Basic scientific problems of nickel rich cathode materials for Li-ion battery: Regulation and mechanism for crystallization of hydroxide precursor
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摘要: 富镍锂过渡金属氧化物正极具有高容量及高工作电压的优点，是理想的高能量动力电池材料。富镍锂过渡金属氧化物正极的性能主要受其氢氧化物前驱体的结构、形貌、粒径等因素影响。一次晶粒和二次颗粒形貌与尺寸可控的球形氢氧化物前驱体是制备优异电化学性能的富镍正极材料的关键。氢氧化物前驱体沉淀结晶过程中工艺参数会影响前驱体性能，其生长机制对于调控沉淀结晶具有指导意义。本论文首先介绍了沉淀结晶相关基础理论，其次探讨了富镍正极材料氢氧化物前驱体沉淀结晶生长机制和沉淀反应因素对氢氧化物物理及化学性能影响，最后介绍了合成单晶、放射状和核壳结构等特殊富镍正极材料的前驱体。Abstract: The nickel-rich lithium transition metal oxide cathode is an ideal high-energy power battery material due to its high capacity and high working voltage. Its performance is mainly affected by the structure, morphology, particle size and other factors of its hydroxide precursor. The spherical hydroxide precursor with controllable morphology and size of primary grain and secondary particles is the key for the preparation of nickel-rich cathode materials with excellent electrochemical performance. During the precipitation and crystallization process of hydroxide precursor, the process parameters will affect the performance of the precursor, and its growth mecha-nism has guiding significance for regulating the precipitation and crystallization. This paper reviews the basic theories related to precipitation crystallization, then discusses the growth mechanism of precipitation crystallization for hydroxide precursors of nickel-rich cathode materials and the influence of precipitation reaction factors on the physical and chemical properties of hydroxide. At last, the precursors for the synthesis of nickel-rich cathode materials with special structures such as single crystal, radial and core-shell structures are introduced.
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图 1 (a)沉淀过程中溶液溶质浓度随时间变化示意图[27]；(b)溶液状态图[25]；(c)系统自由能ΔG与半径r的关系图[32]
Figure 1. (a) Schematic diagram of the change of solution solute concentration with time during precipitation[27]; (b) Solution state diagram[25]; (c) Relationship between the system free energy ΔG and the radius r[32]
0—Solubility curve; 1, 2—Curve of the first and second metastable limits; S—Stable zone; M1, M2—First and second metastable zones; L—Unstable zone; Ⅰ—Nucleation-inducing zone; Ⅱ—Nucleation zone; Ⅲ—Growing zone; $\Delta G_{\rm{k}}^{\text{θ} }$—Minimum nucleation energy barrier; r*—Critical nuclear radius
图 4 反应时间分别为1、2、4、6 、8、10、22 h ((a)~(g))的Ni0.6Co0.2Mn0.2(OH)2前驱体的SEM图像；(h)类折纸灯笼一次晶粒组装为二次颗粒的示意图[47]
Figure 4. SEM images of the Ni0.6Co0.2Mn0.2(OH)2 precursors obtained at reaction time for 1, 2 , 4, 6, 8, 10, 22 h ((a)-(g)), respectively; (h) Diagrammatic sketch for the assembling of secondary particle[47]
图 7 在pH＝11.2((a), (d))、pH＝11.5 ((b), (e)) 和pH＝11.8 ((c), (f))下制备Ni0.8Co0.1Mn0.1(OH)2 的SEM图像[19]；(g) 不同组分Ni1-x-yCoxMny(OH)2的pH值和氨浓度；(h) pH对[Ni(NH3)n]2+、[Co(NH3)n]2+和[Mn(NH3)n]2+浓度的影响[38] (曲线是1≤n≤6的络合物的总和)；(i) 反应5 h时pH对Ni(OH)2、Ni1/2Mn1/2(OH)2和Ni1/3Co1/3Mn1/3(OH)2振实密度的影响[38]
