Na2PO3F对LiNi0.83Co0.11Mn0.06O2材料的复合改性及机理分析

doi:10.6023/A21100477

化学学报 ›› 2022, Vol. 80 ›› Issue (2): 150-158.DOI: 10.6023/A21100477 上一篇下一篇

研究论文

Na₂PO₃F对LiNi_0.83Co_0.11Mn_0.06O₂材料的复合改性及机理分析

黄擎^a^,^b, 丁瑞^a^,^b, 陈来^a^,^b^,^*(), 卢赟^a^,^b, 石奇^a^,^b, 张其雨^a^,^b, 聂启军^a^,^b, 苏岳锋^a^,^b^,^*(), 吴锋^a^,^b

a 北京理工大学材料学院环境科学与工程北京市重点实验室北京 100081
b 北京理工大学重庆创新中心重庆 401120

投稿日期:2021-10-26 发布日期:2022-01-18
通讯作者: 陈来, 苏岳锋
基金资助:
国家自然科学基金(2217090605); 国家自然科学基金(21875022); 国家自然科学基金(51802020); 重庆市自然科学基金(cstc2020jcyj-msxmX0654); 重庆市自然科学基金(cstc2020jcyj-msxmX0589); 中国科学技术协会青年人才托举计划(2018QNRC001); 北京理工大学“青年教师学术启动计划”

Dual-Decoration and Mechanism Analysis of Ni-rich LiNi_0.83Co_0.11Mn_0.06O₂ Cathodes by Na₂PO₃F

Qing Huang^a^,^b, Rui Ding^a^,^b, Lai Chen^a^,^b(), Yun Lu^a^,^b, Qi Shi^a^,^b, Qiyu Zhang^a^,^b, Qijun Nie^a^,^b, Yuefeng Su^a^,^b(), Feng Wu^a^,^b

a School of Materials Science and Engineering, Beijing Key Laboratory of Environmental Science and Engineering, Beijing Institute of Technology, Beijing 100081
b Beijing Institute of Technology Chongqing Innovation Center, Chongqing 401120

Received:2021-10-26 Published:2022-01-18
Contact: Lai Chen, Yuefeng Su
Supported by:
National Natural Science Foundation of China(2217090605); National Natural Science Foundation of China(21875022); National Natural Science Foundation of China(51802020); Natural Science Foundation of Chongqing, China(cstc2020jcyj-msxmX0654); Natural Science Foundation of Chongqing, China(cstc2020jcyj-msxmX0589); Young Elite Scientists Sponsorship Program by China Association for Science and Technology, China(2018QNRC001); L. Chen acknowledges the support from Beijing Institute of Technology Research Fund Program for Young Scholars

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摘要/Abstract

采用湿化学法使用Na₂PO₃F对LiNi_0.83Co_0.11Mn_0.06O₂进行表面改性, 得到F^–掺杂和LiF包覆的正极材料. X射线衍射谱(XRD)结果显示(003)衍射峰向高角度偏移, 结合X射线光电子能谱(XPS)及透射电子显微镜(TEM)证明F^–进入到材料晶格内部; 扫描电镜(SEM)、TEM及XPS结果显示, 改性后材料表面存在均匀LiF包覆层, 可提高电极/电解液界面稳定性, 改善循环稳定性; 通过计算锂离子扩散系数, 证明Li⁺传输速率得到提升, 倍率性能改善. 电化学性能测试结果显示, 材料的循环稳定性和倍率性能均得到显著提高: 在2.75~4.3 V电压窗口下, 材料1 C循环200周后容量保持率由32.2%提高到65.2%, 10 C条件下放电比容量由145.7 mAh/g提高到161.5 mAh/g. 对循环后极片进行XPS分析, 正极-电解质界面(CEI层)层中的LiF, Li_xPO_yF_z, NiF₂减少, 有利于提高材料稳定性及循环性能.

关键词: 锂离子电池, 高镍正极材料, LiF包覆, F^–掺杂, 循环性能, 倍率性能

Since the commercialization of lithium-ion battery in 1991, it has promoted human society development for nearly three decades. Due to its higher energy density, Ni-rich layered oxides currently stand out as the most promising cathode materials to build power batteries for portable electronic devices and new energy electric vehicles. However, the severe side effects on the electrode/electrolyte interface and the structural instability of the material hinder its development, and a lot of research focus on improving the cycling stability and rate capability of nickel-rich cathode material. Here, a facile treatment with Na₂PO₃F was carried out to modify the Ni-rich LiNi_0.83Co_0.11Mn_0.06O₂ material at surface and bulk regions by using wet methods. By virtue of the fact that Na₂PO₃F dissolves in water and releases fluorine ions, a F^– doped and LiF coated Ni-rich LiNi_0.83Co_0.11Mn_0.06O₂ material was obtained. The X-ray diffraction (XRD) results showed that (003) peak shifted to a higher angle due to the replacement of O^2– by smaller F^–. Besides, the XRD Rietveld refinement and X-ray photoelectron spectroscopy (XPS) sputtering data determined that part of F^– ions had been successfully doped into the lattice, and the basic layer structure of the material was still well preserved in the process of modification. Scanning electron microscope (SEM), energy disperse spectroscopy (EDS), and transmission electron microscope (TEM) combined with XPS proved the existence of surface LiF coating layer. The 2~10 nm LiF layer was uniformly covered onto the surface of the cathode material, acting as a physical barrier against direct corrosion from the electrolyte, thus enhancing the cycling stability. In addition, the lithium ion diffusion coefficients (D_Li⁺) for bare and modified samples were calculated from cyclic voltammetry test results, which reveals a better rate capability from the synergistic effect of surface LiF coating and lattice F^– doping. The electrochemical tests also showed a better cycling stability and enhanced rate capability of the modified samples: within 2.75~4.3 V, the capacity retention after 200 cycles at 1 C-rate had been elevated from 32.2% to 65.2%; the discharge capacity under 10 C-rate was also improved from 145.7 to 161.5 mAh/g. To elaborate the improved effect, post-cycling characterizations were conducted. The morphology of modified particles after 200 cycles at 1 C still maintained intact grains, in contrast with the bare samples, exhibiting many micro-cracks. XPS spectra on decorated cathodes after cycling showed weaker signals of by-products including LiF, Li_xPO_yF_z, NiF₂ in the CEI layer, indicating side reaction on the interface was effectively suppressed, thus contributing to enhancing the cycling stability. The applicable method herein demonstrates a promising solution for improvement of Ni-rich cathode materials and their coming commercial application.

