JP2020521712A - 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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- JP2020521712A JP2020521712A JP2019565894A JP2019565894A JP2020521712A JP 2020521712 A JP2020521712 A JP 2020521712A JP 2019565894 A JP2019565894 A JP 2019565894A JP 2019565894 A JP2019565894 A JP 2019565894A JP 2020521712 A JP2020521712 A JP 2020521712A
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- polyimide
- carbon film
- graphene oxide
- composite carbon
- mpa
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 233
- 229920001721 polyimide Polymers 0.000 title claims abstract description 148
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 134
- 239000004642 Polyimide Substances 0.000 title claims abstract description 130
- 239000002131 composite material Substances 0.000 title claims abstract description 85
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 79
- 238000000034 method Methods 0.000 claims abstract description 31
- 238000007731 hot pressing Methods 0.000 claims abstract description 24
- 239000000243 solution Substances 0.000 claims abstract description 20
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 18
- 239000010439 graphite Substances 0.000 claims description 18
- 238000003763 carbonization Methods 0.000 claims description 13
- 238000013517 stratification Methods 0.000 claims description 12
- 239000012298 atmosphere Substances 0.000 claims description 11
- 239000011261 inert gas Substances 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 238000009832 plasma treatment Methods 0.000 claims description 7
- 239000012300 argon atmosphere Substances 0.000 claims description 4
- 238000013329 compounding Methods 0.000 claims 2
- 238000004026 adhesive bonding Methods 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 6
- 230000001070 adhesive effect Effects 0.000 description 8
- 238000005087 graphitization Methods 0.000 description 8
- 230000008439 repair process Effects 0.000 description 5
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- 238000005299 abrasion Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 125000006615 aromatic heterocyclic group Chemical group 0.000 description 1
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- 230000005484 gravity Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
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- 230000035939 shock Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
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Abstract
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、成層現象がなく、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、
(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と、
(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と、
(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と、
(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と、
(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と、
(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とするステップと、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。
- 製造されるグラフェン/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、成層現象がなく、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。
- (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と、
(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と、
(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と、
(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と、
(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とするステップと、
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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