TWI455878B - 石墨烯的製備方法 - Google Patents

石墨烯的製備方法 Download PDF

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TWI455878B
TWI455878B TW101116707A TW101116707A TWI455878B TW I455878 B TWI455878 B TW I455878B TW 101116707 A TW101116707 A TW 101116707A TW 101116707 A TW101116707 A TW 101116707A TW I455878 B TWI455878 B TW I455878B
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electrode
preparation
graphene
group
solvent
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TW101116707A
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TW201345835A (zh
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Yong Chien Ling
Chih Ping Wang
Jen Yu Liu
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Nat Univ Tsing Hua
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00Electrolytic production of inorganic compounds or non-metals
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/182Graphene
    • C01B32/184Preparation
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/182Graphene
    • C01B32/194After-treatment

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
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  • Condensed Matter Physics & Semiconductors (AREA)
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Claims (17)

  1. 一種石墨烯的製備方法,至少包含下列步驟:將一第一電極與一第二電極不接觸地置於一電解液中,且該第一電極為一石墨複層材料,且該第二電極為石墨電極片、鉑電極片或不鑄鋼電極片,該電解液包含至少一離子溶液;使該第一電極與該第二電極間產生一電勢差;該離子溶液藉由該電勢差進入該第一電極之每一層中以生成複數個石墨烯;其中該電解液更包含一輔助溶液,且該輔助溶液包含一第一溶劑與一第二溶劑。
  2. 如申請專利範圍第1項所述之製備方法,更包含下列步驟:氮化該些石墨烯;其中所述之壓力條件的範圍為1至100atm,溫度條件的範圍為攝氏300至400度,環境氣體包含氮氣、氧氣、氫氣、週期表惰性氣體的至少一種以上或其混合物,以及不同溶劑包含水、甲醇、乙醇或其他可以溶解離子液體但不溶解石墨烯的溶劑。
  3. 如申請專利範圍第2項所述之製備方法,其中該些石墨烯於該氮化步驟後所含之氮原子數目為該些石墨烯總原子數目的0.01%至0.99%。
  4. 如申請專利範圍第2項所述之製備方法,其中在氮化該些石墨烯的步驟之前,更包含下列步驟:將該些石墨烯插置於該些石墨烯間以及覆蓋於該些石墨烯表面之該離子溶液自該電解液中分離出來。
  5. 如申請專利範圍第4項所述之製備方法,其中該將該些石墨烯、插置於該些 石墨烯間以及覆蓋於該些石墨烯表面之該離子溶液自該電解液中分離出來的步驟係透過離心、過濾、管柱層析、溫度差、密度差、超臨界流體萃取、靜置或添加與該電解液不相容之一溶劑來完成。
  6. 如申請專利範圍第1項所述之製備方法,其中該離子溶液包含一陽離子與一陰離子,且該陽離子係可選擇自由銨、咪唑鎓、噁唑鎓、派啶翁、吡嗪翁、吡唑鎓、噠嗪翁、吡啶鎓、嘧啶鎓、吡咯烷鎓、吡咯啉鎓、噻唑鎓、三唑鎓及胍鹽陽離子所構成之群組,該陰離子係可選擇自由鹵素、硫酸根、磺酸根、醯胺、醯亞胺、硼酸根、磷酸根、銻酸根、癸酸根及四羰合鈷陰離子所構成之群組。
  7. 如申請專利範圍第1項所述之製備方法,其中該第一溶劑係可選擇自由溴酸、氨水、苯胺、吡咯、塞吩、乙炔、二甲基亞碸、乙醇、對苯、對苯撐乙烯及其組合所構成之群組,而該第二溶劑可選擇自由酯、醚、酮及其組合所構成之群組。
  8. 如申請專利範圍第1項所述之製備方法,其中該第二溶劑為一碳酸酯,且該碳酸酯可選擇自由碳酸二甲酯、碳酸二乙酯、碳酸二丙酯、碳酸甲丙酯、碳酸乙丙酯、碳酸甲乙酯、碳酸亞乙酯、碳酸亞丙酯、碳酸亞丁酯、碳酸亞戊酯及其組合所構成之群組。
  9. 如申請專利範圍第1項所述之製備方法,其中該第二溶劑可選擇自由乙酸甲酯、乙酸乙酯、乙酸正丙酯、乙酸二甲酯、丙酸甲酯、丙酸乙酯、γ-丁內酯、癸內酯、戊內酯、甲瓦龍酸內酯、己內酯及其組合所構成之群組。
  10. 如申請專利範圍第1項所述之製備方法,其中該第二溶劑係可選擇自由二丁醚、四乙二醇二甲醚、二乙二醇二甲醚、二甲氧基乙烷、2一甲基四氮呋喃、四氫呋喃及其組合所構成之群組。
  11. 如申請專利範圍第1項所述之製備方法,其中該第二溶劑係可選擇自環己酮、聚甲基乙烯基酮及其組合所構成之群組。
  12. 如申請專利範圍第1項所述之製備方法,其中使該第一電極與該第二電極間產生該電勢差之步驟係透過於該第一電極與該第二電極之間施加恒流,且其電流條件的範圍為10毫安培/克至20安培/克,恒流時間為0.5小時至24小時。
  13. 如申請專利範圍第1項所述之製備方法,其中使該第一電極與該第二電極間 產生該電勢差之步驟係透過於該第一電極與該第二電極之間施加恒壓,且其電壓條件的範圍為0.5伏特至20伏特,恒壓時間為0.5小時至24小時。
  14. 如申請專利範圍第1項所述之製備方法,其中使該第一電極與該第二電極間產生該電勢差之步驟係透過於該第一電極與該第二電極之間施加掃描電勢,且其電勢範圍為-0.2伏特至20伏特,掃描時間為0.5小時至24小時或掃描次數為10至10000次。
  15. 如申請專利範圍第1項所述之製備方法,其中該離子溶液的濃度範圍為0.0001%至100%。
  16. 如申請專利範圍第1項所述之製備方法,其中該第一電極與該第二電極具有一間距,該間距為20奈米至20公分。
  17. 如申請專利範圍第1項所述之製備方法,其中該第一電極與該第二電極夾有一角度,該角度為0度至180度。
TW101116707A 2012-05-10 2012-05-10 石墨烯的製備方法 TWI455878B (zh)

