JP6609562B2 - グラフェンの製造方法 - Google Patents
グラフェンの製造方法 Download PDFInfo
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- JP6609562B2 JP6609562B2 JP2016551192A JP2016551192A JP6609562B2 JP 6609562 B2 JP6609562 B2 JP 6609562B2 JP 2016551192 A JP2016551192 A JP 2016551192A JP 2016551192 A JP2016551192 A JP 2016551192A JP 6609562 B2 JP6609562 B2 JP 6609562B2
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims description 353
- 229910021389 graphene Inorganic materials 0.000 title claims description 164
- 238000004519 manufacturing process Methods 0.000 title claims description 32
- 229910002804 graphite Inorganic materials 0.000 claims description 162
- 239000010439 graphite Substances 0.000 claims description 162
- 239000000843 powder Substances 0.000 claims description 153
- 150000003839 salts Chemical class 0.000 claims description 130
- 238000000034 method Methods 0.000 claims description 87
- 238000006056 electrooxidation reaction Methods 0.000 claims description 83
- 229910052739 hydrogen Inorganic materials 0.000 claims description 81
- 239000001257 hydrogen Substances 0.000 claims description 79
- 239000012298 atmosphere Substances 0.000 claims description 71
- 239000007789 gas Substances 0.000 claims description 66
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 49
- 238000010438 heat treatment Methods 0.000 claims description 46
- -1 hydrogen ions Chemical class 0.000 claims description 46
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 40
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 33
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 30
- 239000002135 nanosheet Substances 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 230000001590 oxidative effect Effects 0.000 claims description 21
- 229910001868 water Inorganic materials 0.000 claims description 21
- 229910052786 argon Inorganic materials 0.000 claims description 20
- 239000011261 inert gas Substances 0.000 claims description 20
- 239000003792 electrolyte Substances 0.000 claims description 19
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 17
- 229910052757 nitrogen Inorganic materials 0.000 claims description 16
- 230000008569 process Effects 0.000 claims description 16
- 229910052744 lithium Inorganic materials 0.000 claims description 12
- 230000007797 corrosion Effects 0.000 claims description 10
- 238000005260 corrosion Methods 0.000 claims description 10
- 150000002431 hydrogen Chemical class 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 8
- 239000008151 electrolyte solution Substances 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- 229910052700 potassium Inorganic materials 0.000 claims description 7
- 239000011591 potassium Substances 0.000 claims description 7
- 229910052708 sodium Inorganic materials 0.000 claims description 7
- 239000003575 carbonaceous material Substances 0.000 claims description 6
- 238000009830 intercalation Methods 0.000 claims description 6
- 230000002687 intercalation Effects 0.000 claims description 6
- 229910000103 lithium hydride Inorganic materials 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 229910052987 metal hydride Inorganic materials 0.000 claims description 5
- 238000003828 vacuum filtration Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 150000004681 metal hydrides Chemical class 0.000 claims description 4
- 229910021645 metal ion Inorganic materials 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 description 20
- 239000002608 ionic liquid Substances 0.000 description 17
- 239000010410 layer Substances 0.000 description 13
- 230000015572 biosynthetic process Effects 0.000 description 10
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 6
- 239000002041 carbon nanotube Substances 0.000 description 6
