CN104733722A - La掺杂Ti包覆三元正极材料的制备方法 - Google Patents
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- 239000010406 cathode material Substances 0.000 title claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 title abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 235000019441 ethanol Nutrition 0.000 claims abstract description 7
- 239000002243 precursor Substances 0.000 claims abstract description 7
- 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 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000000967 suction filtration Methods 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 7
- 239000007795 chemical reaction product Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000000975 co-precipitation Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 3
- 238000009413 insulation Methods 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
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 2
- 238000009790 rate-determining step (RDS) Methods 0.000 claims description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 6
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 6
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- 239000010936 titanium Substances 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000000605 extraction Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 abstract 1
- 239000010405 anode material Substances 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 2
- 239000006258 conductive agent Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910001290 LiPF6 Inorganic materials 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
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- 239000002931 mesocarbon microbead Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- -1 polyethylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
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- 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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- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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Abstract
本发明涉及一种锂离子电池正极材料的制造方法，具体是一种La掺杂Ti包覆三元正极材料的制备方法。该方法包括以下步骤：1）制备三元前驱体；2）制备三元正极材料；3）将三元正极材料和La2O3混合；4）将混合好的物料二次烧结；5）再将步骤4）得到的物料加入酒精进行分散；6）将异丙醇钛加入无水乙醇中使其完全溶解；再将其加入步骤5）获得的混合液中混合均匀，抽滤，干燥；7）将干燥后的原料烧结；将其粉碎得到最终产物。本发明通过La掺杂和Ti包覆使三元正极材料的倍率性能和循环性能显著提高，可得到低成本、高性能的锂离子电池正极材料。
Description
技术领域
本发明涉及一种锂离子电池正极材料的制造方法，具体是一种La掺杂Ti包覆三元正极材料的制备方法。
背景技术
三元正极材料Li(Ni0.45Co0.2Mn0.35)O2作为锂离子电池正极材料，具有价格低、放电比容量高、循环稳定等特点。但现有三元正极材料存在着倍率性能和循环性能不佳的缺陷。
发明内容
本发明所要解决的技术问题是，提供一种能够提高三元正极材料的倍率性能和循环性能的La掺杂Ti包覆三元正极材料的制备方法。
本发明的La掺杂Ti包覆三元正极材料的制备方法包括以下步骤：
1)采用常规的氢氧化物共沉淀法制备三元前驱体(Ni0.45Co0.2Mn0.35)(OH)2；
