Research progress in solid-phase prelithiation of silicon-oxygen anode material for lithium-ion batteries
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摘要: 固相预锂化技术因其简单的制备工艺、环境友好性以及出色的预锂化效果已成为硅氧负极材料常用的预锂化方法之一。本文对硅氧材料(SiOx)固相预锂化技术进行了综述,分类介绍了固相预锂化技术采用的锂源,从电化学性能、工艺流程复杂性以及环境友好性等方面对各类固相预锂化技术进行了对比分析。归纳了锂源湿法包覆SiOx以及偏硅酸锂(Li2SiO3)组分调控对固相预锂化性能的提升效果。在此基础之上讨论了现有固相预锂化存在的问题、解决方法以及新的发展方向,并展望了固相预锂化在锂离子电池SiOx中的应用趋势。Abstract: Solid-phase prelithiation technology has become one of the commonly used prelithiation methods for silicon-oxygen anode materials due to its simple preparation process, environmental friendliness, and excellent prelithiation effect. This paper reviews the solid-phase prelithiation technology for silicon-oxygen materials (SiOx), categorizing the lithium sources used in solid- phase prelithiation techniques. A comparative analysis of various solid-phase prelithiation methods is conducted in terms of electrochemical performance, process complexity, and environmental friendliness. The paper summarizes the enhancement effects of lithium source wet coating on SiOx and the component regulation of lithium metasilicate (Li2SiO3) on solid-phase prelithiation performance. Based on this, it discusses the existing problems, solutions, and new development directions of solid-phase prelithiation technology, and forecasts the application trends of solid-phase prelithiation in SiOx for lithium-ion batteries.
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Key words:
- solid-phase prelithiation /
- silicon-oxygen /
- lithium source /
- wet coating /
- lithium metasilic
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图 2 CVD碳包覆SiOx示意图(a)和SiOx@C首次脱嵌锂过程示意图(b)、锂金属固相预锂化SiOx@C示意图(c) 以及预锂化SiOx@C的脱嵌锂过程示意图(d)
Figure 2. Schematic diagram of CVD carbon-coated SiOx (a) and the first lithium intercalation and deintercalation process of SiOx@C (b) schematic diagram of lithium metal solid-phase prelithiation of SiOx@C (c) and the lithium deintercalation process of prelithiated SiOx@C (d).
图 5 LiH预锂化SiOx示意图 (a)、预锂化后的XRD图 (b)[9]; Si/TiSi2/Li2SiO3制备示意图 (c) 和倍率性能、循环容量/效率曲线(d) [33]
Figure 5. Schematic diagram of LiH prelithiated SiOx (a) and XRD pattern after prelithiation (b) [9]; Schematic diagram of Si/TiSi2/Li2SiO3 preparation (c) and rate performance, cycling capacity/efficiency curves (d)[33]
图 8 (a) Si/SiOx/Li2SiO3@C制备示意图[47]; M-Li-SiOx的制备示意图 (b) 以及反应过程原理图 (c) [48]; (d) SLMP-SiOx/C、LiBp-SiOx/C的合成过程示意图[52]; (e) ToF-SIMS元素分布图像(a, d)Li−、(b, e) Si−和(c, f) Li−(红色)和Si−(绿色)物质叠加,SLMP-SiOx/C(a、b、c), LiBp-SiOx/C(d、e、f)[52]
Figure 8. (a) Schematic diagram of Si/SiOx/Li2SiO3@C preparation[47]; (b) Preparation schematic of M-Li-SiOx and (c) schematic of the reaction process[48]; (d) Schematic synthesis process of SLMP-SiOx/C, LiBp-SiOx/C[52]; (e) ToF-SIMS elemental distribution images: (a, d) Li−, (b, e) Si−, and (c, f) overlaid images of Li− (in red) and Si− (in green), SLMP-SiOx/C (a, b, c), LiBp-SiOx/C (d, e, f) [52]
图 9 (a) Li-Si-O三元材料的形成能与密度[53]; (b) 不同加热速率下热反应SiOx的TG曲线与XRD图[63]; (c) SiOx/锂粉末混合物的时间-温度-变换图和线性加热曲线[(a)和(b)[63]
Figure 9. (a) Formation energy and density of Li-Si-O ternary materials[53]; (b) TG curves and XRD patterns of thermally reacted SiOx at different heating rates[63]; (c) Time-temperature-transformation diagram and linear heating curves of SiOx/lithium powder mixtures [(a) and (b)][63]
图 10 (a) Si与Li2SiO3的晶粒尺寸与容量、ICE的关系分布图[65]; (b) 脱氢驱动预锂化的相变和微观结构演化示意图[32];(c) 不同温度下Si与Li2SiO3晶粒尺寸大小[32]
Figure 10. (a) Graph showing the relationship distribution between the grain size of Si and Li2SiO3 and their capacity, as well as ICE. [65]; (b) Schematic illustration of phase transition and microstructure evolution driven by dehydrogenation-induced prelithiation[32]; (c) Dimensions of Si and Li2SiO3 at different temperatures[32]
表 1 LiH与LiOH固相预锂化SiOx@C后的硅晶粒尺寸与热处理参数表
Table 1. Silicon grain sizes and heat treatment parameters after solid-phase prelithiation of SiOx@C with LiH and LiOH
Heating rate/℃·min−1 Heating temperature /℃ Heat-up time/h Silicon grain size/nm 3 750 8 LiH solid -phase
prelithiated SiOx@CLiOH solid -phase
prelithiated SiOx@C7.35 5.4 表 2 LiH预锂化SiOx@C前后硅晶粒尺寸对比表
Table 2. Comparison of silicon grain sizes before and after LiH prelithiation of SiOx@C.
Scherrer formula(Dc) Calculated crystal face Silicon grain size/nm [(k×0.1λ/(cosθ×radians(FWHM))] (111) SiOx@C Prelithiated-SiOx@C 3.60 7.35 -
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