- 238000005229 chemical vapour deposition Methods 0.000 description 6
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 6
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 239000010959 steel Substances 0.000 description 6
- 239000012300 argon atmosphere Substances 0.000 description 5
- 239000002717 carbon nanostructure Substances 0.000 description 5
- 229910021393 carbon nanotube Inorganic materials 0.000 description 5
- 239000011229 interlayer Substances 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000001237 Raman spectrum Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000005868 electrolysis reaction Methods 0.000 description 4
- 238000004627 transmission electron microscopy Methods 0.000 description 4
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 3
- 125000004429 atom Chemical group 0.000 description 3
- 239000011852 carbon nanoparticle Substances 0.000 description 3
- 239000010406 cathode material Substances 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 238000004299 exfoliation Methods 0.000 description 3
- 239000007770 graphite material Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000004626 scanning electron microscopy Methods 0.000 description 3
- 238000007086 side reaction Methods 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 125000005587 carbonate group Chemical group 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 238000002524 electron diffraction data Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910001026 inconel Inorganic materials 0.000 description 2
- 238000003780 insertion Methods 0.000 description 2
- 230000037431 insertion Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical group [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 2
- 150000002642 lithium compounds Chemical class 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000002060 nanoflake Substances 0.000 description 2
- 239000002055 nanoplate Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical class C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- 229910002483 Cu Ka Inorganic materials 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 239000002134 carbon nanofiber Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011280 coal tar Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
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- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
- 238000001493 electron microscopy Methods 0.000 description 1
- 239000000374 eutectic mixture Substances 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- 238000004050 hot filament vapor deposition Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000009847 ladle furnace Methods 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- SIAPCJWMELPYOE-UHFFFAOYSA-N lithium hydride Chemical compound [LiH] SIAPCJWMELPYOE-UHFFFAOYSA-N 0.000 description 1
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
- 229910001947 lithium oxide Inorganic materials 0.000 description 1
- HCQWRNRRURULEY-UHFFFAOYSA-L lithium;potassium;dichloride Chemical compound [Li+].[Cl-].[Cl-].[K+] HCQWRNRRURULEY-UHFFFAOYSA-L 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002057 nanoflower Substances 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 238000005502 peroxidation Methods 0.000 description 1
- 239000002006 petroleum coke Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011829 room temperature ionic liquid solvent Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000007847 structural defect Effects 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/042—Electrodes formed of a single material
- C25B11/043—Carbon, e.g. diamond or graphene
- C25B11/044—Impregnation of carbon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S977/00—Nanotechnology
