Investigation on synthesis conditions of LiNi1-x-yCoxMnyO2 cathode material via co-precipitation

doi:10.11949/j.issn.0438-1157.20171308

Abstract

Abstract:

Layer-structured spherical cathode material, LiNi_1-x-yCo_xMn_yO₂, with high purity can be prepared by co-precipitation with high efficiency and low energy consumption. This method has been widely applied in both fundamental research and industrial production, mainly including co-precipitation and high-temperature calcination processes. The mechanisms and influence factors involved in each procedure were elaborated and analyzed. The nucleation process and the complexation and precipitation reactions of Ni, Co and Mn ions were investigated in the key step of co-precipitation for the preparation of precursor. Based on the established equilibrium equations of reactions and thermodynamics, the two-dimensional variations of the three non-precipitated metal concentrations and their mutual ratios for different pH and amounts of NH₃ were thoroughly analyzed. Through the analysis results, theoretical optimum conditions for the cathode material with desired metal-ion ratios were thus proposed for the first time. In addition, by means of analyzing the structural characteristics of the precursor and cathode material as well as the electrochemical activity of the final material, the proper operation conditions were qualitatively investigated. Finally, the scientific method for optimizing the process conditions of LiNi_1-x-yCo_xMn_yO₂ cathode material was prospected.

Key words: LiNi_1-x-yCo_xMn_yO₂, cathode material, particulate processes, co-precipitation, preparation, thermodynamics, calcination

摘要：

共沉淀法可高效、低能耗制备出较高纯度的球形层状LiNi_1-x-yCo_xMn_yO₂正极材料，广泛应用于基础研究和工业生产中，主要包括液相共沉淀及高温煅烧过程。对这两个过程中涉及的机理进行了阐述，并分析相关影响因素，考察了共沉淀制备前体这个关键步骤中颗粒成核过程以及Ni、Co、Mn 3种金属离子发生的络合及沉淀反应。通过建立的反应和热力学平衡方程，分析未沉淀的3种金属离子及其相互之间比值随pH和氨水加入量的二维变化，首次定量得出制备所需Ni、Co、Mn配比三元正极材料的理论最佳条件。此外，从前体及正极材料的结构特性以及最终材料的电化学活性出发，定性探究了最优操作条件。最后，展望了三元正极材料工艺条件优化的科学方法。

关键词: LiNi_1-x-yCo_xMn_yO₂, 正极材料, 颗粒过程, 共沉淀, 制备, 热力学, 高温煅烧

CLC Number:

TQ031.2

GENG Shujun, HUANG Qingshan, ZHU Quanhong, JIN Yongcheng, YANG Chao. Investigation on synthesis conditions of LiNi_1-x-yCo_xMn_yO₂ cathode material via co-precipitation[J]. CIESC Journal, 2018, 69(1): 175-187.

耿淑君, 黄青山, 朱全红, 金永成, 杨超. 共沉淀法制备LiNi_1-x-yCo_xMn_yO₂正极材料工艺条件探究[J]. 化工学报, 2018, 69(1): 175-187.

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[58]	LI L J, LI X H, WANG Z X, et al. A simple and effective method to synthesize layered LiNi0.8Co0.1Mn0.1O2 cathode materials for lithium ion battery[J]. Powder Technology, 2011, 206(3):353-357.
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[63]	YANG S Y, WANG X Y, YANG X K, et al. Influence of Li source on tap density and high rate cycling performance of spherical Li[Ni1/3Co1/3Mn1/3] O2 for advanced lithium-ion batteries[J]. Journal of Solid State Electrochemistry, 2011, 16(3):1229-1237.
[64]	SHIN H, PARK S, BAE Y, et al. Synthesis of Li[NiCoMn]O cathode materials via a carbonate process[J]. Solid State Ionics, 2005, 176(35-36):2577-2581.
[65]	LIU J H, CHEN H Y, XIE J N, et al. Electrochemical performance studies of Li-rich cathode materials with different primary particle sizes[J]. Journal of Power Sources, 2014, 251:208-214.
[66]	CAO H, ZHANG Y, ZHANG J, et al. Synthesis and electrochemical characteristics of layered LiNiCoMnO cathode material for lithium ion batteries[J]. Solid State Ionics, 2005, 176(13-14):1207-1211.
[67]	LI X Q, XIONG X H, WANG Z X, et al. Effect of sintering temperature on cycling performance and rate performance of LiNi0.8Co0.1Mn0.1O2[J]. Transactions of Nonferrous Metals Society of China, 2014, 24(12):4023-4029.
[68]	Li L, Zhang X X, Chen R J, et al. Synthesis and electrochemical performance of cathode material Li1.2Co0.13Ni0.13Mn0.54O2 from spent lithium-ion batteries[J]. Journal of Power Sources, 2014, 249:28-34.
[69]	TODOROV Y M, NUMATA K. Effects of the Li:(Mn+Co+Ni) molar ratio on the electrochemical properties of LiMn1/3Co1/3Ni1/3O2 cathode material[J]. Electrochimica Acta, 2004, 50(2):495-499.
[70]	ZHANG L Q, WANG X Q, MUTA T, et al. The effects of extra Li content, synthesis method, sintering temperature on synthesis and electrochemistry of layered LiNi1/3Mn1/3Co1/3O2[J]. Journal of Power Sources, 2006, 162(1):629-635.

Investigation on synthesis conditions of LiNi_1-x-yCo_xMn_yO₂ cathode material via co-precipitation

共沉淀法制备LiNi_1-x-yCo_xMn_yO₂正极材料工艺条件探究

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