JP2011236061A - チタン酸リチウム結晶構造体、チタン酸リチウム結晶構造体とカーボンの複合体、その製造方法、その複合体を用いた電極及び電気化学素子 - Google Patents
チタン酸リチウム結晶構造体、チタン酸リチウム結晶構造体とカーボンの複合体、その製造方法、その複合体を用いた電極及び電気化学素子 Download PDFInfo
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- JP2011236061A JP2011236061A JP2010106052A JP2010106052A JP2011236061A JP 2011236061 A JP2011236061 A JP 2011236061A JP 2010106052 A JP2010106052 A JP 2010106052A JP 2010106052 A JP2010106052 A JP 2010106052A JP 2011236061 A JP2011236061 A JP 2011236061A
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- Prior art keywords
- crystal structure
- lithium titanate
- titanate crystal
- carbon
- composite
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 126
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 125
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 118
- 239000013078 crystal Substances 0.000 title claims abstract description 98
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims description 40
- 229910052799 carbon Inorganic materials 0.000 title claims description 30
- 239000002134 carbon nanofiber Substances 0.000 claims abstract description 64
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000002243 precursor Substances 0.000 claims abstract description 21
- 239000011230 binding agent Substances 0.000 claims abstract description 6
- 239000002131 composite material Substances 0.000 claims description 50
- 239000010936 titanium Substances 0.000 claims description 28
- 229910052719 titanium Inorganic materials 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000003990 capacitor Substances 0.000 claims description 9
- 230000002829 reductive effect Effects 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 21
- 238000010303 mechanochemical reaction Methods 0.000 abstract description 9
- 239000003153 chemical reaction reagent Substances 0.000 abstract 1
- 230000001747 exhibiting effect Effects 0.000 abstract 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 24
- -1 titanium alkoxide Chemical class 0.000 description 18
- 239000000843 powder Substances 0.000 description 13
- 239000000376 reactant Substances 0.000 description 12
- 239000010409 thin film Substances 0.000 description 10
- 235000011054 acetic acid Nutrition 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 238000003917 TEM image Methods 0.000 description 6
- 239000002041 carbon nanotube Substances 0.000 description 5
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 description 5
- 239000012046 mixed solvent Substances 0.000 description 5
- 239000002683 reaction inhibitor Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- 239000002033 PVDF binder Substances 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 4
- 239000010408 film Substances 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 239000007858 starting material Substances 0.000 description 4
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 239000008151 electrolyte solution Substances 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
