CN103700821A - Co、Mn包覆高镍层状LiNi0.92Co0.04Mn0.04O2锂电池正极材料的制备方法 - Google Patents
Co、Mn包覆高镍层状LiNi0.92Co0.04Mn0.04O2锂电池正极材料的制备方法 Download PDFInfo
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- CN103700821A CN103700821A CN201310699738.7A CN201310699738A CN103700821A CN 103700821 A CN103700821 A CN 103700821A CN 201310699738 A CN201310699738 A CN 201310699738A CN 103700821 A CN103700821 A CN 103700821A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 10
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 10
- 239000010406 cathode material Substances 0.000 title abstract description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title abstract 4
- 229910052759 nickel Inorganic materials 0.000 title abstract 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 239000002243 precursor Substances 0.000 claims abstract description 5
- 230000032683 aging Effects 0.000 claims abstract description 4
- 239000012153 distilled water Substances 0.000 claims abstract description 4
- 238000005245 sintering Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910013716 LiNi Inorganic materials 0.000 claims description 9
- 239000010405 anode material Substances 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000012423 maintenance Methods 0.000 claims description 3
- 239000011812 mixed powder Substances 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 2
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 abstract 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 239000000908 ammonium hydroxide Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium;hydroxide;hydrate Chemical compound [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 abstract 1
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(II) nitrate Inorganic materials [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 229910021508 nickel(II) hydroxide Inorganic materials 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 2
- 239000006258 conductive agent Substances 0.000 description 2
- 238000004519 manufacturing process 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
- 239000011888 foil Substances 0.000 description 1
- 239000002931 mesocarbon microbead Substances 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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- 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
-
- 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
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- 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
-
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
本发明涉及锂电池正极材料的制造，具体是一种Co、Mn包覆高镍层状LiNi0.92Co0.04Mn0.04O2锂电池正极材料的制备方法。该方法包括以下步骤：1）在反应釜中加入一定蒸馏水和球形Ni(OH)2；2）加入所需Co和Mn化学计量比的Co(NO3)2和Mn(NO3)2混合溶液；3）加入氨水与NaOH的混合溶液，调节pH为8-10；4）经陈化后，洗涤、干燥，获得经前驱体；5）前躯体与LiOH·H2O混合均匀；6）在窑炉中烧结，制得LiNi0.92Co0.04Mn0.04O2正极材料。本发明通过对三元正极材料进行表面包覆，能够提高材料表面的晶格稳定性，从而提高了高镍条件下三元正极材料的电池循环性。
Description
技术领域
本发明涉及锂电池正极材料的制造，具体是一种Co、Mn包覆高镍层状LiNi0.92Co0.04Mn0.04O2锂电池正极材料的制备方法。
背景技术
三元材料已经被广泛用于锂电池的正极材料，但现有的高镍三元正极材料存在着材料晶格稳定性差，电池循环性不好的缺陷，难兼顾高容量和高循环性的使用要求。
发明内容
本发明所要解决的技术问题是，提供一种电池循环性好的Co、Mn包覆高镍层状LiNi0.92Co0.04Mn0.04O2锂电池正极材料的制备方法。
本发明的Co、Mn包覆高镍层状LiNi0.92Co0.04Mn0.04O2锂电池正极材料的制备方法包括以下步骤：
1）在反应釜中加入一定蒸馏水和球形Ni(OH)2；
2）在50℃恒温条件下，搅拌，并加入所需Co和Mn化学计量比的Co(NO3)2和Mn(NO3)2混合溶液；
3）加入氨水与NaOH的混合溶液，调节反应釜中溶液的的pH，保持pH为8-10，使Co、Mn均匀沉淀到Ni(OH)2表面；
