JP2023505390A - 炭素被覆リチウムリッチ酸化物複合材料及びその製造方法 - Google Patents
炭素被覆リチウムリッチ酸化物複合材料及びその製造方法 Download PDFInfo
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 114
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 114
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 67
- 239000002131 composite material Substances 0.000 title claims abstract description 38
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 238000005245 sintering Methods 0.000 claims abstract description 69
- 238000000034 method Methods 0.000 claims abstract description 51
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 43
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 20
- 239000010941 cobalt Substances 0.000 claims abstract description 20
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052742 iron Inorganic materials 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000010298 pulverizing process Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 24
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 10
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 6
- 239000002041 carbon nanotube Substances 0.000 claims description 5
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 5
- 239000003273 ketjen black Substances 0.000 claims description 5
- 229910000428 cobalt oxide Inorganic materials 0.000 claims description 4
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 4
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims description 4
- 229910001947 lithium oxide Inorganic materials 0.000 claims description 4
- -1 triiron tetraoxide Chemical compound 0.000 claims description 4
- 239000002028 Biomass Substances 0.000 claims description 3
- CUPCBVUMRUSXIU-UHFFFAOYSA-N [Fe].OOO Chemical compound [Fe].OOO CUPCBVUMRUSXIU-UHFFFAOYSA-N 0.000 claims description 3
- 239000006230 acetylene black Substances 0.000 claims description 3
- 239000002134 carbon nanofiber Substances 0.000 claims description 3
- 239000003245 coal Substances 0.000 claims description 3
- 229910021446 cobalt carbonate Inorganic materials 0.000 claims description 3
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 3
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 3
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 3
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims description 3
- 229940044175 cobalt sulfate Drugs 0.000 claims description 3
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 3
- ZOTKGJBKKKVBJZ-UHFFFAOYSA-L cobalt(2+);carbonate Chemical compound [Co+2].[O-]C([O-])=O ZOTKGJBKKKVBJZ-UHFFFAOYSA-L 0.000 claims description 3
- PQVSTLUFSYVLTO-UHFFFAOYSA-N ethyl n-ethoxycarbonylcarbamate Chemical compound CCOC(=O)NC(=O)OCC PQVSTLUFSYVLTO-UHFFFAOYSA-N 0.000 claims description 3
- 229910021389 graphene Inorganic materials 0.000 claims description 3
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims description 3
- NPFOYSMITVOQOS-UHFFFAOYSA-K iron(III) citrate Chemical compound [Fe+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NPFOYSMITVOQOS-UHFFFAOYSA-K 0.000 claims description 3
- 229910021519 iron(III) oxide-hydroxide Inorganic materials 0.000 claims description 3
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 3
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 3
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium hydroxide monohydrate Substances [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 claims description 3
- 229940040692 lithium hydroxide monohydrate Drugs 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 10
- 229910010648 Li6CoO4 Inorganic materials 0.000 abstract description 3
- 239000000654 additive Substances 0.000 abstract description 3
- 230000007812 deficiency Effects 0.000 abstract description 3
- 229910010699 Li5FeO4 Inorganic materials 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 229910001873 dinitrogen Inorganic materials 0.000 description 12
- 239000006245 Carbon black Super-P Substances 0.000 description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
- 229910001416 lithium ion Inorganic materials 0.000 description 5
- 239000007774 positive electrode material Substances 0.000 description 5
- 229910018068 Li 2 O Inorganic materials 0.000 description 4
- 230000002427 irreversible effect Effects 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical group [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 2