- 229910013063 LiBF 4 Inorganic materials 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 2
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 235000019260 propionic acid Nutrition 0.000 description 2
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 150000001414 amino alcohols Chemical class 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000011852 carbon nanoparticle Substances 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000001530 fumaric acid Substances 0.000 description 1
- 235000011087 fumaric acid Nutrition 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000003273 ketjen black Substances 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
-
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B1/00—Nanostructures formed by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
-
- 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
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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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- 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
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
-
- C—CHEMISTRY; METALLURGY
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/005—Alkali titanates
-
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- 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
- H01G11/04—Hybrid capacitors
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- 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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
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- 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
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- 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
- H01G11/50—Electrodes characterised by their material specially adapted for lithium-ion capacitors, e.g. for lithium-doping or for intercalation
-
- H—ELECTRICITY
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- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/12—Surface area
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- C01P2006/40—Electric properties
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- H—ELECTRICITY
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- 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
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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- 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
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Abstract
【解決手段】数原子層レベルの厚みを有し、二次元面が平面状をしたチタン酸リチウム結晶構造体をカーボンナノファイバー(CNF)に高分散担持させる。チタン酸リチウム結晶構造体の前駆体とこれを担持したCNFは、旋回する反応器内で反応物にずり応力と遠心力を与えるメカノケミカル反応によって作製する。チタン酸リチウム結晶構造体とカーボンナノファイバーの質量比が75:25〜85:15が好ましい。カーボンナノファイバーは、その外径が10〜30nmで、外比表面積は150〜350cm2/gが好ましい。この複合体をバインダーと混合した後、成形して電極を得て、この電極を電気化学素子に用いる。
【選択図】図1
Description
本発明で用いる反応方法は、本出願人等が先に特許出願した特許文献1及び特許文献2に示した方法と同様のメカノケミカル反応であって、化学反応の過程で、旋回する反応器内で反応物にずり応力と遠心力を加えて化学反応を促進させるものである。
