JP2018524249A - 多孔性グラフェン材料の分散液およびその用途 - Google Patents
多孔性グラフェン材料の分散液およびその用途 Download PDFInfo
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- JP2018524249A JP2018524249A JP2017561350A JP2017561350A JP2018524249A JP 2018524249 A JP2018524249 A JP 2018524249A JP 2017561350 A JP2017561350 A JP 2017561350A JP 2017561350 A JP2017561350 A JP 2017561350A JP 2018524249 A JP2018524249 A JP 2018524249A
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- porous graphene
- dispersion
- sheet
- graphene oxide
- porous
- Prior art date
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 209
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 196
- 239000006185 dispersion Substances 0.000 title claims abstract description 102
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- 239000011148 porous material Substances 0.000 claims description 23
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical group OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 14
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- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 14
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 4
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- 125000004432 carbon atom Chemical group C* 0.000 description 4
- 238000012512 characterization method Methods 0.000 description 4
- 229910000428 cobalt oxide Inorganic materials 0.000 description 4
- 229910000152 cobalt phosphate Inorganic materials 0.000 description 4
- ZBDSFTZNNQNSQM-UHFFFAOYSA-H cobalt(2+);diphosphate Chemical compound [Co+2].[Co+2].[Co+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O ZBDSFTZNNQNSQM-UHFFFAOYSA-H 0.000 description 4
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 4
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- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 4
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- 238000001237 Raman spectrum Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
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- 229910020599 Co 3 O 4 Inorganic materials 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
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- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
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- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 2
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 2
- 229910001947 lithium oxide Inorganic materials 0.000 description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
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- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910000480 nickel oxide Inorganic materials 0.000 description 2
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 2
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- 229910001925 ruthenium oxide Inorganic materials 0.000 description 2
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- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 235000010378 sodium ascorbate Nutrition 0.000 description 2
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 description 2
- 229960005055 sodium ascorbate Drugs 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
