CN100376048C - 锂离子二次电池正极材料LiCoxMn2-xO4的合成方法 - Google Patents
锂离子二次电池正极材料LiCoxMn2-xO4的合成方法 Download PDFInfo
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- 239000010405 anode material Substances 0.000 title claims abstract description 19
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title abstract description 13
- 229910011293 LiCoxMn2-xO4 Inorganic materials 0.000 title abstract 2
- 229910011369 LiCoxMn2−xO4 Inorganic materials 0.000 title abstract 2
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- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 8
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- 238000000227 grinding Methods 0.000 description 3
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 description 2
- 239000007774 positive electrode material Substances 0.000 description 2
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910012820 LiCoO Inorganic materials 0.000 description 1
- 229910011297 LiCox Inorganic materials 0.000 description 1
- 229910014127 LiMn2 O4 -LiMn2 O4 Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
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- TYTHZVVGVFAQHF-UHFFFAOYSA-N manganese(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Mn+3].[Mn+3] TYTHZVVGVFAQHF-UHFFFAOYSA-N 0.000 description 1
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- C01G45/1242—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type [Mn2O4]-, e.g. LiMn2O4, Li[MxMn2-x]O4
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Abstract
本发明涉及锂离子二次电池正极材料领域，是一种锂离子二次电池正极材料LiCoxMn2-xO4的合成方法，针对尖晶石锰酸锂LiMn2O4循环性能较差而设计的。其要点是包括溶解、沉淀、烘干、煅烧、包覆、混合、高温烧结等步骤。先制备球形的Mn2O3，然后在球形的Mn2O3表面形成一钴酸锂LiCoO2薄层，再与锂化合物进行混合，用锂化合物与包钴后的Mn2O3按Li∶(Co+Mn)＝1∶2(原子比)的比例进行充分混合；混合物装入坩埚中，置于流动的空气中400-550℃预处理8-12小时；冷却后研磨，然后再置于700-850℃保温24-48小时。通过高温反应而制成符合锂离子二次电池所用的正极材料，提高其循环性能。
Description
技术领域
本发明涉及锂离子二次电池正极材料领域，而且还包含对合成LiCoxMn2-xO4时所用的锰源前驱体进行的化学处理，属于化学工业材料领域。
背景技术
作为锂二次电池正极材料，目前使用最多的是钴酸锂LiCoO2，但由于钴资源贫乏且对环境有污染；而尖晶石锰酸锂LiMn2O4由于锰资源丰富，低污染以及较高的性价比，被认为是继钴酸锂LiCoO2以后的首选正极材料，但由于其循环性能较差，也制约了其商品化进程。尽管合成尖晶石锰酸锂LiMn2O4的方法很多，同时也有一些性能较好的产品，但总存在一些问题没有较好地解决；常用的方法是掺杂其它金属元素，如钴、铬、镁等来提高其循环性能，但是直接用机械方法进行掺杂达不到掺杂均匀的目的。当选择锰源时却没有用常规的二氧化锰，而是选取通过一定的工艺制取的球形Mn2O3，然后对之进行包钴达到掺杂均匀的目的，再与LiOH-H2O充分混合，用这种方法所合成的产物循环性能优越，这是其它方法不能比拟的。
