Basic scientific problems of Ni rich cathode materials for Li-ion battery: Surface residual Li and its removal
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摘要: 层状富Ni正极材料具有高可逆容量、低自放电性能和低成本优势，被认为是最有潜力的Li+电池正极材料。然而，材料结构不稳定、容量衰退和安全性差等问题，阻碍了富Ni正极材料的实际应用。当Ni含量大于80%时，富镍正极易与空气中的水分和CO2反应，在材料表面生成Li2CO3、LiHCO3、LiOH等残Li化合物。残Li存在不仅导致材料不稳定和电化学性能衰退，还造成电池安全问题。本文首先综述了残Li化合物的形成机制及其危害，再探讨了水洗过程中的水洗温度、时间、干燥温度等因素对材料性能的影响，并阐述了水洗造成结构衰退和容量衰减的机制。此外，还论述了其他去除残Li化合物的方法，特别是无水洗表面包覆的方法在去除残Li化合物影响方面呈现出巨大应用潜力。Abstract: The layered Ni-rich cathode materials are considered as the most promising cathode materials for Li-ion batteries due to their high reversible capacity, low self-discharge performance and low cost. However, they have some disadvantages, such as the unstable material structure, capacity decay and poor safety, hindered their practical application. The Ni-rich cathode materials with nickel content over 80% are easy to react with moisture and CO2 in the air, generating residual Li compounds such as Li2CO3, LiHCO3 and LiOH on the surface of materials. The presence of residual Li not only leads to structure instability and electrochemical performance degradation, but also causes battery safety problems. In this paper, the mechanism of the formation of residual Li and its hazards are reviewed. Then, the effect of factors (e.g. washing temperature, time, drying temperature, etc.) during water washing on the material property are discussed, and the mechanisms of structural deterioration and capacity degradation induced by water washing are elaborated. Lastly, other methods for removing residual Li compounds are introduced, especially the non-washing surface coating method, which shows great application potential in removing the influence of residual Li compounds.
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Key words:
- nanomaterials /
- preparation /
- surface /
- Ni-rich cathode /
- residual lithium /
- washing /
- Li-ion battery
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图 2 未处理和包覆Li2CO3、LiF涂层LiNi0.8Co0.1Mn0.1O2的首周放电容量 (a) 和200周循环性能 (b)[49]、碳酸锂对富镍正极首周充放电过程相转变的影响 (c)[50]、富镍正极材料产生气体机制 (d)[34]
Figure 2. Fresh, Li2CO3-coated and LiF-coated LiNi0.8Co0.1Mn0.1O2 first cycle discharge capacity (a) , the cycle performance during 200 cycles (b)[49], effects of Li2CO3 on the phase transition of Ni-rich cathode during first cycle (c)[50]and gas generation mechanism of nickel-rich cathode materials (d)[34]
图 3 水洗时间为0 min (a)、5 min (b)、15 min (c) 及30 min (d) 的LiNi0.83Co0.13Mn0.04O2的SEM图像[60]；不同水洗时间的LiNi0.83Co0.13Mn0.04O2的XRD图谱 (e) 和循环50次的容量保持率 (f)[60]
Figure 3. SEM images of LiNi0.83Co0.13Mn0.04O2 cathode after different washing time: 0 min (a), 5 min (b), 15 min (c) and 30 min (d)[60]; Powder XRD patterns (e) and capacity retention after 50 cycles for LiNi0.83Co0.13Mn0.04O2 after different washing time (f)[60]
图 4 未水洗 (a) 和材料与水比值为1 ∶ 0.7 (b)、1 ∶ 1 (c)、1 ∶ 2 (d) 1 ∶ 2及1 ∶ 5 (e) 的水洗涤后LiNi0.80Co0.15Mn0.05O2的SEM图像[23]；未水洗和水洗后材料的循环性能 (f)[23]；残锂量和容量保持率与洗涤用水量的关系 (g)[23]；未水洗和经不同洗涤次数的LiNi0.83Co0.15Al0.02O2的充放电容量曲线 (h)[61]
Figure 4. SEM images of fresh (a) and washed LiNi0.80Co0.15Mn0.05O2 with ratio of material to water fixed about 1 ∶ 0.7 (b), 1 ∶ 1 (c), 1 ∶ 2 (d) and 1 ∶ 5 (e) [23]; Cycling performance of fresh and washed materials (f)[23]; Relationship between the residual lithium amount and capacity retention rate and the amount of water used for washing (g)[23]; Charge-discharge capacity curve of fresh and washed LiNi0.83Co0.15Al0.02O2 with different washing times (h)[61]
图 5 未处理 (a) 和水洗后不同干燥温度80 ℃ (b)、120 ℃ (c) 和190 ℃ (d) 材料的SEM图像[23]；TGA-MS分析未处理和水洗两次LiNi0.85Co0.1Mn0.05O2随温度升高的质量损失和气体释放 (e)[62]
