JP7509513B2 - リチウムイオン二次電池用正極活物質の製造方法 - Google Patents
リチウムイオン二次電池用正極活物質の製造方法 Download PDFInfo
- Publication number
- JP7509513B2 JP7509513B2 JP2017223441A JP2017223441A JP7509513B2 JP 7509513 B2 JP7509513 B2 JP 7509513B2 JP 2017223441 A JP2017223441 A JP 2017223441A JP 2017223441 A JP2017223441 A JP 2017223441A JP 7509513 B2 JP7509513 B2 JP 7509513B2
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- Japan
- Prior art keywords
- lithium
- positive electrode
- nickel
- composite oxide
- active material
- Prior art date
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- 239000007774 positive electrode material Substances 0.000 title claims description 59
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims description 38
- 229910001416 lithium ion Inorganic materials 0.000 title claims description 38
- 238000004519 manufacturing process Methods 0.000 title claims description 33
- 239000002131 composite material Substances 0.000 claims description 129
- 239000000843 powder Substances 0.000 claims description 94
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 84
- RSNHXDVSISOZOB-UHFFFAOYSA-N lithium nickel Chemical compound [Li].[Ni] RSNHXDVSISOZOB-UHFFFAOYSA-N 0.000 claims description 84
- 238000010304 firing Methods 0.000 claims description 77
- 229910052744 lithium Inorganic materials 0.000 claims description 76
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 66
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 65
- 229910001868 water Inorganic materials 0.000 claims description 64
- 238000005406 washing Methods 0.000 claims description 53
- 239000002245 particle Substances 0.000 claims description 48
- 239000000203 mixture Substances 0.000 claims description 44
- 150000002816 nickel compounds Chemical class 0.000 claims description 44
- 229910052759 nickel Inorganic materials 0.000 claims description 41
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 40
- 229910052760 oxygen Inorganic materials 0.000 claims description 33
- 239000001301 oxygen Substances 0.000 claims description 33
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 32
- 150000002642 lithium compounds Chemical class 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 24
- 239000007789 gas Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 16
- 229910052723 transition metal Inorganic materials 0.000 claims description 16
- 229910052799 carbon Inorganic materials 0.000 claims description 15
- 238000001354 calcination Methods 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 12
- 150000003624 transition metals Chemical class 0.000 claims description 9
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 7
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium;hydroxide;hydrate Chemical compound [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 claims description 4
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 229910052758 niobium Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 description 25
- 238000003786 synthesis reaction Methods 0.000 description 22
- 239000002994 raw material Substances 0.000 description 16
- 238000005245 sintering Methods 0.000 description 15
- -1 Lithium transition metal Chemical class 0.000 description 12
- 239000012298 atmosphere Substances 0.000 description 10
- 230000008569 process Effects 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 238000001035 drying Methods 0.000 description 9
