JP6830928B2 - 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 - Google Patents
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 Download PDFInfo
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- JP6830928B2 JP6830928B2 JP2018133195A JP2018133195A JP6830928B2 JP 6830928 B2 JP6830928 B2 JP 6830928B2 JP 2018133195 A JP2018133195 A JP 2018133195A JP 2018133195 A JP2018133195 A JP 2018133195A JP 6830928 B2 JP6830928 B2 JP 6830928B2
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- Prior art keywords
- titanium oxide
- oxide particles
- particles according
- carbon
- crystallite
- Prior art date
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims description 146
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims description 143
- 239000002245 particle Substances 0.000 title claims description 101
- 238000003860 storage Methods 0.000 title claims description 15
- 238000004519 manufacturing process Methods 0.000 title claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 84
- 239000010936 titanium Substances 0.000 claims description 80
- 229910052799 carbon Inorganic materials 0.000 claims description 70
- 229910052744 lithium Inorganic materials 0.000 claims description 59
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 57
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 54
- 238000010438 heat treatment Methods 0.000 claims description 48
- 239000011148 porous material Substances 0.000 claims description 29
- 229910052760 oxygen Inorganic materials 0.000 claims description 27
- 239000012298 atmosphere Substances 0.000 claims description 25
- 238000002156 mixing Methods 0.000 claims description 21
- 239000001301 oxygen Substances 0.000 claims description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 16
- 239000002131 composite material Substances 0.000 claims description 15
- -1 zero Chemical compound 0.000 claims description 14
- 239000013078 crystal Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 150000002500 ions Chemical class 0.000 claims description 6
- 230000005389 magnetism Effects 0.000 claims description 3
- 239000012071 phase Substances 0.000 description 39
- 229910052719 titanium Inorganic materials 0.000 description 27
- 239000012467 final product Substances 0.000 description 23
- 238000000034 method Methods 0.000 description 19
- 239000000463 material Substances 0.000 description 17
- 239000000243 solution Substances 0.000 description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 15
- 239000003990 capacitor Substances 0.000 description 13
- 239000000523 sample Substances 0.000 description 13
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 12
- 239000012752 auxiliary agent Substances 0.000 description 12
- 239000000126 substance Substances 0.000 description 12
- 239000002243 precursor Substances 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 10
- 238000005259 measurement Methods 0.000 description 10
- 239000002904 solvent Substances 0.000 description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- 238000010586 diagram Methods 0.000 description 8
- 238000000192 extended X-ray absorption fine structure spectroscopy Methods 0.000 description 8
- 238000000024 high-resolution transmission electron micrograph Methods 0.000 description 8
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 8
- 239000011164 primary particle Substances 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 7
- 239000008151 electrolyte solution Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 6
