JP2019189520A - グラフェン材料の製作方法 - Google Patents
グラフェン材料の製作方法 Download PDFInfo
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- JP2019189520A JP2019189520A JP2019080833A JP2019080833A JP2019189520A JP 2019189520 A JP2019189520 A JP 2019189520A JP 2019080833 A JP2019080833 A JP 2019080833A JP 2019080833 A JP2019080833 A JP 2019080833A JP 2019189520 A JP2019189520 A JP 2019189520A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 86
- 239000000463 material Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title abstract 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 37
- 230000003647 oxidation Effects 0.000 claims abstract description 27
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 27
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000007800 oxidant agent Substances 0.000 claims abstract description 11
- 239000001301 oxygen Substances 0.000 claims abstract description 11
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 11
- 230000001590 oxidative effect Effects 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000008367 deionised water Substances 0.000 claims description 21
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- 238000004519 manufacturing process Methods 0.000 claims description 19
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 12
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 12
- 239000003638 chemical reducing agent Substances 0.000 claims description 11
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 230000009467 reduction Effects 0.000 claims description 8
- 239000002244 precipitate Substances 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- 235000010344 sodium nitrate Nutrition 0.000 claims description 6
- 239000004317 sodium nitrate Substances 0.000 claims description 6
- 238000012423 maintenance Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 3
- 235000010323 ascorbic acid Nutrition 0.000 claims description 3
- 239000011668 ascorbic acid Substances 0.000 claims description 3
- 229960005070 ascorbic acid Drugs 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims description 2
- 229930003268 Vitamin C Natural products 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 claims description 2
- 239000012286 potassium permanganate Substances 0.000 claims description 2
- 235000019154 vitamin C Nutrition 0.000 claims description 2
- 239000011718 vitamin C Substances 0.000 claims description 2
- 239000007770 graphite material Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 11
- 230000008569 process Effects 0.000 abstract description 9
- 238000000926 separation method Methods 0.000 abstract description 5
- 238000011946 reduction process Methods 0.000 abstract 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 abstract 1
- 238000006722 reduction reaction Methods 0.000 description 9
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- 238000007792 addition Methods 0.000 description 3
- 125000000524 functional group Chemical group 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000001033 ether group Chemical group 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/198—Graphene oxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
- C01B32/192—Preparation by exfoliation starting from graphitic oxides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
Description
Claims (9)
- 氷浴で、反応容器に10〜40%(wt%)の硫酸、硝酸ナトリウム及びグラフェンを加え、第1撹拌時間で撹拌してから、第1酸化剤として過マンガン酸カリウムを加え、第2撹拌時間で撹拌すると共に、グラフェン、硫酸及び硝酸ナトリウムの相対重量比率が1:1.5〜0.5:1〜6であり、硫酸体積:グラフェン重量が15〜60ml:1gである第1酸化工程と、
前記反応容器を密封した後、第1加熱温度まで加熱し、第3撹拌時間で撹拌する第1加熱工程と、
脱イオン水を加え、前記反応容器を密封した後、第2加熱温度まで加熱し、第4撹拌時間で撹拌してから、初期グラフェン酸化物を得る第2加熱工程と、
前記初期グラフェン酸化物に脱イオン水を加え、第5撹拌時間で撹拌してから、第2酸化剤として過酸化水素溶液を加え、過酸化水素溶液体積:グラフェン重量が1〜20ml:1gであると共に、第6撹拌時間で撹拌する第2酸化工程と、
脱イオン水、塩化水素酸溶液を加え、遠心分離機により分離させ、pHが7±1である上澄み液を除去し、沈澱物を得る分離工程と、