- 239000002002 slurry Substances 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- 239000007788 liquid Substances 0.000 description 8
- 239000002904 solvent Substances 0.000 description 8
- 239000011230 binding agent Substances 0.000 description 7
- 239000013078 crystal Substances 0.000 description 7
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- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 4
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- 229910017052 cobalt Inorganic materials 0.000 description 4
- 239000010941 cobalt Substances 0.000 description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 4
- CKFRRHLHAJZIIN-UHFFFAOYSA-N cobalt lithium Chemical compound [Li].[Co] CKFRRHLHAJZIIN-UHFFFAOYSA-N 0.000 description 4
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910021383 artificial graphite Inorganic materials 0.000 description 2
- 150000001869 cobalt compounds Chemical class 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
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- PQVSTLUFSYVLTO-UHFFFAOYSA-N ethyl n-ethoxycarbonylcarbamate Chemical compound CCOC(=O)NC(=O)OCC PQVSTLUFSYVLTO-UHFFFAOYSA-N 0.000 description 2
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- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 2
- 229910052808 lithium carbonate Inorganic materials 0.000 description 2
- 229940040692 lithium hydroxide monohydrate Drugs 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
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- ZZXUZKXVROWEIF-UHFFFAOYSA-N 1,2-butylene carbonate Chemical compound CCC1COC(=O)O1 ZZXUZKXVROWEIF-UHFFFAOYSA-N 0.000 description 1
- YBJCDTIWNDBNTM-UHFFFAOYSA-N 1-methylsulfonylethane Chemical compound CCS(C)(=O)=O YBJCDTIWNDBNTM-UHFFFAOYSA-N 0.000 description 1
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
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- GKZFQPGIDVGTLZ-UHFFFAOYSA-N 4-(trifluoromethyl)-1,3-dioxolan-2-one Chemical compound FC(F)(F)C1COC(=O)O1 GKZFQPGIDVGTLZ-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 1
- 229920002943 EPDM rubber Polymers 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 229910000733 Li alloy Inorganic materials 0.000 description 1
- 229910008695 Li2Ni8O10 Inorganic materials 0.000 description 1
- 229910015015 LiAsF 6 Inorganic materials 0.000 description 1
- 229910013063 LiBF 4 Inorganic materials 0.000 description 1
- 229910013684 LiClO 4 Inorganic materials 0.000 description 1
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 1
- 229910013131 LiN Inorganic materials 0.000 description 1
- 229910013290 LiNiO 2 Inorganic materials 0.000 description 1
- 229910003005 LiNiO2 Inorganic materials 0.000 description 1
- 229910013870 LiPF 6 Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
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- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
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- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 description 1
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- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 1
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- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
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- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 description 1
- 229910001486 lithium perchlorate Inorganic materials 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