- 229910001873 dinitrogen Inorganic materials 0.000 description 6
- 238000004146 energy storage Methods 0.000 description 6
- 229910001416 lithium ion Inorganic materials 0.000 description 6
- 239000002105 nanoparticle Substances 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 238000002056 X-ray absorption spectroscopy Methods 0.000 description 5
- 230000004075 alteration Effects 0.000 description 5
- 239000002134 carbon nanofiber Substances 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 238000003795 desorption Methods 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 239000008187 granular material Substances 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 238000001694 spray drying Methods 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 229910003077 Ti−O Inorganic materials 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
- 238000013329 compounding Methods 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- 125000004430 oxygen atom Chemical group O* 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 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
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000011149 active material Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 239000003273 ketjen black Substances 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 description 2
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000011817 metal compound particle Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 2
- 239000002683 reaction inhibitor Substances 0.000 description 2
- 238000000851 scanning transmission electron micrograph Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 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
- 229910000505 Al2TiO5 Inorganic materials 0.000 description 1
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound 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
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 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
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 description 1
- 229910018068 Li 2 O Inorganic materials 0.000 description 1
- 101000878457 Macrocallista nimbosa FMRFamide Proteins 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-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
- 229910009848 Ti4O7 Inorganic materials 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 235000001014 amino acid Nutrition 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 150000001414 amino alcohols Chemical class 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- AOWKSNWVBZGMTJ-UHFFFAOYSA-N calcium titanate Chemical compound [Ca+2].[O-][Ti]([O-])=O AOWKSNWVBZGMTJ-UHFFFAOYSA-N 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000006231 channel black Substances 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- NKZSPGSOXYXWQA-UHFFFAOYSA-N dioxido(oxo)titanium;lead(2+) Chemical compound [Pb+2].[O-][Ti]([O-])=O NKZSPGSOXYXWQA-UHFFFAOYSA-N 0.000 description 1
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- 239000001530 fumaric acid Substances 0.000 description 1
- 235000011087 fumaric acid Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 235000013922 glutamic acid Nutrition 0.000 description 1
- 239000004220 glutamic acid Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 1
- 229910052451 lead zirconate titanate Inorganic materials 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
- 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
