富锰P2/P3双相Na0.67Mn0.9Ni0.1O2自蔓延燃烧合成与储钠性能

doi:10.6023/A25080290

摘要/Abstract

富锰层状氧化物因比容量高、成本低等优势, 成为备受关注的钠离子电池正极材料. 然而, 该材料在深度脱钠状态下的容量衰减和合成过程中结构易受煅烧温度影响, 为其应用带来了巨大挑战. 本工作采用自蔓延燃烧合成, 通过调控煅烧温度, 制备了一种P2/P3双相结构Na_0.67Mn_0.9Ni_0.1O₂ (NMNO-800)正极材料. X射线衍射结果表明, 煅烧温度的改变可以促使多相材料形成, 当煅烧温度在700和900 ℃时, NMNO-700和NMNO-900分别为P3相结构(空间群R3m)和P2相结构(空间群P63/mmc), 而当煅烧温度为800 ℃时, NMNO-800呈现出稳定的P2/P3双相结构, 经计算确定两相比例分别为42.4%和57.6%. 扫描电子显微镜分析表明, NMNO-800为纳微复合结构, 微米颗粒分布在1.94~2.57 μm之间, 同时微米级片状颗粒表面附着许多纳米颗粒. NMNO-800结合P2相和P3相的优势, 既有P2相的稳定结构, 又具有P3相的高初始容量, 展现出优异的电化学性能. 该材料在0.2 C下表现出165.44 mAh/g的高可逆比容量, 10 C大倍率下仍有89.18 mAh/g的可逆容量, 在0.5 C下循环100次后容量保持率为84.2%, 显著优于单相层状氧化物. 恒流间歇滴定技术(GITT)和电化学阻抗谱(EIS)分析表明, 具有P2/P3双相结构的NMNO-800表现出较高的钠离子扩散系数.

关键词: 钠离子电池, 正极材料, 层状氧化物, P2/P3双相, 富锰材料

The P2-type manganese-rich layered oxides have emerged as highly promising cathode materials for sodium-ion batteries owing to their exceptional advantages including high specific capacity and low cost. However, huge challenges remain for their practical applications, particularly the capacity degradation under deep desodiation conditions and the structural sensitivity to calcination temperatures during material synthesis. In this study, we successfully fabricated a P2/P3 biphasic Na_0.67Mn_0.9Ni_0.1O₂ (designated as NMNO-800) cathode material through a carefully controlled self-propagating combustion synthesis method with precise temperature regulation. Comprehensive X-ray diffraction characterization revealed that the calcination temperature plays a critical role in phase formation. NMNO-700 (calcined at 700 ℃) exhibited a pure P3-phase structure with R3m space group, while NMNO-900 (calcined at 900 ℃) showed a pure P2-phase structure with P63/mmc space group. Remarkably, the NMNO-800 sample calcined at the optimal temperature of 800 ℃ demonstrated a well-defined and stable P2/P3 biphasic structure, with the phase ratio quantitatively determined to be 42.4% P2-phase and 57.6% P3-phase through Rietveld refinement analysis. Scanning electron microscope (SEM) observations further confirmed that the NMNO-800 possesses a unique hierarchical nano-micro composite architecture, consisting of well-dispersed micron-sized particles ranging from 1.94 to 2.57 μm in diameter, with numerous nanoparticles distributed on the surface of these micron-scale sheet-like particles. This ingenious designed biphasic Na_0.67Mn_0.9Ni_0.1O₂ successfully combines the advantageous features of both P2 and P3 phases, maintaining the excellent structural stability characteristic of P2-phase while preserving the high initial capacity inherent to P3-phase, thereby achieving superior electrochemical performance. Specifically, the NMNO-800 delivers an outstanding reversible capacity of 165.44 mAh/g at 0.2 C rate, maintains a respectable capacity of 89.18 mAh/g even at an extremely high rate of 10 C, and shows excellent cycling stability with 84.2% capacity retention after 100 cycles at 0.5 C rate, significantly outperforming all single-phase counterparts. All the results indicate that the P2/P3 biphasic structure enhances the rate performance of manganese-rich layered oxide cathode materials, improves sodium ion diffusion efficiency, and maintains good cycling stability.

Key words: sodium ion battery, cathode materials, layered oxides, P2/P3 biphase, Mn-rich materials

引用此文

张庆堂, 杜纯阳, 高鹏飞, 王晓梅. 富锰P2/P3双相Na_0.67Mn_0.9Ni_0.1O₂自蔓延燃烧合成与储钠性能[J]. 化学学报, 2026, 84(1): 64-72.

Qingtang Zhang, Chunyang Du, Pengfei Gao, Xiaomei Wang. Self-propagating Combustion Synthesis and Sodium Storage Performance of Manganese-rich P2/P3 Biphasic Na_0.67Mn_0.9Ni_0.1O₂[J]. Acta Chimica Sinica, 2026, 84(1): 64-72.