Figure 5. SEM images of fresh material (a) and washed and dried at 80 ℃ (b), 120 ℃ (c) and 190 ℃ (d) [23]; TGA-MS analysis of the mass loss and gas release of fresh and two times washed LiNi0.85Co0.1Mn0.05O2 (e)[62]
图 6 未处理 ((a), (b)) 和水洗 ((c), (d)) 后富镍正极材料在空气中储存30天后SEM和TEM图像[63]；在空气中储存7天 ((e), (f)) 和30天 ((g), (h)) 未处理和水洗材料在不同倍率下充放电曲线[63]
Figure 6. SEM and TEM images of fresh ((a), (b)) and washed ((c), (d)) nickel-rich cathode materials after storage in air for 30 days[63]; Charge and discharge curves of fresh and washed materials stored in air for 7 days ((e), (f)) and 30 days ((g), (h)) at different rates[63]
FFT—Fast Fourier transform
图 7 未处理 (a) 和水洗后二次煅烧热处理 (b) LiNi0.88Co0.11Al0.01O2第300周电化学阻抗谱和等效电路[14]；未处理和水洗后二次煅烧热处理LiNi0.88Co0.11Al0.01O2的循环性能 (c)[14]；水洗和热处理结构变化的示意简图 ((d)~(f))[14]
Figure 7. Electrochemical impedance spectra and the equivalent circuits of fresh (a) and secondary calcination treated (b) LiNi0.88Co0.11Al0.01O2 at 300th cycle[14]; Cycling performance of fresh and secondary calcination treated LiNi0.88Co0.11Al0.01O2 (c)[14]; Schematic illustration of structural changes during washing and heat treatment ((d)-(f))[14]
Re, Rs and Rct—Resistance of liquid electrolyte, resistance of solid electrolyte interphase film and charge transfer resistance, respectively; L1—Warburg impedance connected with the lithium ions diffusion through the solid particles
图 8 (a)水洗富Ni正极滤液pH随水洗时间变化(NCA：LiNi0.83Co0.15Al0.02O2，NCM523PC：多晶LiNi0.5Co0.2Mn0.3O2，NCM523SC：单晶LiNi0.5Co0.2Mn0.3O2)[64]；(b)两次独立测量未处理和水洗后不同温度干燥的富Ni正极的平均阻抗，误差线表示两次测量的最小值/最大值[62]；(c)循环前后放电过程中Li嵌入的示意图[14]
Figure 8. (a) Changes of pH for the filtrate obtained at different washing time (NCA: LiNi0.83Co0.15Al0.02O2, NCM523 PC: Polycrystalline LiNi0.5Co0.2Mn0.3O2, NCM523 SC: single-crystalline LiNi0.5Co0.2Mn0.3O2)[64]; (b) Average impedance from two independent measurements for fresh and washed and dried Ni-rich cathode, the error bars indicate the minimum/maximum of two measurements[62]; (c) Schematic illustration of the Li intercalation during the discharge process before/after cycle[14]
表 1 不同水洗温度下材料的Li、Ni、Co和Al含量变化[58]
Table 1. Changes in the content of Li, Ni, Co and Al under different washing temperature[58]
Washing temperature/℃ Li/wt% Ni/wt% Co/wt% Al/wt% Fresh 7.28 48.83 9.16 1.38 5 7.23 48.87 9.19 1.40 15 7.21 48.88 9.18 1.39 25 7.16 48.92 9.20 1.41 35 7.08 48.99 9.22 1.41 45 6.92 49.14 9.31 1.42 
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表 2 不同水洗时间样品的晶胞结构参数及I(003)/I(104)值[60]
Table 2. Unit cell structure parameters and I(003)/I(104) values of samples with different washing time[60]
Washing time/min a/nm c/nm c/a I(003)/I(104) Fresh 0.2874 1.4206 4.943 1.14 5 0.2872 1.4203 4.945 1.21 15 0.2872 1.4204 4.946 1.17 30 0.2873 1.4208 4.945 1.15 Notes: a, c—Lattice parameters of the crystal; c/a—Ratio of c to a; I(003)/I(104)—Intensity ratio of (003) to (104) peaks in XRD.
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表 3 未处理以及水洗干燥LiNi0.80Co0.15Mn0.05O2中的总残Li量[23]
Table 3. Total amount of residual Li of fresh and washed and dried LiNi0.80Co0.15Mn0.05O2[23]
Drying
temperature/℃Total amount of
residual lithium/10−6Fresh 2319 80 1203 120 1130 190 916
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表 4 未处理和经水洗干燥的LiNi0.85Co0.1Mn0.05O2在石墨全电池的电化学性能[62]
Table 4. Electrochemical performance of fresh and washed and dried LiNi0.85Co0.1Mn0.05O2 in full battery with graphite anode[62]
Drying temperature/℃ Discharge capacity of 0.1C
cycle 2 times/(mA·h·g−1)Discharge capacity
loss of 0.1 C to 1 C/%Discharge capacity
loss after 198 cycles of 1 C/%Fresh 188 5 12 80 178 11 20 180 175 16 25 300 130 31 92
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