- Y10S977/70—Nanostructure
- Y10S977/734—Fullerenes, i.e. graphene-based structures, such as nanohorns, nanococoons, nanoscrolls or fullerene-like structures, e.g. WS2 or MoS2 chalcogenide nanotubes, planar C3N4, etc.
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S977/00—Nanotechnology
- Y10S977/84—Manufacture, treatment, or detection of nanostructure
- Y10S977/842—Manufacture, treatment, or detection of nanostructure for carbon nanotubes or fullerenes
- Y10S977/845—Purification or separation of fullerenes or nanotubes
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
- Nanotechnology (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Carbon And Carbon Compounds (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Description
上記に開示した1つ以上の態様による本発明の特定の実施形態を、図面を参照して以下に説明する;
Claims (25)
- (a)水素イオンを含む溶融塩中でのグラファイト電極の電気化学的腐食によって炭素質粉末を形成し、前記溶融塩はリチウム、ナトリウム又はカリウムのハロゲン化物塩を含むステップと、
(b)前記得られた炭素質粉末を前記溶融塩液体から回収するステップと、
(c)前記炭素質粉末を非酸化雰囲気中で加熱することによって前記炭素質粉末を熱処理して、グラフェンシートを含む熱処理粉末を生成するステップと、
を含む、グラフェンシートの製造方法。 - 前記溶融塩が塩化リチウムを含む、請求項1に記載の方法。
- 前記溶融塩が、前記グラファイト電極の前記電気化学的腐食中、湿潤気体と接触しており、前記湿潤気体からの水が、前記溶融塩に溶解し、又は前記溶融塩と反応して前記溶融塩中に水素イオンを導入する、請求項1又は2に記載の方法。
- 前記グラファイト電極の電気化学的腐食が、例えば前記溶融塩が湿潤気体の流れの下で包み込まれる、湿潤気体の雰囲気下で行われる、請求項1から3のいずれか一項に記載の方法。
- 前記溶融塩が、前記グラファイト電極の電気化学的腐食中、前記湿潤気体を散布される、請求項4に記載の方法。
- 前記湿潤気体が、湿潤不活性ガス、例えば湿潤アルゴン又は湿潤窒素である、請求項4又は5に記載の方法。
- 前記湿潤気体が、水源の上部にて、又は水源を通して気体を流すことにより生成される、請求項4から6のいずれか一項に記載の方法。
- 前記グラファイト電極の前記電気化学的腐食中の前記溶融塩の温度が、800℃を超える、請求項1から7のいずれか一項に記載の方法。
- 前記溶融塩が、前記グラファイト電極の前記電気化学的腐食中、乾燥気体と接触しており、前記乾燥気体が、アルゴン又は窒素等の不活性ガスと水素とを含む、請求項1又は2に記載の方法。
- 前記溶融塩及び前記炭素質粉末が、前記溶融塩を冷却し及び凝固させ、前記凝固された塩を前記炭素質粉末から洗浄するステップを含むプロセスによって、前記溶融塩から回収される、請求項1から9のいずれか一項に記載の方法。
- 前記洗浄された炭素質材料の真空濾過のステップを更に含む、請求項10に記載の方法。
- 前記熱処理のステップに先だって、前記炭素質粉末が金属水素化物化合物、例えば水素化リチウムを含み、前記金属水素化物中の金属種が、前記溶融塩に由来する、請求項1から11のいずれか一項に記載の方法。
- 前記炭素質粉末が、還元雰囲気中、例えば、還元気体雰囲気、例えば窒素と水素との混合物を含む雰囲気中で、1000℃を超える温度、例えば1250℃+/−50℃に加熱することによって熱処理される、請求項1から12のいずれか一項に記載の方法。
- 前記炭素質粉末が、低圧環境内で、例えば真空下、又は部分真空下で加熱することによって熱処理される、請求項1から12のいずれか一項に記載の方法。
- 前記グラフェンシートが、200ナノメートルを超える横寸法を有するグラフェンナノシートである、請求項1から14のいずれか一項に記載の方法。
- 前記電極の電気化学的腐食中の前記グラファイト電極における電流が、0.5A/cm2を超え、好ましくは2A/cm2+/−0.5A/cm2である、請求項1から15のいずれか一項に記載の方法。
- 前記グラフェンシートが、前記溶融塩中に浸漬されたグラファイト電極の平方メートル当たり1kg/時間を超える、好ましく1.5kg/時間を超える速度で生成される、請求項1から16のいずれか一項に記載の方法。
- 前記グラファイト電極が、電気化学的腐食中、極性がカソードである、請求項1から17のいずれか一項に記載の方法。
- (a)水素イオンを含む溶融塩中での2つ以上のグラファイト電極の電気化学的腐食によって炭素質粉末を形成するステップであって、前記2つ以上のグラファイト電極のそれぞれは、交互に、ある時間に亘って、正の対電極に関連して負電極として機能して、前記電気化学的腐食を達成する、ステップを含む、請求項1から18のいずれか一項に記載の方法。
- (a)グラファイト電極中への金属イオン種及び水素イオン種の電気化学的インターカレーションによって炭素質粉末を形成し、前記金属イオン種はリチウム、ナトリウム又はカリウムであるステップであって、前記グラファイト電極が電解液と接触して配置されており、前記電解液は前記金属イオン種及び前記水素イオン種を含み、前記電解液はリチウム、ナトリウム又はカリウムのハロゲン化物塩を含む溶融塩であるステップと、
(b)前記得られた炭素質粉末を前記電解液から回収するステップと、
(c)前記炭素質粉末を非酸化雰囲気又は還元雰囲気中で加熱することによって前記炭素質粉末を熱処理して、グラフェンシートを含む熱処理粉末を生成するステップと、
を含む、グラフェンシートの製造方法。 - (a)電解液と接触して配置されたグラファイト電極中への水素の電気化学的インターカレーションによって炭素質粉末を形成するステップであって、前記電解液が水素イオンを含み、前記電解液はリチウム、ナトリウム又はカリウムのハロゲン化物塩を含む溶融塩であるステップと、
(b)前記得られた炭素質粉末を前記電解液から回収するステップと、
(c)前記炭素質粉末を非酸化雰囲気又は還元雰囲気中で加熱することによって前記炭素質粉末を熱処理して、グラフェンシートを含む熱処理粉末を生成するステップと、
を含む、グラフェンシートの製造方法。 - (a)溶融塩中でのグラファイト電極の電気化学的腐食によって炭素質粉末を形成するステップであって、前記溶融塩はリチウム、ナトリウム又はカリウムのハロゲン化物塩を含み、前記グラファイト電極の電気化学的腐食が、不活性ガス及び水素を含む雰囲気下で行われる、ステップと、
(b)前記得られたグラフェンシートを含む炭素質粉末を前記溶融塩から回収するステップと、
を含む、グラフェンシートの製造方法。 - (c)前記炭素質粉末を非酸化雰囲気中で加熱することによって前記炭素質粉末を熱処理して、グラフェンシートを含む熱処理粉末を生成するステップを更に含む、請求項22に記載の方法。
- 前記非酸化雰囲気がアルゴン及び窒素からなるリストから選択される不活性ガスと、水素、好ましくは2〜10モルパーセントの水素、例えば約4モルパーセントの水素とを含み、好ましくは前記非酸化雰囲気が乾燥雰囲気である、請求項23に記載の方法。
- (a)水素イオンを含む溶融塩中での2つ以上のグラファイト電極の電気化学的腐食によって炭素質粉末を形成するステップであって、前記溶融塩はリチウム、ナトリウム又はカリウムのハロゲン化物塩を含み、前記グラファイト電極の電気化学的腐食が、不活性ガス及び水素を含む雰囲気下で行われる、ステップと、
(b)前記得られたグラフェンシートを含む炭素質粉末を前記溶融塩から回収するステップと、
を含む、グラフェンシートの製造方法。
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