4）经陈化后，洗涤、干燥，获得经前驱体；
5）将上述制备的前躯体与LiOH·H2O按照1:1.03摩尔比混合均匀；
6）将混合粉末在窑炉中烧结，其温度制度为：500℃下保温5h，然后再700℃下保温12h；升温与降温速率都为2℃/min，制得LiNi0.92Co0.04Mn0.04O2正极材料。
本发明通过对三元正极材料进行表面包覆，能够提高材料表面的晶格稳定性，从而提高了高镍条件下三元正极材料的电池循环性；同时其生产工艺便于产业化，成本低，绿色无污染。
附图说明
图1是本发明实施例获得的正极材料制成电池在0.1C和0.5C下的循环性能曲线图。
具体实施方式
本发明实施例的方法包括以下步骤：
1）在反应釜中加入一定蒸馏水和球形Ni(OH)2；
2）在50℃恒温条件下，以500r/min搅拌，并加入所需Co和Mn化学计量比的Co(NO3)2和Mn(NO3)2混合溶液；
3）加入氨水与NaOH的混合溶液，调节反应釜中溶液的的pH，保持pH为8-10，使Co、Mn均匀沉淀到Ni(OH)2表面；
4）经陈化后，洗涤、干燥，获得经前驱体；
5）将上述制备的前躯体与LiOH·H2O按照1:1.03摩尔比混合均匀；
6）将混合粉末在窑炉中烧结，其温度制度为：500℃下保温5h，然后再700℃下保温12h；升温与降温速率都为2℃/min，制得LiNi0.92Co0.04Mn0.04O2正极材料。
对上述实施例获得的材料进行检测和试验：以制备的LiNi0.92Co0.04Mn0.04O2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，组装软包型电池。经检测其容量比传统三元正极材料克容量高出约20mAh/g，高达197mAh/g。循环性能优于普通三元正极材料（检测结果曲线如图1）。
Claims (1)
1.一种Co、Mn包覆高镍层状LiNi0.92Co0.04Mn0.04O2锂电池正极材料的制备方法，其特征是：包括以下步骤，
1）在反应釜中加入一定蒸馏水和球形Ni(OH)2；
2）在50℃恒温条件下，搅拌，并加入所需Co和Mn化学计量比的Co(NO3)2和Mn(NO3)2混合溶液；
3）加入氨水与NaOH的混合溶液，调节反应釜中溶液的的pH，保持pH为8-10，使Co、Mn均匀沉淀到Ni(OH)2表面；
4）经陈化后，洗涤、干燥，获得经前驱体；
5）将上述制备的前躯体与LiOH·H2O按照1:1.03摩尔比混合均匀；
6）将混合粉末在窑炉中烧结，其温度制度为：500℃下保温5h，然后再700℃下保温12h；升温与降温速率都为2℃/min，制得LiNi0.92Co0.04Mn0.04O2正极材料。
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104319391A (zh) * | 2014-10-08 | 2015-01-28 | 赣州腾远钴业有限公司 | 一种锂电池用高镍低钴低锰三元正极材料前驱体的制备方法 |
| CN105390691A (zh) * | 2015-10-23 | 2016-03-09 | 赣州市芯隆新能源材料有限公司 | 一种液相模板法制备球形镍钴锰酸锂的方法 |
| CN105789616A (zh) * | 2014-12-22 | 2016-07-20 | 深圳市格林美高新技术股份有限公司 | 修复镍钴锰三元电池材料前驱体的方法 |
| CN108091927A (zh) * | 2017-12-13 | 2018-05-29 | 桑顿新能源科技有限公司 | 一种高安全、长循环寿命的锂离子电池及其制备方法 |
| CN109455773A (zh) * | 2018-11-30 | 2019-03-12 | 上海电力学院 | 一种锂离子电池高镍三元正极材料及其制备方法 |
| CN110140242A (zh) * | 2016-12-28 | 2019-08-16 | 株式会社Lg化学 | 二次电池用正极活性材料、其制造方法、包含其的二次电池用正极以及包含其的二次电池 |
| KR20210052375A (ko) * | 2019-10-31 | 2021-05-10 | 한양대학교 에리카산학협력단 | 양이온 교환 반응을 이용하여 제조된 양극 활물질, 및 그 제조 방법 |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104319391B (zh) * | 2014-10-08 | 2016-09-07 | 赣州腾远钴业有限公司 | 一种锂电池用高镍低钴低锰三元正极材料前驱体的制备方法 |
| CN104319391A (zh) * | 2014-10-08 | 2015-01-28 | 赣州腾远钴业有限公司 | 一种锂电池用高镍低钴低锰三元正极材料前驱体的制备方法 |
| CN105789616A (zh) * | 2014-12-22 | 2016-07-20 | 深圳市格林美高新技术股份有限公司 | 修复镍钴锰三元电池材料前驱体的方法 |
| CN105789616B (zh) * | 2014-12-22 | 2019-03-08 | 深圳市格林美高新技术股份有限公司 | 修复镍钴锰三元电池材料前驱体的方法 |
| CN105390691A (zh) * | 2015-10-23 | 2016-03-09 | 赣州市芯隆新能源材料有限公司 | 一种液相模板法制备球形镍钴锰酸锂的方法 |
| CN110140242B (zh) * | 2016-12-28 | 2022-05-27 | 株式会社Lg化学 | 二次电池用正极活性材料、其制造方法、包含其的二次电池用正极以及包含其的二次电池 |
| CN110140242A (zh) * | 2016-12-28 | 2019-08-16 | 株式会社Lg化学 | 二次电池用正极活性材料、其制造方法、包含其的二次电池用正极以及包含其的二次电池 |
| CN108091927A (zh) * | 2017-12-13 | 2018-05-29 | 桑顿新能源科技有限公司 | 一种高安全、长循环寿命的锂离子电池及其制备方法 |
| CN109455773A (zh) * | 2018-11-30 | 2019-03-12 | 上海电力学院 | 一种锂离子电池高镍三元正极材料及其制备方法 |
| CN109455773B (zh) * | 2018-11-30 | 2021-07-20 | 上海电力学院 | 一种锂离子电池高镍三元正极材料及其制备方法 |
| KR20210052375A (ko) * | 2019-10-31 | 2021-05-10 | 한양대학교 에리카산학협력단 | 양이온 교환 반응을 이용하여 제조된 양극 활물질, 및 그 제조 방법 |
| KR102479179B1 (ko) * | 2019-10-31 | 2022-12-20 | 한양대학교 에리카산학협력단 | 양이온 교환 반응을 이용하여 제조된 양극 활물질, 및 그 제조 방법 |
| KR20230002191A (ko) * | 2019-10-31 | 2023-01-05 | 한양대학교 에리카산학협력단 | 양이온 교환 반응을 이용하여 제조된 양극 활물질, 및 그 제조 방법 |
| KR102565290B1 (ko) * | 2019-10-31 | 2023-08-09 | 한양대학교 에리카산학협력단 | 양이온 교환 반응을 이용하여 제조된 양극 활물질, 및 그 제조 방법 |
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