前記沈澱物にエタノール溶液を加え、−20℃〜80℃の乾燥温度で、加熱乾燥又は凍結乾燥処理を4時間〜2日行うことで、グラフェン酸化物を得る乾燥工程と、
前記グラフェン酸化物に脱イオン水を加え、超音波振動機により超音波振動を行う第1超音波振動工程と、
還元剤を加え、25%(wt%)のアンモニア水を徐々に加えることで、pHを9〜10に保つと共に、前記還元剤重量:前記グラフェン酸化物重量の比率が0.5〜5.0:0.5である還元工程と、
脱イオン水を加え、前記超音波振動機又は別体の超音波振動機により超音波振動を行う第2超音波振動工程と、
第3加熱温度まで加熱し、第7撹拌時間で撹拌する加熱工程と、
吸引濾過処理及び乾燥処理を行い、還元グラフェン材料を得る濾過工程とを備え、
前記グラフェン酸化物における炭元素:酸素元素の含有量比率が1.14〜2.81であり、前記還元グラフェン材料の抵抗率が1.45〜150Ω/cmである、
グラフェン材料の製作方法。 - 前記第1酸化工程が20℃以下の温度で行い、前記第1撹拌時間が1〜5時間であり、前記第2撹拌時間が10分〜3時間である、請求項1に記載のグラフェン材料の製作方法。
- 前記第1加熱温度が30〜40℃であり、前記第3撹拌時間が10分〜1時間である、請求項1に記載のグラフェン材料の製作方法。
- 前記第2加熱工程で加えられた前記脱イオン水体積:前記第1酸化工程で加えられた前記グラファイト材料重量の比率が30〜98ml:1gであり、前記第2加熱温度が80〜99℃であり、前記第4加熱時間が10分〜1時間である、請求項1に記載のグラフェン材料の製作方法。
- 前記第2酸化工程で加えられた前記脱イオン水体積:前記第1酸化工程で加えられた前記グラフェン重量の比率が65〜350ml:1gであり、前記第5撹拌時間が30分〜2時間であり、前記第6撹拌時間が1〜3時間である、請求項1に記載のグラフェン材料の製作方法。
- 前記エタノール溶液が10〜70%(wt%)のエタノール溶液である、請求項1に記載のグラフェン材料の製作方法。
- 前記還元剤がビタミンC又はアスコルビン酸である、請求項1に記載のグラフェン材料の製作方法。
- 前記第1超音波振動工程で加えられた前記脱イオン水体積:前記第2酸化工程での前記グラフェン酸化物重量の比率が500〜1500ml:0.5gであり、前記第1超音波振動工程の維持時間が30分〜2時間であり、前記第2超音波振動工程の維持時間が10〜40分である、請求項1に記載のグラフェン材料の製作方法。
- 前記第3加熱温度が80〜98℃であり、前記第7撹拌時間が1〜3時間である、請求項1に記載のグラフェン材料の製作方法。
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US15/960,305 US10287168B1 (en) | 2018-04-23 | 2018-04-23 | Method of manufacturing graphene material |
US15/960,305 | 2018-04-23 |
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EP (1) | EP3567609B1 (ja) |
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Citations (4)
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US20150284253A1 (en) * | 2014-04-03 | 2015-10-08 | Aruna Zhamu | Process for producing highly conducting graphitic films from graphene liquid crystals |
JP2016102034A (ja) * | 2014-11-27 | 2016-06-02 | 旭化成株式会社 | 導電性グラファイトの製造方法及び導電性グラファイト |
CN107158444A (zh) * | 2017-05-05 | 2017-09-15 | 苏州大学 | 一种抗菌增生复合膜及其制备方法 |
WO2017217266A1 (ja) * | 2016-06-14 | 2017-12-21 | コニカミノルタ株式会社 | グラフェン積層体とその製造方法 |
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JP6077347B2 (ja) * | 2012-04-10 | 2017-02-08 | 株式会社半導体エネルギー研究所 | 非水系二次電池用正極の製造方法 |
KR101648139B1 (ko) * | 2013-08-21 | 2016-08-12 | 한화케미칼 주식회사 | 그래핀, 그래핀의 제조 방법, 및 제조 장치 |
EP2960205A1 (en) * | 2014-06-23 | 2015-12-30 | Solvay SA | Stable aqueous graphene suspension and its use in producing graphene polymer nanocomposites |
CN104891482A (zh) * | 2015-06-03 | 2015-09-09 | 盐城纳新天地新材料科技有限公司 | 一种碱性水相下制备氧化石墨烯的方法 |
CN104998266B (zh) * | 2015-06-30 | 2018-06-19 | 浙江师范大学 | 磁性氧化石墨烯复合物的制备和应用 |
US11097951B2 (en) * | 2016-06-24 | 2021-08-24 | The Regents Of The University Of California | Production of carbon-based oxide and reduced carbon-based oxide on a large scale |
TW201811669A (zh) * | 2016-09-20 | 2018-04-01 | 國立臺灣科技大學 | 氧化石墨烯之製造方法及抗菌生物活性玻璃之製造方法 |
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US20150284253A1 (en) * | 2014-04-03 | 2015-10-08 | Aruna Zhamu | Process for producing highly conducting graphitic films from graphene liquid crystals |
JP2016102034A (ja) * | 2014-11-27 | 2016-06-02 | 旭化成株式会社 | 導電性グラファイトの製造方法及び導電性グラファイト |
WO2017217266A1 (ja) * | 2016-06-14 | 2017-12-21 | コニカミノルタ株式会社 | グラフェン積層体とその製造方法 |
CN107158444A (zh) * | 2017-05-05 | 2017-09-15 | 苏州大学 | 一种抗菌增生复合膜及其制备方法 |
Non-Patent Citations (2)
Title |
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ADVANCED MATERIALS, vol. 25, JPN6020013241, 2013, pages 3657 - 3662, ISSN: 0004415763 * |
SCIENTIFIC REPORTS, vol. Vol. 4, Article number: 4684, JPN6020013243, 2014, pages 1 - 8, ISSN: 0004415764 * |
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JP6901155B2 (ja) | 2021-07-14 |
EP3567609B1 (en) | 2021-05-26 |
TW201943643A (zh) | 2019-11-16 |
EP3567609A1 (en) | 2019-11-13 |
TWI655154B (zh) | 2019-04-01 |
US10287168B1 (en) | 2019-05-14 |
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