- 230000007246 mechanism Effects 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 150000002926 oxygen Chemical class 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- AABBHSMFGKYLKE-SNAWJCMRSA-N propan-2-yl (e)-but-2-enoate Chemical compound C\C=C\C(=O)OC(C)C AABBHSMFGKYLKE-SNAWJCMRSA-N 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- 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 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004098 selected area electron diffraction Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 235000000346 sugar Nutrition 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 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
- 238000005199 ultracentrifugation Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/005—Alkali titanates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/043—Titanium sub-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
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
- H01B1/08—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances oxides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01G11/46—Metal oxides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01G11/50—Electrodes characterised by their material specially adapted for lithium-ion capacitors, e.g. for lithium-doping or for intercalation
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2027—Light-sensitive devices comprising an oxide semiconductor electrode
- H01G9/2031—Light-sensitive devices comprising an oxide semiconductor electrode comprising titanium oxide, e.g. TiO2
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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Description
図1に示すように、本発明に係る新規のチタン酸化物粒子1は、複数の結晶子2が連続的に結合して三次元ネットワーク構造を成し、結晶子2の表面の一部にマグネリ相2aを有する造粒体である。結晶子2は、ランダムに配向して互いに卓面や端面などの表面で結合している。結晶子2が平板形状の場合、三次元ネットワーク構造はカードハウス構造である。チタン酸化物粒子1の内部にはナノサイズの空間部3を多数存在させている。結晶子2の接合界面に粒界を無くし、一方で結晶子2間には微小の細孔4を多数存在させている。
このチタン酸化物粒子1は、チタン酸化物の結晶子2とカーボンの複合体を酸素雰囲気下で熱処理することで得られる。図2に示すように、酸素雰囲気下で複合体を熱処理することによって、複合体からカーボンが焼失し、結晶子2同士が焼結する。更に、酸素雰囲気下で複合体を熱処理することによって、結晶子2の表面がマグネリ相2aへ変質し、以ってチタン酸化物粒子1が生成される。
以下、本発明の実施例1を示すが、本発明は実施例1に限定されるものではない。まず、実施例1として、最初に混合工程を実行した。カーボンナノファイバ20gとテトライソプロポキシチタン245gとをイソプロピルアルコール1300gに添加して、テトライソプロポキシチタンをイソプロピルアルコールに溶解させた。チタンアルコキシドとカーボンナノファイバの重量比は、第1熱処理工程後のチタン酸リチウムとカーボンナノファイバの重量比が約8:2となるように選択した。得られた液を、外筒と内筒の同心円筒からなり、内筒の側面に貫通孔が設けられ、外筒の開口部にせき板が配置されている反応器の内筒内に導入し、35000kgms−2の遠心力が液に印加されるように内筒を300秒間旋回させて、カーボンナノファイバを液に高分散させた。
(従来例1)
従来例1として、水酸化リチウム38g、水800gの水溶液に、ナノサイズ(200nm程度)となるように粉砕した酸化チタン(TiO2)87gを添加して攪拌して溶液を得る。この溶液をスプレードライ装置に導入し噴霧乾燥して乾燥物を得た。得られた乾燥造粒物を大気中で700℃の温度で3時間熱処理を行いチタン酸リチウムの造粒体を得た。この造粒体は、カーボン未使用であるため、熱処理に伴うカーボンとリチウムの結びつきがなく、カーボンとリチウムのそれぞれのガス化に伴う酸素脱離はないものと思われ、マグネリ相2aは形成されていない。また、製造工程中にカーボンが存在しないために、カーボンが除去された空間そのものが存在しない。
実施例1のチタン酸化物粒子1及び従来例1のチタン酸リチウムの細孔分布を測定した。測定方法としては、窒素ガス吸着測定法を用いる。具体的には、粒子表面及び、粒子表面と連通した内部に形成された細孔に窒素ガスを導入し、窒素ガスの吸着量を求める。次いで、導入する窒素ガスの圧力を徐々に増加させ、各平衡圧に対する窒素ガスの吸着量をプロットし、吸着等温曲線を得る。高精度ガス/蒸気吸着量測定装置BELSORP-max-N(日本ベル株式会社製)を用いて測定した。図15は、横軸に細孔径を取り、測定ポイント間の細孔容積の増加分を縦軸に取った差分細孔容積分布を示す。
第2熱処理工程において、実施例1では500℃で6時間の熱処理を施したのに対し、実施例2では収集物100gを350℃で3時間の熱処理を施し、実施例3では収集物100gを300℃で1時間の熱処理を施した。それ以外は、実施例1乃至3は全て同じである。
実施例1のチタン酸化物粒子1及び従来例1のチタン酸リチウムの造粒体に対して5重量%のポリフッ化ビニリデンと適量のN−メチルピロリドンを加えて十分に混練してスラリーを形成し、アルミニウム箔上に塗布し、乾燥して、電極を得た。さらに、得られた電極を用いて、1MのLiBF4のプロピレンカーボネート溶液を電解液とし、対極に活性炭電極を用いたラミネート封止のキャパシタを作成した。
実施例1のチタン酸化物粒子1の導電性を評価した。図17に示すように、三次元ネットワーク構造を有するチタン酸化物粒子1の2箇所にプローブ10,11を接触させて電圧を印加した。すなわち、プローブ10とプローブ11とを接触させたチタン酸結晶体1は異なり、離間している。電圧の印加には、微小デバイス特性評価装置(日立ハイテクノロジーズ社製、N−6000SS)を用いた。