Figure 7. SEM images of Ni0.8Co0.1Mn0.1(OH)2 prepared at pH of 11.2 ((a), (d)), 11.5 ((b), (e)) and 11.8 ((c), (f))[19]; (g) pH value and ammonia concentration of Ni1-x-yCoxMny(OH)2 with different compositions; (h) Influence of pH on the concentration of [Ni(NH3)n]2+, [Co(NH3)n]2+ and [Mn(NH3)n]2+ (the curve is the sum of complexes for 1≤n≤6)[38]; (i) Effect of pH on the tap density of Ni(OH)2, Ni1/2Mn1/2(OH)2, and Ni1/3Co1/3Mn1/3(OH)2 when reaction time was 5 hours[38]
图 8 (a)二次颗粒粒径随时间变化图[53]；(b)不同温度下Ni1/3Co1/3Mn1/3(OH)2前驱体的粒度变化图[54]；(c)无保护气氛时和有N2保护时Ni0.45Co0.1Mn0.45(OH)2前驱体的XRD图谱[56]
Figure 8. (a) Size of the secondary particles at difference reaction time[53]; (b) Size of the Ni1/3Co1/3Mn1/3(OH)2 precursor at different temperatures[54]; (c) XRD spectrum of Ni0.45Co0.1Mn0.45(OH)2 precursor synthesized with or without the protection of N2[56]
D10, D50, D90—Cumulative distribution of particles is 10%, 50%, 90% of the particle size, respectively
图 9 (a)螺旋桨叶轮；(b)平直涡轮式叶轮；(c)折叶涡轮式叶轮；(d)螺旋桨叶轮的水平旋流；(e)平直涡轮式叶轮安装挡板后的液流；((f)~(h)) 在400、600、800 r/min转速下合成Ni0.6Co0.2Mn0.2(OH)2的SEM图像[48]
Figure 9. (a) Propeller impeller; (b) Flat turbine impeller; (c) Folded blade turbine impeller; (d) Horizontal swirl of propeller impeller; (e) Liquid flow after installation of baffle on flat turbine impeller; ((f)-(h)) SEM images of Ni0.6Co0.2Mn0.2(OH)2 powders prepared at stirring speed for 400, 600 and 800 r/min[48]
图 10 间歇和连续操作过程反应器结晶示意图((a), (d))、停留时间分布((b), (e))及代表性前驱体SEM图像((c), (f))[65, 67]
Figure 10. Reactor schematic diagram ((a), (d)), residence time ((b), (e)) and typical SEM image ((c), (f)) for batch and continuous precipitation[65, 67]
BR—Batch reactor; CSTR—Continuous stirred tank reactor; C(t)—From the time the fluid enters the reactor, the ratio of the fluid flowing out of the reactor to the total number of fluids in the time t
图 11 单晶 ((a), (b)) 和多晶 ((c), (d)) 富镍正极所用前驱体的SEM图像
Figure 11. SEM images of precursors for single ((a), (b)) and polycrystalline ((c), (d)) Ni-rich cathode
图 12 (a)放射状富镍正极材料的结构和特性示意图[76]；((b)~(d))放射状前驱体的SEM和横截面SEM图像[76]；((e)~(j)) 在0 min、20 min、40 min、2 h、3 h、4 h不同时间下合成的由Ni0.5Mn0.5(OH)2包覆Ni0.8Co0.1Mn0.1(OH)2的SEM图像[77]；(k)核壳结构正极材料颗粒示意图[78]
Figure 12. (a) Schematic diagram of the structure and characteristics of the radial Ni-rich material[76]; ((b)-(d)) SEM and cross-sectional SEM images of the radial precursor[76]; ((e)-(j)) SEM image of Ni0.5Mn0.5(OH)2 coated Ni0.8Co0.1Mn0.1(OH)2 synthesized at different times for 0 min, 20 min, 40 min, 2 h, 3 h and 4 h[77]; (k) Schematic diagram of core-shell structure cathode material[78]
表 1 富镍三元正极材料相关氢氧化物溶度积常数(25℃时)[25]
Table 1. Solubility product constant of hydroxide related to nickel-rich ternary cathode material (at 25℃)[25]
Insoluble electrolyte Ni(OH)2 Co(OH)2 Mn(OH)2 Mg(OH)2 Al(OH)3 Solubility product constant Ksp 2.0×10−15(Fresh) 1.9×10−15(Fresh) 1.6×10−13 1.2×10−11 1.3×10−33 
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