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Effect of B and Al co-Doping on Single-Crystal Morphology and Electrochemical Property of Spinel LiMn2O4
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Long SHI1, Yongsheng YANG1, Yuxu LUO2, Junming GUO1, Kaikun WANG3
Journal of the Chinese Ceramic Society | 2025, 53(11) : 3339 - 3351
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Journal of the Chinese Ceramic Society | 2025, 53(11): 3339-3351
• Research Article •
Effect of B and Al co-Doping on Single-Crystal Morphology and Electrochemical Property of Spinel LiMn2O4
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Long SHI1, Yongsheng YANG1, Yuxu LUO2, Junming GUO1, Kaikun WANG3
Affiliations
  • 1.School of Chemistry and Chemical Engineering, Zhaotong University, Zhaotong 657000, Yunnan, China
  • 2.School of Chemistry and Environment, Yunnan Minzu University, Kunming 650500, China
  • 3.School of Materials Science and Engineering, University of Science and Technology Beijing, Beijing 100083, China
  • SHI Long (1984-), male, Ph.D., Associate Professor. E-mail:

About Author:

SHI Long (1984-), male, Ph.D., Associate Professor. E-mail:

Published: 2025-11-20 doi: 10.14062/j.issn.0454-5648.20250107
Outline
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Introduction

Rechargeable lithium-ion batteries (LIBs) are critical energy storage devices widely used in smartphones, electric vehicles, and hybrid vehicles due to their high efficiency and versatility. Spinel LiMn2O4 stands out as a promising cathode material owing to its eco-friendliness, safety, and cost-effectiveness. However, its practical application is limited by rapid capacity fading during cycling, especially under high current densities or elevated temperatures (55 ℃), caused by Jahn-Teller (J-T) distortion, Mn3+ dissolution, and oxygen defects. To address these issues, doping LiMn2O4 with elements like Al3+, B3+, Ni2+, or Mg2+ is a common strategy to stabilize Mn's average oxidation state (+3.5) and suppress J-T distortion. Concurrently, crystal facet engineering optimizes performance: truncated octahedral particles with dominant (111) facets (low surface energy, dense Mn packing) minimize Mn dissolution, while (100)/(110) facets enhance Li+ mobility for improved rate capability. Combining doping and facet control has emerged as a key research focus. For instance, B-doped LiMn1.96B0.06O4 exhibited 110.3 mA·h·g-1 at 5.0 C with 51.8% capacity retention after 2000 cycles, outperforming undoped LiMn2O4. Ni—B co-doping further refined morphology and boosted retention to 70.6%. Similarly, Mg—Al co-doped LiMg0.03Al0.10Mn1.87O4 retained 76.2% capacity after 1000 cycles at 10.0 C, while Zn—Al doping achieved 70%-75% retention over 2000 cycles. These studies highlight how doping regulates crystal growth, favoring truncated octahedral morphologies with balanced stability and kinetics. Building on this, our work synthesizes LiB0.08AlyMn1.92-yO4 (y=0.01, 0.02, 0.04, 0.06, 0.08) via solid-state combustion to study Al doping's impact. Results reveal that Al content modulates facet growth: low doping levels yield two-facet (111/100) truncated octahedrons, while higher doping introduces (110) facets, ultimately leading to quasi-spherical particles. This controlled facet producing strategy is designed to optimize structural stability and electrochemical performance for advanced LIBs.

Methods

LiB0.08Mn1.92O4 and LiB0.08AlyMn1.92-yO4 (y=0.01, 0.02, 0.04, 0.06, 0.08) were synthesized by stoichiometric mixing of Li2CO3, H3BO3, MnCO3, and Al(OH)(CH3COO)2 (total 30 g) with 1.5 g citric acid as a combustion agent. The mixture was ball-milled in ethanol for 10 h, dried, and calcined at 500 ℃ for 1 h. After grinding, it was sintered at 650 ℃ for 6 h. Products were labeled as B0.08 and B0.08Aly. Cathode slurry was prepared by blending active material, carbon black, and PVDF (8∶1∶1) with NMP solvent, followed by 30 min ball milling. The slurry was coated onto Al foil, dried at 80 ℃ for 4 h, and cut into 14 mm discs (active material loading: about 1.0 mg/cm2). CR2032 coin cells were assembled in an Ar-filled glovebox using Li metal anode, LiPF6 electrolyte (1.0 M in EC/DMC/EMC), and Celgard 2320 separator. Material phases were analyzed via XRD (Cu Kα, 10°-80°). Morphology and microstructure were examined by FE-SEM and TEM. Surface composition and valence states were determined via XPS. Electrochemical tests (Land CT2001A) included cycling (25/55 ℃, 3.0-4.5 V) and rate performance. CV and EIS were conducted using a CHI604D workstation.