Key words: lithium-ion batteries, nickel-rich cathode, LiF coating, F^– doping, cycling stability, rate performance

引用此文

黄擎, 丁瑞, 陈来, 卢赟, 石奇, 张其雨, 聂启军, 苏岳锋, 吴锋. Na₂PO₃F对LiNi_0.83Co_0.11Mn_0.06O₂材料的复合改性及机理分析[J]. 化学学报, 2022, 80(2): 150-158.

Qing Huang, Rui Ding, Lai Chen, Yun Lu, Qi Shi, Qiyu Zhang, Qijun Nie, Yuefeng Su, Feng Wu. Dual-Decoration and Mechanism Analysis of Ni-rich LiNi_0.83Co_0.11Mn_0.06O₂ Cathodes by Na₂PO₃F[J]. Acta Chimica Sinica, 2022, 80(2): 150-158.

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图/表 12

Element	F-0	F-1
Li/%	1.0539	1.0192
Ni/%	0.8285	0.8286
Co/%	0.1137	0.1142
Mn/%	0.0577	0.0572
Na/%	—	0.0002
P/%	—

表1. F-0和F-1样品的元素含量a

Table 1. Elemental composition of F-0 and F-1

图1. (a) F-0, F-0.5, F-1和F-2样品的XRD图谱; (b) (003)峰的放大图谱图; (c) F-0和(d) F-1的XRD精修结果

Figure 1. (a) XRD patterns and (b) magnification of the (003) peaks of F-0, F-0.5, F-1 and F-2; XRD Rietveld refinement results of (c) F-0 and (d) F-1

Parameter	F-0	F-1
a/nm	0.28699	0.28718
c/nm	1.41955	1.41949
Unit volume/nm³	0.10125	0.10138
c∶a	4.946	4.943
R_wp/%	1.61	1.62
R_p/%	1.01	1.14

表2. F-0和F-1样品的精修数据

Table 2. The results of rietveld refinement for F-0 and F-1

图2. (a) F-0, (b) F-0.5, (c) F-1和(d) F-2的场发射扫描电子显微镜图

Figure 2. SEM images of (a) F-0, (b) F-0.5, (c) F-1 and (d) F-2

图3. F-1样品的元素分布图

Figure 3. EDS mapping of F-1

图4. (a) F-0和(b) F-1样品的透射电子显微镜图像; (c~g) F-1样品的元素分布图

Figure 4. TEM images of (a) F-0 and (b) F-1; (c~g) element mapping of F-1

图5. F-0和F-1样品的XPS谱图(a) Ni 2p, (b) O 1s, (c) Li 1s; (d) F-1的F1s谱图

Figure 5. XPS patterns of F-0 and F-1 samples (a) Ni 2p, (b) O 1s, (c) Li 1s; (d) F 1s of F-1

图6. (a) F-0, (b) F-0.5, (c) F-1和(d) F-2在0.2 mV•s–1扫描速率下的循环伏安曲线

Figure 6. CV curves of (a) F-0, (b) F-0.5, (c) F-1 and (d) F-2 with a scan rate of 0.2 mV•s–1

图7. (a)首周充放电曲线; (b ) 0.2 C倍率下循环性能; (c) 1 C倍率下循环性能; (d) 2.75~4.5 V, 1 C倍率下循环性能; (e) 2.75~4.5 V, 1 C倍率下循环的容量保持率; (f)倍率性能对比

Figure 7. (a) Initial charge-discharge curves; (b) cycling performance at 0.2 C rate; (c) cycling performance at 1 C; (d) cycling performance at 1 C, 2.75~4.5 V; (e) capacity retention of 1 C at 2.75~4.5 V; (f) rate performance comparison

图8. (a) F-0和(b) F-1样品在不同扫描速率下的CV曲线; (c)锂离子扩散系数拟合图

Figure 8. CV curves of (a) F-0 and (b) F-1 at various scan rates; (c) fitting diagram of diffusion coefficient of Li+

图9. 循环200周后F-0和F-1极片的场发射扫描电子显微镜图: (a) F-0, (b) F-1

Figure 9. SEM images of F-0 and F-1 samples after 200 cycles: (a) F-0, (b) F-1

图10. 循环200周后F-0和F-1样品的XPS谱图: (a) F 1s, (b) C 1s, (c) Ni 2p

Figure 10. XPS patterns of F-0 and F-1 samples after 200 cycles: (a) F 1s, (b) C 1s, (c) Ni 2p

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Na₂PO₃F对LiNi_0.83Co_0.11Mn_0.06O₂材料的复合改性及机理分析

Dual-Decoration and Mechanism Analysis of Ni-rich LiNi_0.83Co_0.11Mn_0.06O₂ Cathodes by Na₂PO₃F

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