- 239000010406 cathode material Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 229910013870 LiPF 6 Inorganic materials 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 230000000996 additive effect Effects 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
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
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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
- H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
-
- 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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
-
- 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
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/0018—Mixed oxides or hydroxides
- C01G49/0027—Mixed oxides or hydroxides containing one alkali metal
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/40—Cobaltates
- C01G51/42—Cobaltates containing alkali metals, e.g. LiCoO2
-
- H—ELECTRICITY
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- 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
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- H—ELECTRICITY
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- 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
-
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- 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
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Abstract
Description
本願は、2020年7月9日に出願された中国特許出願第202010657297.4号の優先権を主張し、当該出願の内容は、参照により本明細書に組み込まれる。
鉄源又はコバルト源をリチウム源と混合し、焼結した後にリチウムリッチ酸化物Li5FeO4又はLi6CoO4を得るステップであって、前記リチウム源と前記鉄源のモル比が5~25:1であり、前記リチウム源と前記コバルト源のモル比が6~30:1であるステップ(1)と、
ステップ(1)で得られたリチウムリッチ酸化物を粉砕するステップ(2)と、
ステップ(2)で粉砕されたリチウムリッチ酸化物を炭素源と混合し、焼結した後に炭素被覆リチウムリッチ酸化物複合材料を得るステップ(3)と、を含む、炭素被覆リチウムリッチ酸化物複合材料を製造する方法が提供される。
鉄源又はコバルト源をリチウム源と混合し、焼結した後にリチウムリッチ酸化物Li5FeO4又はLi6CoO4を得るステップであって、前記リチウム源と前記鉄源のモル比が5~25:1であり、前記リチウム源と前記コバルト源のモル比が6~30:1であるステップ(1)と、
ステップ(1)で得られたリチウムリッチ酸化物を粉砕するステップ(2)と、
ステップ(2)で粉砕されたリチウムリッチ酸化物を炭素源と混合し、焼結した後に炭素被覆リチウムリッチ酸化物複合材料を得るステップ(3)と、を含む、炭素被覆リチウムリッチ酸化物複合材料を製造する方法が提供される。
(実施例1)
(実施例2)
(実施例3)
(比較例1)
(実施例4)
(実施例5)
(実施例6)
(比較例2)
(試験例)
Claims (10)
- 鉄源又はコバルト源をリチウム源と混合し、焼結した後にリチウムリッチ酸化物Li5FeO4又はLi6CoO4を得るステップであって、前記リチウム源と前記鉄源のモル比が5~25:1であり、前記リチウム源と前記コバルト源のモル比が6~30:1であるステップ(1)と、
ステップ(1)で得られたリチウムリッチ酸化物を粉砕するステップ(2)と、
ステップ(2)で粉砕されたリチウムリッチ酸化物を炭素源と混合し、焼結した後に炭素被覆リチウムリッチ酸化物複合材料を得るステップ(3)と、を含むことを特徴とする、
炭素被覆リチウムリッチ酸化物複合材料を製造する方法。 - ステップ(1)において、前記鉄源は、三酸化二鉄、四酸化三鉄、オキシ水酸化鉄、硝酸鉄及びクエン酸鉄のうちの1種又は複数種であることを特徴とする、
請求項1に記載の方法。 - ステップ(1)において、前記コバルト源は、酸化コバルト、四酸化三コバルト、炭酸コバルト、硫酸コバルト、塩化コバルト及び硝酸コバルトのうちの1種又は複数種であることを特徴とする、
請求項1に記載の方法。 - ステップ(1)において、前記リチウム源は、炭酸リチウム、水酸化リチウム一水和物、無水水酸化リチウム及び酸化リチウムのうちの1種又は複数種であることを特徴とする、
請求項1に記載の方法。 - ステップ(1)において、前記焼結過程は、鉄源又はコバルト源とリチウム源の混合物を焼結炉に入れ、不活性ガスの条件下で、所定の第1昇温速度で第1焼結温度まで昇温させて焼結を行うステップを含み、
好ましくは、前記所定の第1昇温速度は、1~10℃/minであり、
好ましくは、前記第1焼結温度は、500~1000℃であり、第1焼結時間は、3~60hであることを特徴とする、
請求項1に記載の方法。 - ステップ(2)において、前記リチウムリッチ酸化物を、平均粒径が2~50μmになるまで粉砕することを特徴とする、
請求項1に記載の方法。 - ステップ(3)において、前記炭素源は、導電性カーボンブラック、ケッチェンブラック、カーボンナノチューブ、アセチレンブラック、気相成長炭素繊維、グラフェン及びバイオマス炭のうちの1種又は複数種であることを特徴とする、
請求項1に記載の方法。 - ステップ(3)において、リチウムリッチ酸化物と炭素源の総重量を基準として、前記炭素源が占める割合は、0.5~10重量%であることを特徴とする、
請求項1に記載の方法。 - ステップ(3)において、前記焼結過程は、粉砕されたリチウムリッチ酸化物と炭素源を均一に混合した後、不活性ガスの条件下で、所定の第2昇温速度で第2焼結温度まで昇温させて焼結を行うステップを含み、
好ましくは、前記所定の第2昇温速度は、1~10℃/minであり、
好ましくは、前記第2焼結温度は、200~600℃であり、第2焼結時間は、2~20hであることを特徴とする、
請求項1に記載の方法。 - 請求項1~9のいずれか一項に記載の方法により製造された炭素被覆リチウムリッチ酸化物複合材料であって、当該炭素被覆リチウムリッチ酸化物複合材料は、炭素層と、炭素層で被覆されたリチウムリッチ酸化物とを含み、前記リチウムリッチ酸化物は、Li5FeO4又はLi6CoO4であることを特徴とする、
炭素被覆リチウムリッチ酸化物複合材料。
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CN202010657297.4A CN111725576B (zh) | 2020-07-09 | 2020-07-09 | 一种碳包覆富锂氧化物复合材料及其制备方法 |
CN202010657297.4 | 2020-07-09 | ||
PCT/CN2020/104574 WO2022007021A1 (zh) | 2020-07-09 | 2020-07-24 | 一种碳包覆富锂氧化物复合材料及其制备方法 |
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WO2024098198A1 (zh) * | 2022-11-07 | 2024-05-16 | 宁德时代新能源科技股份有限公司 | 包覆型富锂金属氧化物材料及制备方法、测定包覆型富锂金属氧化物材料中包覆层的方法、正极极片、电池及用电装置 |
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CN116632220A (zh) * | 2023-07-21 | 2023-08-22 | 宁德时代新能源科技股份有限公司 | 补钠材料及其制备方法、正极极片、电极组件、电池和用电装置 |
CN116789191B (zh) * | 2023-07-25 | 2024-01-12 | 宁德时代新能源科技股份有限公司 | 补钠材料及其制备方法、正极极片、电极组件、电池和用电装置 |
CN117497743A (zh) * | 2023-11-01 | 2024-02-02 | 湖南沃尔顿新能源科技有限公司 | 一种动力电池正极材料及其制备方法 |
CN117558922B (zh) * | 2024-01-12 | 2024-03-29 | 紫金矿业新能源新材料科技(长沙)有限公司 | 富锂铁酸锂补锂材料及其制备方法 |
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