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- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/52—Electrically conductive inks
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- 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
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- 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
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- 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
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- 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
- C01B32/20—Graphite
- C01B32/21—After-treatment
- C01B32/23—Oxidation
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
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- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
- C09D11/037—Printing inks characterised by features other than the chemical nature of the binder characterised by the pigment
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/32—Inkjet printing inks characterised by colouring agents
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
- H01M4/8828—Coating with slurry or ink
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- 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
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- 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
- C01B2204/22—Electronic properties
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
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- H—ELECTRICITY
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
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Abstract
Description
本出願は、2015年5月26日に出願された米国仮出願番号第62/166,621号の利益、および2015年6月5日に出願された米国仮出願番号第62/171,737号の利益を主張しており、これら仮出願の内容は、それらの全体が参考として本明細書中に援用される。
本開示は、一般に、多孔性グラフェン材料、より詳細には多孔性グラフェン材料の分散液およびこのような分散液の用途に関する。
グラフェンは、その複数の注目すべき物理的特性および化学的特性により、幅広い技術分野を革新することが予想されてきた。しかし、基底面にπ共役の広がりを有する未加工(primitive)グラフェンまたは化学的に変換されているグラフェンシートは、π−πスタッキング相互作用およびファンデルワールス力によって、互いに再スタックし易く、不可逆的な凝集体を形成し、その結果、比表面積の著しい減少および質量拡散速度の有意な低下を含めた、その特性のかなりの悪化が生じる。さらに、グラフェンシートの再スタッキングは、代表的には、グラファイト様粉末をもたらし、このことは、最終製品を作製するために、さらなる処理手順または不活性(passive)添加物(例えば、電気化学的用途ではバインダ)の含有を必要とし、これは、総合的な性能をさらに悪化させる恐れがある。個々のグラフェンシートが十分に維持されている特性を有する独立したモノリシックグラフェン材料が非常に望ましいが、グラフェンの多数の用途、とりわけ電気化学的エネルギー貯蔵および変換デバイスにとって大きな難題である。多数の提案されている用途のグラフェンの珍しい特質を有効に活用するためには、少なくとも2つの大きな必要条件がある。1つは、大量の溶液処理可能なグラフェンおよびその化学的誘導体が利用可能なことである。もう1つは、グラフェンシートがバルク材料へと処理される際に、再スタッキングにより誘導される特性悪化を低減することである。
高い比表面積および設計された細孔度を有する、溶液処理可能なグラフェンおよびそのバルク材料の大規模化可能な調製が多くの実用的用途で所望されている。本明細書において、本開示の一部の実施形態は、都合のよい温和な欠陥エッチング反応により、豊富な面内ナノ細孔を有する多孔性酸化グラフェンの分散液(例えば、水性分散液)を生成するための大規模化可能な手法を対象としており、多孔性酸化グラフェンは、三次元階層細孔度を有する多孔性グラフェンヒドロゲル、および密集しているが多孔質積層構造を有する多孔性グラフェン紙を含めた、マクロ構造の組立体のための、多様なビルディングブロックとして機能することができることを実証する。これらの多孔性グラフェンのマクロ構造は、非多孔性の対応物と比較して、比表面積およびイオン拡散速度が顕著に改善されていることを示し、約283F/g(またはそれ超)および約234F/cm3(またはそれ超)の極めて高い比静電容量(specific capacitance)、優れた速度能、および優れたサイクル安定性を有する、バインダを含まないスーパーキャパシタ電極として直接使用することができる。より一般には、約1A/gの電流密度(または、約10A/gもしくは約20A/g、または別のより高いもしくはより低い電流密度)における重量比静電容量(gravimetric capacitance)は、少なくとも約160F/g、少なくとも約180F/g、少なくとも約200F/g、少なくとも約220F/g、少なくとも約240F/g、少なくとも約250F/g、少なくとも約260F/gまたは少なくとも約280F/g、および最大約320F/g、最大約360F/g、最大約400F/g、最大約440F/gまたはそれ超とすることができ、約1A/gの電流密度(または、約10A/gもしくは約20A/gまたは別のより高いもしくはより低い電流密度)における体積静電容量(volumetric capacitance)は、少なくとも約140F/cm3、少なくとも約160F/cm3、少なくとも約180F/cm3、少なくとも約200F/cm3または少なくとも約210F/cm3、および最大約240F/cm3、最大約280F/cm3、最大約320F/cm3、最大約360F/cm3またはそれ超であり得る。本開示の実施形態は、溶液処理可能な多孔性グラフェン材料への大規模化可能な経路を提供し、多様な技術分野において、グラフェンの用途に大きく影響を及ぼす。