本発明に係るチタン酸リチウム結晶構造体は、例えば、チタンアルコキシドなどのチタン源、酢酸リチウム、硝酸リチウム、炭酸リチウム、水酸化リチウムなどのリチウム源を出発原料として使用し、前記メカノケミカル反応により、チタン酸リチウム結晶構造体の前駆体を生成する。本実施例では、このチタン酸リチウム結晶構造体の前駆体を窒素雰囲気中で加熱することにより、酸素欠陥のサイトに窒素がドープされたチタン酸リチウム結晶構造体を生成する。
反応過程でCNFを加えることによって、5〜100nmのチタン酸リチウム結晶構造体とカーボンの複合体を得ることができる。すなわち、反応器の内筒の内部に前記チタン源とリチウム源、反応抑制剤と所定量のCNFを投入して、内筒を旋回して金属塩と反応抑制剤とCNFを混合、分散する。さらに内筒を旋回させながら水酸化ナトリウムなどの触媒を投入して加水分解、縮合反応を進行させ、チタン酸リチウムを生成すると共に、このチタン酸リチウムとカーボンを分散状態で、混合する。反応終了後にこれを急速加熱することで、チタン酸リチウム結晶構造体を高分散担持させたカーボンを形成することができる。
複合体において、チタン酸リチウム結晶構造体とカーボンの割合は、75:25〜85:15、特に、この割合は、従来提案されていた70:30に比較して、チタン酸リチウム結晶構造体の割合が多く、そのため、メカノケミカル反応下で、チタン酸リチウムが反応器の周方向に向かってシート状に成長することを助けている。また、この範囲の臨界的意義は、電極あたりの容量によって定まるものであり、この範囲では大きな電極容量を得ることができる。
溶媒としては、アルコール類、水、これらの混合溶媒を用いることができる。例えば、酢酸と酢酸リチウムをイソプロパノールと水の混合物に溶解した混合溶媒を使用することができる。
出発原料としてチタンアルコキシドを使用した場合には、特許文献2に記載のように、前記メカノケミカル反応を適用する所定のチタンアルコキシドに、反応抑制剤として該チタンアルコキシドと錯体を形成する所定の化合物を添加することができる。これにより、化学反応が促進しすぎるのを抑制することができる。
本実施例では、メカノケミカル反応によりカーボンナノ粒子の構造体の内部にチタン酸リチウム結晶構造体の前駆体を担持させた複合体を得ると共に、このチタン酸リチウム結晶構造体とカーボンの複合体を加熱することによって、チタン酸リチウムの結晶化を促進させ、この複合体を使用した電極や電気化学素子の容量、出力特性を向上させる。
本発明により得られたチタン酸リチウム結晶構造体とカーボンの複合体は、バインダーと混錬、成型し、電気化学素子の電極、すなわち電気エネルギー貯蔵用電極とすることができ、その電極は高出力特性、高容量特性を示す。
この電極を用いることができる電気化学素子は、リチウムやマグネシウムなどの金属イオンを含有する電解液を用いる電気化学キャパシタ、電池である。すなわち、本発明の電極は、金属イオンの吸蔵、脱着を行うことができ、負極や正極として作動する。したがって、リチウムイオンを含有する電解液を用い、対極として活性炭、リチウムイオンを吸蔵、脱着するカーボンや金属酸化物等を用いることによって、電気化学キャパシタ、電池を構成することができる。
チタンアルコキシド1モルに対して、酢酸1.8モル、酢酸リチウム1モルとなる量の酢酸と酢酸リチウムをイソプロパノールと水の混合物に溶解して混合溶媒を作製した。この混合溶媒とチタンアルコキシド、CNFを旋回反応器内に投入し、66000N(kgms-2)の遠心力で5分間、内筒を旋回して外筒の内壁に反応物の薄膜を形成すると共に、反応物にずり応力と遠心力を加えて化学反応を促進させ、チタン酸リチウム結晶構造体の前駆体を高分散担持したCNFを得た。この場合、混合溶媒に溶解するチタンアルコキシドとCNFの量は、得られる複合体の組成が、チタン酸リチウム/CNFが、80/20の質量比(w/w)となるように設定した。
得られるチタン酸リチウム結晶構造体とCNFの配合比が75/25となるように混合溶液に溶解するチタンアルコキシドとCNFの量を変更する以外は、前記実施例と同様にして、チタン酸リチウム結晶構造体とCNFの複合体粉末を作製した。
得られるチタン酸リチウム結晶構造体とCNFの配合比が85/15となるように混合溶液に溶解するチタンアルコキシドとCNFの量を変更する以外は、前記実施例と同様にして、チタン酸リチウム結晶構造体とCNFの複合体粉末を作製した。
得られるチタン酸リチウム結晶構造体とCNFの配合比が70/30となるように混合溶液に溶解するチタンアルコキシドとCNFの量を変更する以外は、前記実施例と同様にして、チタン酸リチウム結晶構造体とCNFの複合体粉末を作製した。
Li4Ti5O12:CNF=80:20 容量:131mAh/g
(2) 実施例2
Li4Ti5O12:CNF=75:25 容量:125mAh/g
(3) 実施例3
Li4Ti5O12:CNF=85:15 容量:137mAh/g
(4) 比較例1
Li4Ti5O12:CNF=70:30 容量:118mAh/g
実施例1の複合体粉末9重量部と、1重量部のPVDF(ポリフッ化ビニリデン)バインダーを混練し、圧延してシートを形成した。このシートを真空乾燥後、銅箔に接合し、負極とした。
実施例2の複合体粉末を用いて、同様にして、ハイブリッドキャパシタセルを作製した。
実施例3の複合体粉末を用いて、同様にして、ハイブリッドキャパシタセルを作製した。
比較例1の複合体粉末を用いて、同様にして、ハイブリッドキャパシタセルを作製した。
Claims (13)
- 2〜5原子層レベルで1nm以下の厚みを有し、二次元面の一辺が5〜100nmの平板状に展開しているチタン酸リチウム結晶構造体。
- 二次元面が(111)面である請求項1に記載のチタン酸リチウム結晶構造体。
- 厚みと二次元面の一辺の比が1:5〜1:350である請求項1に記載のチタン酸リチウム結晶構造体。
- チタン源とリチウム源を含む溶液にずり応力と遠心力を加えて反応させて、チタン酸リチウム結晶構造体の前駆体を製造し、この前駆体を加熱して得られる数原子層レベルの厚みを有する平板状の結晶構造体からなる請求項1から請求項3のいずれか1項に記載のチタン酸リチウム結晶構造体。
- 請求項1に記載のチタン酸リチウム結晶構造体をカーボンナノファイバーに分散担持させたチタン酸リチウム結晶構造体とカーボンの複合体。
- チタン酸リチウム結晶構造体とカーボンナノファイバーの質量比が75:25〜85:15である請求項5に記載のチタン酸リチウム結晶構造体とカーボンの複合体。
- 前記カーボンナノファイバーが、その外径が10〜30nmで、外比表面積は150〜350cm2/gである請求項5に記載のチタン酸リチウム結晶構造体とカーボンの複合体。