2 結晶子
2a マグネリ相
3 空間部
4 細孔
Claims (19)
- スピネル型のチタン酸リチウムの結晶子が連なった三次元ネットワーク構造を有し、
前記結晶子の表面にマグネリ相としてTi4O7が形成されていること、
を特徴とするチタン酸化物粒子。 - 前記結晶子は、Li4+wTi5O12(0≦w≦3)を含む、請求項1記載のチタン酸化物粒子。
- 前記結晶子の連なりにより前記マグネリ相を含む電子パスが形成されていること、
を特徴とする請求項1又は2記載のチタン酸化物粒子。 - 前記三次元ネットワーク構造内に複数の空間部を有すること、
を特徴とする請求項1乃至3の何れかに一項記載のチタン酸化物粒子。 - 前記結晶子間に前記三次元ネットワーク構造内部に繋がる複数の細孔を有すること、
を特徴とする請求項4記載のチタン酸化物粒子。 - 前記細孔から前記空間部に繋がるイオンパスが形成されていること、
を特徴とする請求項5記載のチタン酸化物粒子。 - 前記結晶子は、互いに粒界なく結合していること、
を特徴とする請求項1乃至6の何れかに記載のチタン酸化物粒子。 - 粒子全体に対してカーボンがゼロを含む5重量%未満であること、
を特徴とする請求項1乃至7の何れかに記載のチタン酸化物粒子。 - 前記結晶子は、平板形状を有し、
前記三次元ネットワーク構造はカードハウス構造であること、
を特徴とする請求項1乃至8の何れかに記載のチタン酸化物粒子。 - 前記結晶子の縁表面にマグネリ相が形成されていること、
を特徴とする請求項1乃至9の何れかに記載のチタン酸化物粒子。 - 請求項1乃至10の何れかに記載のチタン酸化物粒子を含み構成されること、
を特徴とする蓄電デバイス用電極。 - 請求項1乃至10の何れかに記載のチタン酸化物粒子を含み構成される電極を備えた蓄電デバイス。
- スピネル型のチタン酸リチウムの結晶子とカーボンとの複合体を酸素雰囲気下で熱処理することで、前記カーボンを焼失させ、且つチタン酸化物の結晶子同士を連ならせて三次元ネットワーク構造の粒子を形成するとともに、前記結晶子の表面にマグネリ相としてTi4O7を形成すること、
を特徴とするチタン酸化物粒子の製造方法。 - 前記結晶子は、Li4+wTi5O12(0≦w≦3)を含む、請求項13記載のチタン酸化物粒子の製造方法。
- 前記熱処理の温度は400〜600℃であること、
を特徴とする請求項13又は14記載のチタン酸化物粒子の製造方法。 - 前記熱処理の時間は、0.5以上10時間以下であること、
を特徴とする請求項13乃至15の何れかに記載のチタン酸化物粒子の製造方法。 - 前記複合体は、
前記チタン酸化物源とカーボン源の混合工程と、
前記混合工程を経た混合物を不活性雰囲気下で熱処理する工程と、
により生成されること、
を特徴とする請求項13乃至16の何れかに記載のチタン酸化物粒子の製造方法。 - 前記不活性雰囲気下での熱処理の温度は、600〜950℃であること、
を特徴とする請求項17記載のチタン酸化物粒子の製造方法。 - 前記混合工程は、溶液中の前記チタン酸化物源とカーボン源に対するメカノケミカル処理を含むこと、
を特徴とする請求項17又は18記載のチタン酸化物粒子の製造方法。
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EP3279143A4 (en) * | 2015-03-31 | 2018-10-31 | 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 |
JP6767180B2 (ja) * | 2016-06-22 | 2020-10-14 | 日本ケミコン株式会社 | リチウム二次電池及びその製造方法 |
FR3060554B1 (fr) * | 2016-12-20 | 2022-04-01 | Saint Gobain Ct Recherches | Produits ceramiques de sous oxydes de titane |
JP7181709B2 (ja) * | 2018-06-06 | 2022-12-01 | 株式会社豊田中央研究所 | 蓄電デバイス |
CN108862377B (zh) * | 2018-08-27 | 2021-03-02 | 中科廊坊过程工程研究院 | 一种Ti4O7纳米材料及其制备方法和用途 |
CN108946798B (zh) * | 2018-09-06 | 2021-04-30 | 中国石油天然气股份有限公司 | 一种线状分级结构钛酸锂材料及制备和应用 |
EP3885316A4 (en) * | 2018-11-22 | 2022-05-04 | Nippon Chemi-Con Corporation | METAL COMPOUND, ELECTRODE FOR POWER STORAGE DEVICE, POWER STORAGE DEVICE AND METHOD OF MAKING METAL COMPOUND |
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US20120251887A1 (en) * | 2011-04-04 | 2012-10-04 | Brookhaven Science Associates, Llc | Carbon-Coated Magneli-Phase TinO2n-1 Nanomaterials and a Method of Synthesis Thereof |
JP5916007B2 (ja) | 2011-09-28 | 2016-05-11 | 日本ケミコン株式会社 | チタン酸リチウムとカーボンナノファイバーとの複合体の製造方法 |
KR101938439B1 (ko) | 2011-10-29 | 2019-01-14 | 닛뽄 케미콘 가부시끼가이샤 | 전극 재료의 제조 방법 |
CN102496704B (zh) | 2011-12-08 | 2014-04-23 | 中信国安盟固利电源技术有限公司 | 一种钛酸锂/亚氧化钛负极材料及其制备方法 |
KR102110777B1 (ko) | 2012-09-03 | 2020-05-14 | 닛뽄 케미콘 가부시끼가이샤 | 리튬 이온 이차 전지용 전극 재료, 이 전극 재료의 제조 방법, 및 리튬 이온 이차 전지 |
JP6363550B2 (ja) | 2014-12-16 | 2018-07-25 | 日本ケミコン株式会社 | 金属化合物粒子群の製造方法、金属化合物粒子群及び金属化合物粒子群を含む蓄電デバイス用電極 |
EP3279143A4 (en) * | 2015-03-31 | 2018-10-31 | 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 |
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EP3279143A1 (en) | 2018-02-07 |
KR102394216B1 (ko) | 2022-05-09 |
US10490316B2 (en) | 2019-11-26 |
JP2016193816A (ja) | 2016-11-17 |
US20180072584A1 (en) | 2018-03-15 |
CN107428553B (zh) | 2020-09-29 |
JP6375331B2 (ja) | 2018-08-15 |
KR20170133323A (ko) | 2017-12-05 |
JP2018203615A (ja) | 2018-12-27 |
WO2016157551A1 (ja) | 2016-10-06 |
EP3279143A4 (en) | 2018-10-31 |
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