发明内容
本发明将向本领域提供一种锂离子二次电池正极材料LiCoxMn2-xO4的合成方法，这种合成方法通过化学方法先制备球形Mn2O3，然后在球形的Mn2O3表面包覆一层钴化合物，该层钴化合物在空气中于400～550℃预处理8～12小时，在球形的Mn2O3表面形成一钴酸锂LiCoO2薄层，预处理目的是使钴化合物结构稳定。由于钴酸锂LiCoO2具有较高的容量及较好的循环性能，从而解决了尖晶石锰酸锂LiMn2O4循环性能较差的问题。尔后将锂化合物与包覆钴的Mn2O3按Li∶Co+Mn＝1∶2原子比例进行充分混合；PH值控制在8.5-11.0之间；混合物装入坩埚中，冷却后研磨，于700～850℃保温24～48小时。
所述的合成方法在于金属锰片用酸溶解，然后用沉淀剂NH4HCO3进行沉淀，PH值控制在6～10之间，其产物MnCO3的粒度控制在10～25微米。
所述的合成方法在于锰片经溶解，沉淀、热处理后所得产物是球形Mn2O3。
所述的合成方法在于掺杂钴时采用对锰化合物Mn2O3进行表面包钴后再与锂化合物混合。
所述的合成方法在于锂化合物为LiOH-H2O或LiNO3。
本发明中的球形Mn2O3须保证包覆的均匀性，因为掺杂物的量较少，如果不均匀就不能达到通过掺杂稳定LiMn2O4结构，从而改善其循环性能的目的；而且在制备MnCO3时的PH值及粒度控制、Mn2O3的粒度以及包钴时的PH值也很必要；同时对LiOH-H2O的前期处理以及热处理时的预处理对提高掺杂的均匀度也有一定的帮助。
本发明的步骤是：
1)金属锰片先用酸(盐酸、硫酸、硝酸中的一种或两种)溶解，溶解后的溶液并控制其酸度和摩尔浓度，然后才能用沉淀剂(一种可溶性碳酸盐，如NH4HCO3)进行沉淀，控制沉淀时的PH值6-10，同时也要控制沉淀物MnCO3的粒度大小，粒度控制在10-25微米；
2)对沉淀物MnCO3进行热处理得到球形的Mn2O3，温度的400-800℃；3)对球形的Mn2O3进行钴包覆，PH值8.5-12.0，Co∶Mn＝x∶(2-x)(原子比)；4)包覆后的产物经烘干后与锂化合物按Li∶(Co+Mn)＝1∶2(原子比)进行充分混合均匀，再在空气中于400-700℃预处理8-12小时，然后再于700-850℃保温24-48小时。用锂化合物与包钴后的Mn2O3按Li∶(Co+Mn)＝1∶2(原子比)的比例进行充分混合，PH值控制在8.5-11.0之间；混合物装入坩埚中，置于流动的空气中400-550℃预处理8-12小时；冷却后研磨，然后再置于700-850℃保温24-48小时。所述的锂离子二次电池正极材料LiCoxMn2-xO4的合成方法，其特征在于：MnCO3经热处理后的产物Mn2O3呈球形，这样才能保证其包钴时的均匀程度，PH值控制在8.5-11.0之间。
所述的锂离子二次电池正极材料LiCoxMn2-xO4的合成方法，锰源为直接用锰片溶解，经沉淀、热处理后所得的Mn2O3，而不是常用的二氧化锰。
所述的锂离子二次电池正极材料LiCoxMn2-xO4的合成方法，掺杂钴时不是直接用钴化合物与锂化合物、锰化合物进行机械混合，而是对锰化合物(Mn2O3)进行包钴后再与锂化合物混合。
所述的锂离子二次电池正极材料LiCoxMn2-xO4的合成方法，锂化合物为LiOH-H2O或LiNO3，考虑环境因素，首选LiOH-H2O，而且为保证混合均匀，对LiOH-H2O要作前期处理，即对粒度要有一定的要求。
这种锂离子二次电池正极材料，具有结晶度好，资源丰富，循环性能优良等特点，将替代价格昂贵的钴酸锂合成的产品，加快其产业化的进程。
附图说明
图1至图4是用本方法生产的产品比容量与循环次数曲线图。虽然用这种方法生产的产品比容量比其它方法小几个单位，但是循环性能却有明显的改善，而且循环性能不好正是制约钴酸锂实现产业化的根本原因；基于这一目的对传统的制备方法进行必要的改进，从而提高锂离子二次电池正极材料LiCoxMn2-xO4的合成方法的综合性能，加快其产业化的进程。
具体实施方式
对下述几种不同的方法所制得的正极材料直接做成电池进行电性能测试，电池正极所用材料组成为：80-90％正极活性物质+10-15％导电剂乙炔黑+5-10％的粘结剂聚四氟乙烯PTFE；电池负极为石墨；电解液为1MliPF6的1：1EC+DEC；隔膜纸为Cellgard2400微孔薄膜。
实施例1
将LiOH-H2O与二氧化锰按Li∶Mn＝1∶2(原子比)的比例进行混合，混合物装入坩埚中，置于流动的空气中450℃预处理9小时，冷却后研磨，然后再于800℃保温30小时，将产物研磨过筛后按前述比例制成电池进行充放电测试，电压范围为4.20-3.15V，充放电倍率为0.5C，如图1比容量(mAh/g)与循环次数所示的曲线。
实施例2
将LiOH-H2O、电解二氧化锰(EMD)及Co3O4按Li∶Mn∶Co＝1∶(2-x)∶x(原子比)的比例混合，混合物装入坩埚中，于流动的空气中450℃预处理9小时，冷却后研磨，然后再置于800℃保温30小时，将产物研磨过筛后按前述比例制成电池进行充放电测试，电压范围为4.20-3.15V，充放电倍率为0.5C，如图2比容量(mAh/g)与循环次数所示的曲线。
实施例3