2)将步骤1)所制备的三元前驱体(Ni0.45Co0.2Mn0.35)(OH)2，电池级碳酸锂，按照1:1.04的摩尔比例混合烧结得到三元正极材料Li(Ni0.45Co0.2Mn0.35)O2；将其粉碎；
3)将三元正极材料Li(Ni0.45Co0.2Mn0.35)O2和La2O3在三维混料罐中混合，其中La的重量占混合后总质量的0.02－0.03％；
4)将混合好的物料放置于空气气氛马弗炉内二次烧结；烧结过程是以3-5℃/min的升温速率升到800-900℃，保温8－12h，随炉冷却，取出；粉碎；
5)再将步骤4)得到的物料加入酒精进行分散，物料占酒精质量的3/4；
6)称取一定质量的异丙醇钛加入无水乙醇中搅拌使其完全溶解；再将其加入步骤5)获得的混合液中混合均匀，用抽滤装置抽滤，将抽滤后的物料干燥；
7)将已上一步干燥后的原料置于空气气氛马弗炉内烧结；烧结过程是在500－600℃烧8－10h后随炉自然冷却，取出；将其粉碎得到最终产物；通过控制步骤6)中异丙醇钛的加入量，使TiO2包覆量为最终产物质量的3％-5％。
本发明通过La掺杂和Ti包覆使三元正极材料的倍率性能和循环性能显著提高，可得到低成本、高性能的锂离子电池正极材料。
具体实施方式
本发明实施例步骤如下：
1)采用常规的氢氧化物共沉淀法制备三元前驱体(Ni0.45Co0.2Mn0.35)(OH)2；
2)将步骤1)所制备的三元前驱体(Ni0.45Co0.2Mn0.35)(OH)2，电池级碳酸锂，按照1:1.04的摩尔比例混合烧结得到三元正极材料Li(Ni0.45Co0.2Mn0.35)O2
3)将已混好的原料置于空气气氛马弗炉内烧结，先在620℃的预烧6h；再在900℃烧结12h；随炉自然冷却，取出；将其粉碎后过200目筛网；
4)将Li(Ni0.45Co0.2Mn0.35)O2和La2O3在三维混料罐中混合4h，球：料＝1.5:1，其中La的质量占混合后材料总质量的0.03％。
5)将混合好的物料放置于空气气氛马弗炉内二次烧结，以4℃/min的升温速率升到900℃，保温10h，随炉冷却，取出；将其粉碎后过200目筛网；
6)再将步骤5)中物料加入酒精进行分散，物料占酒精质量的3/4；
7)称取一定质量的异丙醇钛加入无水乙醇中搅拌使其完全溶解；再将其加入步骤6)获得的混合液中，搅拌3h；搅拌结束后用抽滤装置抽滤，将抽滤后的物料在110℃下干燥10h；
8)将已干燥的原料置于空气气氛马弗炉内烧结，在500－600℃的预烧8－10h；随炉自然冷却，取出；将其粉碎后过200目筛网；最终产物的TiO2包覆量为最终产物质量的4％。
对本发明实施例制备的材料进行测试：
以该实施例制备的材料为正极活性物质，乙炔黑为导电剂，聚偏氟乙烯为粘结剂，三者质量比为90：4：6，加入N-甲基吡咯烷酮，混合均匀制成浆料，涂于铝箔集流体上，制成电池的正极。以MCMB为负极活性物质，导电剂、粘结剂同上，质量比不变，制成浆料后涂于铜箔集流体上，得到电池的负极。采用1mol/L的LiPF6/EC+DMC+DEC(体积比为1：l：1)电解液，聚乙烯薄膜，在流动干燥空气的手套箱中，组装纽扣电池。经检测其容量比改性前高出约15mAh/g，高达188mAh/g。循环性能优于普通三元正极材料。
其全电池倍率数据如下表：
从上表可以看出，掺杂包覆改性后的材料在1C的放电倍率平均为96.1％，2C放电倍率平均为92.6％。
Claims (3)
1.一种La掺杂Ti包覆三元正极材料的制备方法，其特征是：包括以下步骤，
1）采用常规的氢氧化物共沉淀法制备三元前驱体(Ni0.45Co0.2Mn0.35)(OH)2 ；
2）将步骤1）所制备的三元前驱体(Ni0.45Co0.2Mn0.35)(OH)2，电池级碳酸锂，按照1:1.04 的摩尔比例混合烧结得到三元正极材料Li（Ni0.45Co0.2Mn0.35）O2；将其粉碎；
3）将三元正极材料Li（Ni0.45Co0.2Mn0.35）O2和La2O3在三维混料罐中混合，其中La的重量占混合后总质量的0.02－0.03%；
4）将混合好的物料放置于空气气氛马弗炉内二次烧结；取出粉碎；
5）再将步骤4）得到的物料加入酒精进行分散，物料占酒精质量的3/4；
6）称取一定质量的异丙醇钛加入无水乙醇中搅拌使其完全溶解；再将其加入步骤5）获得的混合液中混合均匀，用抽滤装置抽滤，将抽滤后的物料干燥；
7）将已上一步干燥后的原料置于空气气氛马弗炉内烧结；将其粉碎得到最终产物；通过控制步骤6）中异丙醇钛的加入量，使TiO2包覆量为最终产物质量的3%-5%。
2.根据权利要求1所述的La掺杂Ti包覆三元正极材料的制备方法，其特征是：步骤4）中烧结过程是以3-5℃ /min 的升温速率升到800-900℃，保温8 － 12h ，随炉冷却。
3.根据权利要求1所述的La掺杂Ti包覆三元正极材料的制备方法，其特征是：步骤7）中烧结过程是在500 － 600℃烧8－ 10h 后随炉自然冷却。
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Cited By (5)
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| CN105355887A (zh) * | 2015-11-28 | 2016-02-24 | 中信大锰矿业有限责任公司大新锰矿分公司 | 一种氧化镁包覆镍钴锰酸锂正极材料的制备方法 |
| CN105680015A (zh) * | 2016-01-28 | 2016-06-15 | 深圳大学 | 一种在三元材料表面包覆氧化镧的正极材料及其制备方法 |
| CN107516731A (zh) * | 2017-07-18 | 2017-12-26 | 南京创源天地动力科技有限公司 | 改性锂离子电池正极材料及其制备方法以及使用改性锂离子电池正极材料的电化学储能装置 |
| CN111106343A (zh) * | 2019-12-30 | 2020-05-05 | 华南理工大学 | 一种镧、氟共掺杂的高镍三元正极材料及其制备方法与应用 |
| CN114560512A (zh) * | 2022-02-23 | 2022-05-31 | 浙江格派钴业新材料有限公司 | 一种利用共沉淀法实现Ti/La共包覆NCM高镍三元前驱体的制备方法 |
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