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- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 description 1
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Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/40—Nickelates
- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/04—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/40—Nickelates
- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
- C01G53/50—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [MnO2]n-, e.g. Li(NixMn1-x)O2, Li(MyNixMn1-x-y)O2
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- 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
- H01M4/36—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
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/50—Solid solutions
- C01P2002/52—Solid solutions containing elements as dopants
- C01P2002/54—Solid solutions containing elements as dopants one element only
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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Description
NiO+LiOH+1/4O2→LiNiO2+1/2H2O
8NiO+2LiOH+1/2O2→Li2Ni8O10+H2O
原料のニッケル化合物粉末には、公知技術の晶析法により作成したニッケル複合水酸化物の粉末を用いた。すなわち、2mol/Lの硫酸ナトリウム水溶液を貯めた反応槽に、ニッケルとコバルトの物質量のモル比が88:9となるように調製した硫酸ニッケルおよび硫酸コバルトの2mol/L混合水溶液と、1mol/Lアルミン酸ナトリウム水溶液とを、ニッケルとコバルトとアルミニウムの物質量のモル比が88:9:3となるような投入量で攪拌しつつ連続的に滴下した。並行して、反応槽内の溶液のアンモニア濃度が5g/Lとなるように28%アンモニア水を添加し、さらに反応槽内のpHが11.5~12.5となるように40%水酸化ナトリウム水溶液を添加した。この時、目的とするニッケル複合水酸化物の粒度が得られるように反応槽内のpHを上記の40%水酸化ナトリウム水溶液の添加量で微調整しながら反応を進めた。
実施例1と同様にして作成したニッケル複合水酸化物に対して、小型マッフル炉を用いて空気雰囲気中において焙焼温度400℃で5時間かけて焙焼し、ニッケル複合酸化物を生成した。得られたニッケル複合酸化物は体積平均粒径MVが11.8μmであり、炭素品位は0.21質量%であった。なお、無水水酸化リチウムには試料5と同じ平均粒径MV25.3μmのものを用いた。以降は実施例1と同様にして試料6のリチウムニッケル複合酸化物を合成し、実施例1と同様に電池特性の評価を行った。その結果、水洗処理前後のリチウムメタル比の比は0.950であり、初期放電容量は201.5mAh/g、正極抵抗の相対値は266であった。さらに小型マッフル炉を用いた焙焼時の焙焼温度を400℃に代えてそれぞれ500℃、650℃、700℃、および750℃にした以外は上記試料6の場合と同様にして試料7~10のリチウムニッケル複合酸化物を合成した。
実施例1と同様にして作成したニッケル複合水酸化物に対して、小型マッフル炉を用いて空気雰囲気中において焙焼温度650℃で5時間かけて焙焼し、ニッケル複合酸化物を生成した。得られたニッケル複合酸化物は体積平均粒径MVが11.6μmであり、炭素品位は0.066質量%であった。なお、無水水酸化リチウムには試料3と同じ平均粒径MV18.4μmのものを用いた。
2 ケース
2a 正極缶
2b 負極缶
2c ガスケット
3 電極
3a 正極
3b 負極
4 セパレータ
5 集電体
Claims (8)
- ニッケルとリチウムとを少なくとも含むリチウムイオン二次電池用正極活物質の製造方法であって、炭素含有量が0.042質量%以上0.25質量%以下で且つ体積平均粒径MVが10μm以上26μm以下のニッケル化合物粉末と体積平均粒径MVが10μm以上26μm以下(10μmを除く)のリチウム化合物粉末との混合物を焼成処理する焼成工程と、前記焼成工程で得たリチウムニッケル複合酸化物粉末を水洗処理する水洗工程と、前記水洗処理後のリチウムニッケル複合酸化物粉末中のリチウム以外の遷移金属の総物質量に対するリチウムの物質量の比を、前記水洗処理前のリチウムニッケル複合酸化物粉末中のリチウム以外の遷移金属の総物質量に対するリチウムの物質量の比で除した値が0.95を超えているか否かを判断する工程とを有し、
前記値が0.95以下の場合は、前記ニッケル化合物粉末に体積平均粒径MVがより小さいものを採用するか、前記ニッケル化合物粉末により高い温度で焙焼処理したものを用いるか、前記焼成処理時の雰囲気ガスの酸素濃度をより高くするか、前記焼成処理時の最高焼成温度をより高温にするか、又は前記最高焼成温度の保持時間をより長くすることで、前記値が0.95を超えるように前記焼成工程の条件の調整を行うことを特徴とするリチウムイオン二次電池用正極活物質の製造方法。 - 前記ニッケル化合物粉末がニッケル酸化物またはニッケル水酸化物の粉末である、請求項1に記載のリチウムイオン二次電池用正極活物質の製造方法。
- 前記リチウム化合物粉末が水酸化リチウムまたは水酸化リチウム水和物の粉末である、請求項1または2に記載のリチウムイオン二次電池用正極活物質の製造方法。
- 前記ニッケル化合物粉末と前記リチウム化合物粉末との混合物を焼成処理する際の雰囲気ガスの酸素濃度が60容量%以上である、請求項1から3のいずれか1項に記載のリチウムイオン二次電池用正極活物質の製造方法。
- 前記ニッケル化合物粉末が、ニッケルとその他遷移金属との複合酸化物または複合水酸化物の粉末を含む、請求項1から4のいずれか1項に記載のリチウムイオン二次電池用正極活物質の製造方法。
- 前記焼成工程における最高焼成温度が650℃以上850℃以下であり、かつ該最高焼成温度での保持時間が2時間以上である、請求項1~5のいずれか1項に記載のリチウムイオン二次電池用正極活物質の製造方法。
- 前記焼成工程の前に、前記ニッケル化合物粉末を焙焼温度500℃以上800℃以下で焙焼してニッケル酸化物粉末とする前処理工程を有する、請求項1~6のいずれか1項に記載のリチウムイオン二次電池用正極活物質の製造方法。
- 前記リチウムニッケル複合酸化物は、一般式LixNi1-y-zMyNzO2(式中、MはCoおよびMnの中からから選ばれた少なくとも1種の元素であり、NはAl、Ti、Nb、V、Mg、WおよびMoの中から選ばれた少なくとも1種の元素であり、xは0.90~1.10、yは0.05~0.35、Zは0.005~0.05である)で表される、請求項1~7のいずれか1項に記載のリチウムイオン二次電池用正極活物質の製造方法。
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