锂离子电池正极材料超声强化水洗过程研究

doi:10.16085/j.issn.1000-6613.2019-0901

摘要/Abstract

摘要：

针对高镍三元锂离子电池正极材料的降碱处理方式主要局限于去离子水洗涤且清洗效果不佳的问题，提出了一种超声强化水洗处理高镍三元锂离子电池正极材料的新方法。以LiNi_0.8Co_0.15Al_0.05O₂（NCA）为研究对象，去离子水为溶剂，通过正交试验探讨了超声强化水洗对高镍三元锂离子电池正极材料进行降碱处理的影响因素，并就单一固含量因素影响与简单去离子水洗涤进行对比。采用pH测定、粒度分析、SEM、电化学性能测试等手段进行分析，研究了固含量、搅拌时间、超声时间、超声频率、超声功率等对高镍三元锂离子电池正极材料降碱效果的影响。研究结果表明：在固含量10%、搅拌时间更均匀的情况下，颗粒表面形貌无明显影响，材料电化学性能提高。实际工业生产过程中水洗的固含量为40%更为合适。

关键词: 锂电池, 正极材料, 超声水洗, 正交试验

Abstract:

The alkali reduction treatment of cathode materials for high nickel ternary lithium ion batteries is confined to pure water washing and the effect is limited. There are few reports on ultrasonic cleaning. A new technology of treating cathode materials of high nickel ternary lithium ion batteries by ultrasonic water washing was proposed. LiNi_0.8Co_0.15Al_0.05O₂ (NCA) was the research object and pure water as solvent. The factors affecting the alkali reduction of cathode materials by ultrasonic washing were discussed through orthogonal experiments. The influence of single solid content factor on washing with pure water was compared. The effects of solid content, stirring time, ultrasonic time, frequency and power on alkali reduction of cathode materials for high nickel lithium ion batteries were studied by means of pH, particle size analysis, SEM and electrochemical performance test. The results showed that the treatment effect was the best when solid content was 10% with stirring time of 5min, ultrasonic time of 1min, ultrasonic frequency of 200kHz and ultrasonic power of 100W. pH of cathode material decreased by 12.02%. The particle size distribution was more uniform, the surface morphology of the particles had no obvious influence, and the electrochemical properties of materials were improved. The solid content of washing was 40% in the actual industrial production process.

Key words: lithium batteries, cathode material, ultrasound washing, orthogonal test

中图分类号:

TM912.9

李萌,刘雪东,诸士春,虞兰剑,许晶. 锂离子电池正极材料超声强化水洗过程研究[J]. 化工进展, 2020, 39(2): 635-642.

Meng LI,Xuedong LIU,Shichun ZHU,Lanjian YU,Jing XU. Application of ultrasound in cathode materials of ternary lithium ion batteries[J]. Chemical Industry and Engineering Progress, 2020, 39(2): 635-642.

图/表 11

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水平	固含量A/%	搅拌时间B/min	超声时间C/min	超声频率D/kHz	超声功率E/W
水平1	10	1	1	17	20
水平2	20	2	2	28	40
水平3	30	3	3	68	60
水平4	40	4	4	120	80
水平5	50	5	5	200	100

水平	固含量A/%	搅拌时间B/min	超声时间C/min	超声频率D/kHz	超声功率E/W
水平1	10	1	1	17	20
水平2	20	2	2	28	40
水平3	30	3	3	68	60
水平4	40	4	4	120	80
水平5	50	5	5	200	100

pH方差	A	B	C	D	E
k1	11.00	11.34	11.19	11.15	11.25
k2	11.27	11.18	11.26	11.20	11.26
k3	11.19	11.15	11.27	11.28	11.16
k4	11.18	11.22	11.09	11.20	11.15
k5	11.33	11.08	11.17	11.14	11.14
极差	0.33	0.26	0.18	0.14	0.12
最优方案	A1	B5	C4	D5	E5

pH方差	A	B	C	D	E
k1	11.00	11.34	11.19	11.15	11.25
k2	11.27	11.18	11.26	11.20	11.26
k3	11.19	11.15	11.27	11.28	11.16
k4	11.18	11.22	11.09	11.20	11.15
k5	11.33	11.08	11.17	11.14	11.14
极差	0.33	0.26	0.18	0.14	0.12
最优方案	A1	B5	C4	D5	E5

样品	Li₂CO₃含量/%	LiOH含量/%
原料	1.78	0.97
超声1min	0.24	0.16
超声2min	0.31	0.17
超声3min	0.33	0.18
超声4min	0.16	0.09
超声5min	0.14	0.21