グラフェンは、その固有の高い導電率、優れた機械的可撓性、約2630m2/gの例外的に大きな理論的表面積、および約550F/gの理論的重量比静電容量のために、スーパーキャパシタ電極材料(他の用途の中でも特に)として望ましい。しかし、グラフェンシート間に強いπ−π相互作用があるので、グラフェンシートは、再スタックしてグラファイト様粉末またはフィルムを形成する傾向があり、このために、表面積がかなり減少してイオン拡散速度が低下し、その結果、重量比静電容量が不十分となって(代表的には、有機電解質中では、<180F/g)、充電/放電速度が相対的に低くなる恐れがある。重量比静電容量に加えて、スーパーキャパシタ用の電極材料を評価するための、別の性能指数は、体積静電容量である。大部分の電極設計では、代表的には、重量比静電容量と体積静電容量との間に両立しない関係性がある。例えば、より高い多孔質の電極は、大きな比表面積をもたらすことができ、高い重量比静電容量のためのイオン拡散に有利であり得るが、その相対的に低い充填密度のために、より低い体積静電容量を有することがある。一方、より密集した電極は体積静電容量を高めるが、イオンが接近可能な表面積およびイオン拡散速度を低下させ、その結果、重量比静電容量がより低くなり、速度性能に乏しくなることがある。したがって、高いエネルギー密度および出力密度を有する実用的なスーパーキャパシタを開発するのに望ましい、優れた速度能を保持しながら、高い重量比静電容量と体積静電容量の両方を実現するには、大変な難題がある。
Claims (18)
- グラフェンをベースとする材料を形成する方法であって、
エッチング液および酸化グラフェンシートを含む混合物を処理するステップであって、多孔性酸化グラフェンシートの形成をもたらすステップ、
再分散用溶媒中で、前記多孔性酸化グラフェンシートを分散するステップであって、前記多孔性酸化グラフェンシートを含む多孔性酸化グラフェン分散液を得るステップ、および
前記多孔性酸化グラフェン分散液を還元条件下で処理するステップであって、前記多孔性酸化グラフェンシートの、グラフェンをベースとする材料への自己集合をもたらすステップ
を含む、方法。 - 前記エッチング液が過酸化水素である、請求項1に記載の方法。
- 前記多孔性酸化グラフェンシートが前記グラフェンをベースとする材料に自己集合する前に、前記多孔性酸化グラフェンシート上に擬似静電容量材料、電気化学的活性材料または触媒を装填するステップをさらに含む、請求項1に記載の方法。
- 前記多孔性酸化グラフェンシートが前記グラフェンをベースとする材料に自己集合した後に、前記グラフェンをベースとする材料に擬似静電容量材料、電気化学的活性材料または触媒を組み込むステップをさらに含む、請求項1に記載の方法。
- グラフェンをベースとする材料を形成する方法であって、
エッチング液および酸化グラフェンシートを含む混合物を処理するステップであって、多孔性酸化グラフェンシートの形成をもたらすステップ、
再分散用溶媒中で、前記多孔性酸化グラフェンシートを分散するステップであって、多孔性酸化グラフェン分散液を得るステップ、
前記多孔性酸化グラフェン分散液を還元条件下で処理するステップであって、多孔性グラフェンシートを含む多孔性グラフェン分散液を得るステップ、および
前記多孔性グラフェンシートを圧縮に供するステップであって、グラフェンをベースとする材料を得るステップ
を含む、方法。 - 前記エッチング液が過酸化水素である、請求項5に記載の方法。
- 前記多孔性グラフェンシートを圧縮に供するステップが、フィルターにより前記多孔性グラフェン分散液の流れ支援式圧縮を行うステップを含む、請求項5に記載の方法。
- 前記多孔性グラフェンシートの圧縮前に、前記多孔性グラフェンシート上に擬似静電容量材料、電気化学的活性材料または触媒を装填するステップをさらに含む、請求項5に記載の方法。
- 前記多孔性グラフェンシートの圧縮に続いて、前記グラフェンをベースとする材料に擬似静電容量材料、電気化学的活性材料または触媒を組み込むステップをさらに含む、請求項5に記載の方法。
- 溶媒、および前記溶媒中に分散している多孔性酸化グラフェンシートを含む、グラフェンをベースとする材料の分散液。
- 前記多孔性酸化グラフェンシートが、最大約50nmのサイズの基底面細孔を有する、請求項10に記載の分散液。
- 前記多孔性酸化グラフェンシートを修飾する無機ナノ構造体をさらに含む、請求項10に記載の分散液。
- 前記溶媒中に分散している無機ナノ構造体をさらに含む、請求項10に記載の分散液。
- 溶媒、および前記溶媒中に分散している多孔性グラフェンシートを含む、グラフェンをベースとする材料の分散液。
- 前記多孔性グラフェンシートが、最大約50nmのサイズの基底面細孔を有する、請求項14に記載の分散液。
- 前記多孔性グラフェンシートを修飾する無機ナノ構造体をさらに含む、請求項14に記載の分散液。
- 前記溶媒中に分散している無機ナノ構造体をさらに含む、請求項14に記載の分散液。
- 請求項10から17のいずれかに記載の分散液を使用する方法であって、
前記分散液を含むインク組成物を形成するステップ、および
薄膜を形成するために前記インク組成物をコーティングするステップ
を含む、方法。
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IL255811A (en) | 2019-08-29 |
HK1252745A1 (zh) | 2019-05-31 |
CN107735360B (zh) | 2022-01-28 |
US20180142114A1 (en) | 2018-05-24 |
EP3303219A4 (en) | 2019-01-09 |
WO2016191564A1 (en) | 2016-12-01 |
EA201792363A1 (ru) | 2018-06-29 |
MX2017015130A (es) | 2018-08-01 |
CA2986897C (en) | 2024-01-09 |
US10689537B2 (en) | 2020-06-23 |
AU2016268388B2 (en) | 2020-10-22 |
AU2016268388A1 (en) | 2017-12-21 |
CN107735360A (zh) | 2018-02-23 |
KR20180061087A (ko) | 2018-06-07 |
EP3303219A1 (en) | 2018-04-11 |
JP7101959B2 (ja) | 2022-07-19 |
IL255811B (en) | 2022-04-01 |
BR112017025163A2 (pt) | 2018-08-07 |
CA2986897A1 (en) | 2016-12-01 |
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