- 旋回する反応器内において、製造される複合体のチタン酸リチウム結晶構造体とカーボンナノファイバーとの質量比が75:25〜85:15となるような量のチタン源、リチウム源及びカーボンナノファイバーを含む溶液に、ずり応力と遠心力を加えて反応させてチタン酸リチウム結晶構造体の前駆体とカーボンナノファイバーの複合体を製造し、この複合体を加熱して得られる数原子層レベルの厚みを有する平板状のチタン酸リチウム結晶構造体がカーボンナノファイバーに担持されている請求項5に記載のチタン酸リチウム結晶構造体とカーボンの複合体。
- 前記請求項5に記載の複合体をバインダーと混合した後、成形して得られる電極。
- 請求項5に記載の電極を用いた電気化学素子。
- 請求項9に記載の電極を負極に用い、分極性電極を正極に用いた電気化学キャパシタ。
- 旋回する反応器内において、チタン源とリチウム源を含む溶液にずり応力と遠心力を加えて反応させて、チタン酸リチウム結晶構造体の前駆体を製造し、この前駆体を加熱して数原子層レベルの厚みを有する平板状のチタン酸リチウム結晶構造体を製造することを特徴とするチタン酸リチウム結晶構造体の製造方法。
- 旋回する反応器内において、製造される複合体のチタン酸リチウム結晶構造体とカーボンナノファイバーとの質量比が75:25〜85:15となるような量のチタン源、リチウム源及びカーボンナノファイバーを含む溶液に、ずり応力と遠心力を加えて反応させてチタン酸リチウム結晶構造体の前駆体とカーボンナノファイバーの複合体を製造し、この前駆体とカーボンナノファイバーの複合体を加熱して数原子層レベルの厚みを有する平板状のチタン酸リチウム結晶構造体とカーボンナノファイバーの複合体を生成することを特徴とするチタン酸リチウム結晶構造体とカーボンナノファイバーの複合体の製造方法。
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JP2012209032A (ja) * | 2011-03-29 | 2012-10-25 | Toray Ind Inc | 金属化合物−導電剤複合体およびそれを用いてなるリチウム二次電池、および金属化合物−導電剤複合体の製造方法 |
JP2015050170A (ja) * | 2013-09-04 | 2015-03-16 | 日本ケミコン株式会社 | 電極材料、該電極材料を備えた蓄電デバイス及び電極材料の製造方法 |
WO2016157551A1 (ja) * | 2015-03-31 | 2016-10-06 | 日本ケミコン株式会社 | チタン酸化物粒子、チタン酸化物粒子の製造方法、チタン酸化物粒子を含む蓄電デバイス用電極、チタン酸化物粒子を含む電極を備えた蓄電デバイス |
JPWO2016159323A1 (ja) * | 2015-03-31 | 2018-04-26 | 日本ケミコン株式会社 | チタン酸化物結晶体、チタン酸化物結晶体を含む蓄電デバイス用電極 |
JP7457228B1 (ja) | 2023-06-30 | 2024-03-28 | artience株式会社 | 二次電池電極用複合物の製造方法 |
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JP5965015B2 (ja) * | 2015-03-23 | 2016-08-03 | 日本ケミコン株式会社 | チタン酸リチウム結晶構造体 |
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CN108134072B (zh) * | 2018-01-30 | 2022-01-28 | 中国科学院宁波材料技术与工程研究所 | 一种钛酸锂基复合材料及其制备方法 |
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CN113659127A (zh) * | 2021-08-19 | 2021-11-16 | 电子科技大学长三角研究院(湖州) | 一种碳纳米纤维/钛酸锂复合电极材料及其制备方法和应用 |
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JP2015050170A (ja) * | 2013-09-04 | 2015-03-16 | 日本ケミコン株式会社 | 電極材料、該電極材料を備えた蓄電デバイス及び電極材料の製造方法 |
WO2016157551A1 (ja) * | 2015-03-31 | 2016-10-06 | 日本ケミコン株式会社 | チタン酸化物粒子、チタン酸化物粒子の製造方法、チタン酸化物粒子を含む蓄電デバイス用電極、チタン酸化物粒子を含む電極を備えた蓄電デバイス |
JP2016193816A (ja) * | 2015-03-31 | 2016-11-17 | 日本ケミコン株式会社 | チタン酸化物粒子、チタン酸化物粒子の製造方法、チタン酸化物粒子を含む蓄電デバイス用電極、チタン酸化物粒子を含む電極を備えた蓄電デバイス |
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US10438751B2 (en) | 2015-03-31 | 2019-10-08 | Nippon Chemi-Con Corporation | Titanium oxide crystal body and power storage device electrode including titanium oxide crystalline body |
US10490316B2 (en) | 2015-03-31 | 2019-11-26 | Nippon Chemi-Con Corporation | Titanium oxide particles, titanium oxide particle production method, power storage device electrode including titanium oxide particles, and power storage device provided with electrode including titanium oxide particles |
JP7457228B1 (ja) | 2023-06-30 | 2024-03-28 | artience株式会社 | 二次電池電極用複合物の製造方法 |
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KR101793307B1 (ko) | 2017-11-02 |
JP5836568B2 (ja) | 2015-12-24 |
WO2011138866A1 (ja) | 2011-11-10 |
US9368793B2 (en) | 2016-06-14 |
US20130115516A1 (en) | 2013-05-09 |
US9005814B2 (en) | 2015-04-14 |
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