JP7092752B2 - 正極活物質粒子の作製方法 - Google Patents
正極活物質粒子の作製方法 Download PDFInfo
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- JP7092752B2 JP7092752B2 JP2019516295A JP2019516295A JP7092752B2 JP 7092752 B2 JP7092752 B2 JP 7092752B2 JP 2019516295 A JP2019516295 A JP 2019516295A JP 2019516295 A JP2019516295 A JP 2019516295A JP 7092752 B2 JP7092752 B2 JP 7092752B2
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- 239000002245 particle Substances 0.000 title claims description 97
- 239000007774 positive electrode material Substances 0.000 title claims description 56
- 238000004519 manufacturing process Methods 0.000 title claims description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 20
- 239000007784 solid electrolyte Substances 0.000 claims description 20
- -1 graphene compound Chemical class 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 19
- 229910021389 graphene Inorganic materials 0.000 claims description 17
- 239000000725 suspension Substances 0.000 claims description 14
- 150000002642 lithium compounds Chemical class 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 10
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 10
- 229910052744 lithium Inorganic materials 0.000 claims description 10
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 239000007921 spray Substances 0.000 claims description 7
- 229910052723 transition metal Inorganic materials 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
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- 239000001569 carbon dioxide Substances 0.000 claims description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical group [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 238000007600 charging Methods 0.000 description 63
- 229910000664 lithium aluminum titanium phosphates (LATP) Inorganic materials 0.000 description 31
- 238000000034 method Methods 0.000 description 21
- 239000011241 protective layer Substances 0.000 description 20
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- 238000007599 discharging Methods 0.000 description 13
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 12
- 229910001416 lithium ion Inorganic materials 0.000 description 12
- 239000010410 layer Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 8
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 8
- 238000001694 spray drying Methods 0.000 description 8
- 238000003860 storage Methods 0.000 description 8
- VAYTZRYEBVHVLE-UHFFFAOYSA-N 1,3-dioxol-2-one Chemical compound O=C1OC=CO1 VAYTZRYEBVHVLE-UHFFFAOYSA-N 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000010281 constant-current constant-voltage charging Methods 0.000 description 7
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 6
- 229910052731 fluorine Inorganic materials 0.000 description 6
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- 239000011777 magnesium Substances 0.000 description 6
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- 230000007423 decrease Effects 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 230000006866 deterioration Effects 0.000 description 4
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- 150000002500 ions Chemical class 0.000 description 4
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- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 3
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
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- 235000002639 sodium chloride Nutrition 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 102100031786 Adiponectin Human genes 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 101000775469 Homo sapiens Adiponectin Proteins 0.000 description 1
- 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 description 1
- 229910009178 Li1.3Al0.3Ti1.7(PO4)3 Inorganic materials 0.000 description 1
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 1
- 229910002099 LiNi0.5Mn1.5O4 Inorganic materials 0.000 description 1
- 229910013870 LiPF 6 Inorganic materials 0.000 description 1
- 239000002228 NASICON Substances 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- PFYQFCKUASLJLL-UHFFFAOYSA-N [Co].[Ni].[Li] Chemical compound [Co].[Ni].[Li] PFYQFCKUASLJLL-UHFFFAOYSA-N 0.000 description 1
- ZYXUQEDFWHDILZ-UHFFFAOYSA-N [Ni].[Mn].[Li] Chemical compound [Ni].[Mn].[Li] ZYXUQEDFWHDILZ-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
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- 229910052791 calcium Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- CKFRRHLHAJZIIN-UHFFFAOYSA-N cobalt lithium Chemical compound [Li].[Co] CKFRRHLHAJZIIN-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
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- 239000002241 glass-ceramic Substances 0.000 description 1
- VGYDTVNNDKLMHX-UHFFFAOYSA-N lithium;manganese;nickel;oxocobalt Chemical compound [Li].[Mn].[Ni].[Co]=O VGYDTVNNDKLMHX-UHFFFAOYSA-N 0.000 description 1
- URIIGZKXFBNRAU-UHFFFAOYSA-N lithium;oxonickel Chemical compound [Li].[Ni]=O URIIGZKXFBNRAU-UHFFFAOYSA-N 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
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Description
図1に工程フロー図を示す。
本実施の形態では、車両に本発明の一態様である二次電池を搭載する例を示す。
サンプル1:GOは0.5wt%(LATPを5wt%)
サンプル2:GOは0.2wt%(LATPを5wt%)
サンプル3:LATPを2wt%(GOは0.5wt%)
サンプル4:LATPを4wt%(GOは0.5wt%)
サンプル5:LATPを8wt%(GOは0.5wt%)
サンプル6:GOなし、LATPなし
サンプル7:GO0.5wt%、LATPなし
サンプル8:LATPを0.2wt%(GOは0.5wt%)
サンプル9:LATPを0.5wt%(GOは0.5wt%)
次に、上記で作製したサンプル1、2の二次電池のサイクル特性の評価を行った。結果を図6に示す。図6の結果から、GOは、0.2wt%よりも0.5wt%としたサンプル1のサイクル特性が良好であった。
なお、二次電池の充放電は、たとえば下記のように行うことができる。
Claims (6)
- リチウムと遷移金属元素と酸素を有するリチウム化合物粒子と、グラフェン化合物と、固体電解質と、溶媒とを含む懸濁液を噴霧し、
加熱により表面に含まれる炭素を炭酸ガスに変えて揮散させる正極活物質粒子の作製方法。 - 請求項1において、前記噴霧はスプレーノズルを用いる正極活物質粒子の作製方法。
- 請求項1または請求項2において、前記固体電解質はNASICON型のリン酸化合物である正極活物質粒子の作製方法。
- 請求項1乃至請求項3のいずれか一において、前記溶媒は、水およびエタノールである正極活物質粒子の作製方法。
- 請求項1乃至請求項4のいずれか一において、前記加熱は大気雰囲気下で前記固体電解質の融点以上の温度で行う正極活物質粒子の作製方法。
- 請求項1乃至請求項5のいずれか一において、前記遷移金属元素はコバルトである正極活物質粒子の作製方法。
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KR102606545B1 (ko) | 2017-05-12 | 2023-11-24 | 가부시키가이샤 한도오따이 에네루기 켄큐쇼 | 양극 활물질 입자 |
CN117096337A (zh) | 2017-05-19 | 2023-11-21 | 株式会社半导体能源研究所 | 锂离子二次电池 |
KR102529620B1 (ko) | 2017-06-26 | 2023-05-04 | 가부시키가이샤 한도오따이 에네루기 켄큐쇼 | 양극 활물질의 제작 방법 및 이차 전지 |
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