将LiOH-H2O、三氧化二锰(Mn2O3)及Co3O4按Li∶Mn∶Co＝1∶(2-x)∶x(原子比)的比例混合，混合物装入坩埚中，于流动的空气中450℃预处理9小时，冷却后研磨，然后再置于800℃保温30小时，将产物研磨过筛后按前述比例制成电池进行充放电测试，电压范围为4.20-3.15V，充放电倍率为0.5C，如图3比容量(mAh/g)与循环次数所示的曲线。
实施例4
将LiOH-H2O、包覆钴(Co)后的三氧化二锰(Mn2O3)按Li∶(Mn+Co)＝1∶2(原子比)的比例混合，混合物装入坩埚中，于流动的空气中450℃预处理9小时，冷却后研磨，然后再置于800℃保温30小时，将产物研磨过筛后按前述比例制成电池进行充放电测试，电压范围为4.20-3.15V，充放电倍率为0.5C，如图4比容量(mAh/g)与循环次数所示的曲线。
Claims (5)
1.一种锂离子二次电池正极材料LiCoxMn2-xO4的合成方法，这种合成方法的特征在于先制备球形的Mn2O3，然后在球形的Mn2O3表面包覆一层钴化合物，该层钴化合物在空气中于400～550℃预处理8～12小时，在球形的Mn2O3表面形成一钴酸锂LiCoO2薄层，将锂化合物与包覆钴的Mn2O3按Li∶Co+Mn＝1∶2原子比例进行充分混合；冷却后研磨，于700～850℃保温24～48小时。
2.根据权利要求1所述的锂离子二次电池正极材料LiCoxMn2-xO4的合成方法，其特征在于金属锰片用酸溶解，然后用沉淀剂NH4HCO3进行沉淀，PH值控制在6～10之间，其产物MnCO3的粒度控制在10～25微米。
3.根据权利要求1所述的锂离子二次电池正极材料LiCoxMn2-xO4的合成方法，其特征在于锰片经溶解，沉淀、热处理后所得产物是球形Mn2O3。
4.根据权利要求1所述的锂离子二次电池正极材料LiCoxMn2-xO4的合成方法，其特征在于掺杂钴时采用对锰化合物Mn2O3进行表面包钴后再与锂化合物混合。
5.根据权利要求1所述的锂离子二次电池正极材料LiCoxMn2-xO4的合成方法，其特征在于锂化合物为LiOH-H2O或LiNO3。
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| CN103035904B (zh) * | 2012-12-21 | 2015-03-04 | 浙江工业大学 | 一种改性锰酸锂材料及其制备方法和应用 |
| TWI622211B (zh) * | 2013-02-14 | 2018-04-21 | Ｌｇ化學股份有限公司 | 用於鋰二次電池之陰極及包含彼之鋰二次電池 |
| CN104064743B (zh) * | 2013-03-19 | 2016-04-06 | 南通瑞翔新材料有限公司 | 一种锂电池锰基正极材料的制备方法 |
| CN108682809A (zh) * | 2018-05-07 | 2018-10-19 | 新乡学院 | 一种改性锂离子电池正极材料及其制备方法 |
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| US5866279A (en) * | 1996-03-19 | 1999-02-02 | Mitsubishi Chemical Corporation | Nonaqueous electrolyte secondary cell |
| JP2001163622A (ja) * | 1999-10-01 | 2001-06-19 | Tosoh Corp | リチウムマンガン酸化物およびその製造方法、並びにこれを用いた二次電池 |
| JP2002075355A (ja) * | 2000-08-23 | 2002-03-15 | Chisso Corp | 有機電解液二次電池用正極活物質、その製造方法およびそれを用いた有機電解液二次電池 |
| CN1416189A (zh) * | 2001-11-02 | 2003-05-07 | 中国科学院物理研究所 | 以纳米表面包覆复合材料为正极活性物质的锂二次电池 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US5866279A (en) * | 1996-03-19 | 1999-02-02 | Mitsubishi Chemical Corporation | Nonaqueous electrolyte secondary cell |
| JP2001163622A (ja) * | 1999-10-01 | 2001-06-19 | Tosoh Corp | リチウムマンガン酸化物およびその製造方法、並びにこれを用いた二次電池 |
| JP2002075355A (ja) * | 2000-08-23 | 2002-03-15 | Chisso Corp | 有機電解液二次電池用正極活物質、その製造方法およびそれを用いた有機電解液二次電池 |
| CN1416189A (zh) * | 2001-11-02 | 2003-05-07 | 中国科学院物理研究所 | 以纳米表面包覆复合材料为正极活性物质的锂二次电池 |
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