Results and discussion

XRD analysis confirmed that B0.08 and B—Al co-doped samples crystallized in the spinel LiMn2O4 structure (). B—Al co-doping enhanced crystallinity, with diffraction peaks intensifying until y(Al)≥0.06, beyond which crystallinity declined. A lattice contraction was observed via (400) peak shifts, attributed to smaller B3+/Al3+(0.0400/0.0535 nm) replacing Mn3+(0.0645 nm) and shorter B/Al—O bonds, suppressing J-T distortion. SEM revealed that B—Al co-doping refined particle uniformity and morphology: B0.08Al0.02 exhibited truncated octahedral single-crystals with high (111) and minor (100)/(110) facets, while higher Al content (y≥0.04) led to spherical polyhedrons due to reduced facet growth rates. TEM/SAED confirmed improved crystallinity for B0.08Al0.02, with distinct lattice fringes (0.476 nm for (111)) and ordered diffraction patterns. XPS verified B3+/Al3+ incorporation and a higher Mn4+ ratio (B0.08Al0.02∶ Mn3+/Mn4+=47.29%/52.71%), stabilizing the Mn—O framework. Electrochemical tests demonstrated superior performance for B0.08Al0.02∶ At 5.0 C, it retained 83.9% capacity after 500 cycles (vs. 71.3% for B0.08) due to suppressed Mn dissolution and enhanced Li+ transport from truncated octahedral morphology. High-rate testing (15.0 C, 20.0 C) showed B0.08Al0.02 retained 77.2% capacity after 500 cycles, outperforming B0.08 (58.2%). Elevated-temperature (55 ℃) cycling revealed B0.08Al0.02 maintained 70% capacity retention (200 cycles), attributed to reduced side reactions and structural stability. CV and EIS confirmed faster Li+ diffusion (DLi+: 3.14×10-11 cm2·s-1) and lower charge-transfer resistance for B0.08Al0.02. Kinetic analysis showed a lower activation energy (24.76 kJ/mol vs. 28.53 kJ/mol for B0.08), indicating an enhanced reaction kinetics.

Conclusions

B—Al co-doped LiB0.08AlyMn1.92-yO4 (y=0.01, 0.02, 0.04, 0.06, 0.08) cathode materials were synthesized via solid-phase combustion. B—Al co-doping enhanced crystal growth and facet evolution: particles transitioned from truncated octahedrons with two facets (111, 100) to those incorporating (111), (100), and (110) facets as Al content increased. At y(Al)≥0.04, spherical-like polyhedrons dominated. The optimized LiB0.08Al0.02Mn1.90O4 (B0.08Al0.02) exhibited superior crystallinity and well-defined truncated octahedral single-crystals. B0.08Al0.02 demonstrated exceptional rate capability and cycling stability. At 1.0 C, 5.0 C, 10.0 C, 15.0 C, 20.0 C, and 55 ℃/5.0 C, initial discharge capacities reached 114.7, 102.8, 86.3, 82.6, 75.3, and 107.4 mA·h·g-1, respectively. After 500 cycles, capacity retention rates were 83.9% (5.0 C), 81.9% (10 C), 90.3% (15.0 C), 77.2% (20.0 C), and 62.0% (55 ℃/5.0 C), outperforming other samples. CV and EIS analyses demonstrated superior electrochemical properties for the B0.08Al0.02, including a higher Li+ diffusion coefficient (3.14×10-11 cm2·s-1), a lower apparent activation energy (24.76 kJ/mol), and a reduced charge-transfer resistance (114.2 Ω). These results indicate enhanced Li+ transport kinetics and improved structural stability.

spinel lithium manganese oxide  /  boron-aluminum co-doping  /  cathode material  /  truncated octahedron  /  crystal plane regulation
时龙, 杨永胜, 罗宇旭, 郭俊明, 王开坤. B和Al复合掺杂对尖晶石型LiMn2O4单晶形貌及电化学性能的影响. 硅酸盐学报, 2025 , 53 (11) : 3339 -3351 . DOI: 10.14062/j.issn.0454-5648.20250107
Long SHI, Yongsheng YANG, Yuxu LUO, Junming GUO, Kaikun WANG. Effect of B and Al co-Doping on Single-Crystal Morphology and Electrochemical Property of Spinel LiMn2O4[J]. Journal of the Chinese Ceramic Society, 2025 , 53 (11) : 3339 -3351 . DOI: 10.14062/j.issn.0454-5648.20250107
Year 2025 volume 53 Issue 11
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doi: 10.14062/j.issn.0454-5648.20250107
  • Receive Date:2025-02-19
  • Online Date:2026-10-21
  • Published:2025-11-20
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History
  • Received:2025-02-19
  • Revised:2025-03-09
Funding
Affiliations
    1.School of Chemistry and Chemical Engineering, Zhaotong University, Zhaotong 657000, Yunnan, China
    2.School of Chemistry and Environment, Yunnan Minzu University, Kunming 650500, China
    3.School of Materials Science and Engineering, University of Science and Technology Beijing, Beijing 100083, China

Corresponding:

YANG Yongsheng (1971-), male, Ph.D., Associate Professor. E-mail: ;
GUO Junming (1962-), male, Master, Professor.
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表12种不同金属材料的力学参数
科
Family
属数
Number of
genus
种数
Number of
species
占总种数比例
Percentage of
total species (%)
属
Genus
种数
Number of
species
占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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