6とを含む高熱伝導のポリイミド系複合炭素膜の製造方法。 - 前記ステップ1の酸化グラフェンのC/O比が1.8〜2.1であることを特徴とする請求項2に記載の方法。
- グラフェン/ポリイミド複合炭素膜の厚みが100μmを超え、空孔率が10〜40%であり、面方向熱伝導率が1000〜1700W/mKであり、任意の2つの隣接するグラファイトシート層の間隔は20nm未満であることを特徴とする高熱伝導のグラフェン/ポリイミド複合炭素膜。
- (ステップ1)平均寸法が50μmを超える酸化グラフェンで濃度1〜10mg/mLの酸化グラフェン水溶液を調製するステップ1と、
(ステップ2)複数のポリイミド膜を複合化するステップであって、ステップ1における酸化グラフェン溶液をポリイミド膜表面に均等に塗布した後、複数のポリイミド膜を厚み方向に接着するステップ2と、
(ステップ3)接着後の酸化グラフェン/ポリイミド複合膜をオーブンに置いて乾燥させ、オーブンの温度を40℃未満とするステップ3と、
(ステップ5)乾燥させた酸化グラフェン/ポリイミド複合膜をアルゴン雰囲気の炭化炉の中に置き、0.1〜5℃/分の速度で1000℃まで徐々に昇温して熱処理し、100℃ごとに1時間恒温状態とし、プロセス全体で圧力を20MPa〜200MPaに維持するステップ5と、
(ステップ6)ステップ5でホットプレスしたグラフェン/ポリイミド複合炭素膜を、不活性ガス雰囲気において1〜20℃/分の速度で2500〜3000℃まで昇温し、さらなるホットプレスを行い、0.5〜8時間保温保圧し、圧力を60MPaとし、冷却プレス後に、高熱伝導のグラフェン/ポリイミド複合炭素膜を得るステップ6とを含むことを特徴とする高熱伝導のグラフェン/ポリイミド複合炭素膜の製造方法。 - 前記ステップ1の酸化グラフェンのC/O比が1.8〜2.1である請求項5に記載の方法。
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