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图/表 12

图1. (a) NMNO-700、NMNO-800和NMNO-900的XRD谱图; (b) NMNO-700、NMNO-800和NMNO-900的晶体结构示意图; (c) NMNO-700、(d) NMNO-800和(e) NMNO-900的XRD Rietveld精修图

Figure 1. (a) XRD spectra of NMNO-700, NMNO-800 and NMNO-900; (b) Schematic diagram of the crystal structure of NMNO-700, NMNO-800 and NMNO-900; XRD Rietveld refinement of (c) NMNO-700, (d) NMNO-800 and (e) NMNO-900

Sample	P2-Na_0.67Mn_0.9Ni_0.1O₂				P3-Na_0.67Mn_0.9Ni_0.1O₂
Sample	a/nm	b/nm	c/nm	V/nm³	a/nm	b/nm	c/nm	V/nm³
NMNO-700	—	—	—	—	0.285	0.285	1.679	0.11879
NMNO-800	0.287	0.287	1.122	0.08051	0.287	0.287	1.675	0.12027
NMNO-900	0.288	0.288	1.129	0.08126	—	—	—	—

表1. NMNO-700、NMNO-800和NMNO-900的晶胞参数

Table 1. Unit cell parameters of NMNO-700, NMNO-800 and NMNO-900

图2. (a) NMNO-700, (b) NMNO-800和(c) NMNO-900的SEM图; (d) NMNO-800的EDS元素分布图

Figure 2. SEM images of (a) NMNO-700, (b) NMNO-800 and (c) NMNO-900; (d) EDS element mapping of NMNO-800

图3. (a) NMNO-800的TEM图; (b) NMNO-800的HRTEM图; (c) NMNO-800的SAED图

Figure 3. (a) TEM image of NMNO-800; (b) HRTEM image of NMNO-800; (c) SAED image of NMNO-800

图4. (a) NMNO-800的XPS图谱; NMNO-800的(b) Mn 2p图谱和(c) Ni 2p图谱

Figure 4. (a) XPS profile of NMNO-800; (b) Mn 2p and (c) Ni 2p spectra of NMNO-800

测试元素	样品质量m₀/g	元素含量w/%	元素物质的量/mol	物质的量比
Na	0.1030	14.3005%	6.407×10^-4	0.65
Mn		47.0286%	8.817×10^-4	0.89
Ni		5.6639%	9.940×10^-5	0.1

表2. 电感耦合等离子体发射光谱(ICP-OES)测定的NMNO-800元素含量

Table 2. Element content of NMNO-800 determined by inductively coupled plasma optical emission spectrometer (ICP-OES)

图5. NMNO-700、NMNO-800和NMNO-900在0.2 C下(a)首次、(b)第三次和(c)第五次充放电曲线

Figure 5. (a) First, (b) third and (c) fifth charges and discharges of NMNO-700, NMNO-800, and NMNO-900 at 0.2 C

图6. (a) NMNO-700、NMNO-800和NMNO-900的倍率性能; (b) NMNO-700、NMNO-800和NMNO-900在0.5 C下的循环性能

Figure 6. (a) Rate performance of NMNO-700, NMNO-800 and NMNO-900; (b) Cycling performance of NMNO-700, NMNO-800 and NMNO-900 at 0.5 C

图7. (a) NMNO-800极片在循环前的SEM示意图; (b) NMNO-800极片在0.5 C下循环48圈后的SEM示意图

Figure 7. (a) SEM images of the NMNO-800 electrode sheet before cycling; (b) SEM images of the NMNO-800 electrode sheet after 48 cycles at 0.5 C

图8. NMNO-700、NMNO-800和NMNO-900的第二圈(a)和第三圈(b)的CV曲线

Figure 8. The CV curves of NMNO-700, NMNO-800, and NMNO-900 for (a) the second cycle and (b) the third cycle

图9. (a) NMNO-800在充电过程中的ΔEt和ΔEs; (b)三种NMNO在0.2 C倍率下第三次充放电的GITT曲线; (c)由GITT计算的反应电阻; NMNO的钠离子扩散系数: (d)充电, (e)放电; (f) NMNO材料循环100次后的EIS

Figure 9. (a) ΔEt and ΔEs during charge process of NMNO-800; (b) the third charge-discharge GITT curves of three NMNO at 0.2 C rate; (c) reaction resistance calculated by GITT; sodium diffusion coefficient of NMNO: (d) charge, (e) discharge; (f) EIS plot of NMNO material after 100 cycles

	R_e/Ω	R_f/Ω	R_ct/Ω
NMNO-700	21.15	696.6	1540
NMNO-800	22.42	494.5	739
NMNO-900	24.72	1129.0	1129

表3. NMNO的EIS参数

Table 3. EIS parameters of NMNO

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富锰P2/P3双相Na_0.67Mn_0.9Ni_0.1O₂自蔓延燃烧合成与储钠性能

Self-propagating Combustion Synthesis and Sodium Storage Performance of Manganese-rich P2/P3 Biphasic Na_0.67Mn_0.9Ni_0.1O₂

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