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GB2516919B (en) * 2013-08-06 2019-06-26 Univ Manchester Production of graphene and graphane
EP2933356A1 (en) * 2014-04-17 2015-10-21 Basf Se Two-dimensional carbon materials prepared by electrochemical exfoliation
CN105088261B (zh) * 2014-05-14 2017-10-20 国能纳米科技有限公司 石墨烯的制备方法
CN104894594A (zh) * 2015-05-26 2015-09-09 广东烛光新能源科技有限公司 一种石墨烯的制备方法
GB201517784D0 (en) 2015-10-08 2015-11-25 Univ Manchester Production of graphene
CN105609326B (zh) * 2015-12-25 2018-01-30 哈尔滨工业大学 一种聚吡咯/石墨烯/细菌纤维素导电膜材料的制备方法及其应用
CN107845506B (zh) * 2017-10-26 2020-06-30 中国科学院福建物质结构研究所 一种增强型石墨烯基超级电容器及其制备方法
CN108037171B (zh) * 2017-12-26 2020-02-14 南京师范大学 一种水相中高分散的氮掺杂石墨烯量子点的制备方法和应用
DE102017223892A1 (de) * 2017-12-29 2019-07-04 Sixonia Tech Gmbh Verfahren zur Herstellung eines funktionalisierten Halbleiter- oder Leitermaterials und dessen Verwendung
KR102550122B1 (ko) 2018-07-26 2023-07-03 한국전력공사 그래핀 파이버 도핑장치 및 도핑방법
CN114032561A (zh) * 2021-11-05 2022-02-11 安庆师范大学 一种石墨烯和在离子液体中电解乙醇制备石墨烯的方法
CN116376403B (zh) * 2023-04-25 2024-06-04 国网江西省电力有限公司电力科学研究院 一种石墨烯涂料及其制备方法

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