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CERAMICS INTERNATIONAL · 2025 · IF 5.6

Effect of lithium bis(trifluoromethanesulfonyl)imide on 3D-printed lithium iron phosphate electrodes

Tielin Wang,Lijie Zhai,Mengting Lv,Jiahao Ji,Tao Lin,Fang Lian,Nan Meng,Huiping Shao

With the rapid advancement of microelectronic devices, 3D printed batteries hold significant potential for development in the battery fields. In this study, the network-structured lithium iron phosphate (LFP) electrodes containing lithium bis(trifluoromethanesulfonyl)imide (LiTFSI) were prepared by 3D gel printing (3DGP) technology and the effect of different LiTFSI content on 3D-printed LFP electrodes was investigated. With increasing the LiTFSI content from 0 to 10 wt%, the apparent viscosity of the 3D printing slurry showed a gradual increase. The printing slurry of 3 wt% LiTFSI showed an apparent viscosity of 9.43 Pa s at a shear rate of 129 s −1 with the 0.16 mm inner diameter printing needle and 0.60 MPa air pressure, and the 3 wt% LiTFSI electrode printed maintained the intact network structure and the printing lines were uniform. The LFP electrodes with LiTFSI contents of 0 wt%, 3 wt%, 6 wt% and 10 wt% showed respectively specific capacities of 147 mAh g −1 , 142 mAh g −1 , 139 mAh g −1 and 127 mAh g −1 at 0.1C. After 0.5C and 300 charge-discharge cycles, the specific capacities of the electrodes were respectively 108.6 mAh g −1 , 104.7 mAh g −1 , 101.6 mAh g −1 and 99 mAh g −1 , and the capacity retention are respectively 87 %, 85 %, 85 % and 88 %, which indicates that these electrodes are cyclically stable and provide some reference for printing composite electrodes.

CAS / MDL: 872-50-4 90076-65-6
研究领域: 材料科学 · 电池技术
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SEPARATION AND PURIFICATION TECHNOLOGY · 2024 · IF 8.1

Waste to treasure: A sustainable technic to prepare high-performance lithium iron phosphate from laterite nickel tailings

Zhi-Zhong Shen,Rui-Xiang Wang,Hong-Yan Yuan,Yong Guo,Dan Xiao,Yan Meng

The abundance of laterite nickel tailings after nickel extraction not only generate severe environmental contamination but also result in significant waste of metal resources, particularly iron (Fe). Herein, a promising technic of recycling tailings to high-value Fe-based energy storage materials is developed to address above challenges. The traditional hydrometallurgy is firstly applied to leach Fe source from laterite nickel tailings. By referencing the Eh-pH thermodynamic stability phase diagram of the phosphorus system, Fe could be preferentially precipitated in various metal elements, enabling the effective extraction of Fe as raw iron phosphate (FePO 4 ). Notably, a two-step purification strategy is designed to remove residual impurity and adjust Fe/P ratio, subsequently obtaining the high-purity battery-grade FePO 4 . Finally, a solid-phase method is conducted to prepare nano lithium iron phosphate (LiFePO 4 ) with outstanding electrochemical performance (1C > 150 mAh/g), meeting rigorous commercial standards. Economic analysis further confirms the significant value of implementing this scalable recycling technic, and the potential industrial application is highly anticipated. Thus, this research proposes a sustainable tailings recovery methodology, offering valuable insights for the recycling of other Fe-containing resources.

CAS / MDL: 554-13-2
研究领域: 材料科学 · 环境科学 · 能源存储
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Journal of Water Process Engineering · 2025 · IF 6.7

Phosphorus recovery from simulated anaerobic fermentation supernatant through vivianite crystallization: the role of aluminium and its implications for the synthesis of LiFePO4

Shilong Wang,SuNa Wang,Weiyi Zhao,Shiyu Fang,E. Yang,Runze Xu,Fang Fang,Weijing Liu,Jiashun Cao,Song Cheng

Recovering phosphorus (P) from wastewater benefits both the environment and the field of clean energy. Vivianite is a key precursor for clean energy lithium batteries, making it a highly valuable and promising product in wastewater P recovery. As a widely used cathode material in lithium-ion batteries, LiFePO 4 is valued for its excellent thermal stability, safety, and long cycle life, making it a promising material for sustainable energy applications. However, the large amount of aluminium (Al) present in the recirculated sludge can be released into the supernatant during the anaerobic digestion process, which affects the recovery of vivianite and further impacts the performance of LiFePO 4 . This study investigated the effect of Al on vivianite crystallization throughout the P recovery process and explored the direct synthesis of LiFePO 4 using Al-containing vivianite. Varying initial Al concentrations were examined to understand their influence on the crystallization kinetics, purity, and morphology of vivianite. At low Al concentrations (1–50 mg/L), Al formed amorphous aluminium phosphate that attached to vivianite crystals via electrostatic interactions and surface adsorption. At high Al concentrations (100–300 mg/L), Al predominantly entered the solid phase through co-precipitation, significantly inhibiting vivianite formation. LiFePO 4 /C cathode materials were synthesized using the recovered Al-containing vivianite. The results revealed that Al existed as inert substances within LiFePO 4 /C, reducing its crystallinity and specific discharge capacity. These findings elucidate how Al affects vivianite crystallization during P recovery and provide theoretical insights for converting Al-containing vivianite into value-added LiFePO 4 .

研究领域: 环境科学 · 能源材料科学
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SEPARATION AND PURIFICATION TECHNOLOGY · 2024 · IF 8.1

Recycle of spent LiFePO4 batteries: An eco-friendly closed-loop technique based on less solvent solid state reaction

Zhiliang Guo,Shuai Ji,Changgan Lai,Donghuai Zhang,Liu Nie,Yujie Hou,Yuli Zhang,Yifan Zhang,Ling Bai

Lithium iron phosphate (LFP) batteries have become one of the most popular batteries due to their high safety and low cost. However, the lifespan of LFP batteries is limited, making effective recycling processes crucial for environmental protection, resource conservation, and economic benefits. Less solvent solid state reaction (LSR) is reactions of solids with the help of a little solvent, which has advantage of almost 100% conversion of reactants and no waste generation. Herein, LFP (S-LFP) from spent batteries was first entirely decomposed to produce FePO 4 and LiH 2 PO 4 in H 3 PO 4 -H 2 O 2 leaching systems using the LSR method. Then, battery-grade Li 2 CO 3 was prepared by adding CaCl 2 and Na 2 CO 3 to LiH 2 PO 4 . As a result, the battery of regenerated LiFePO 4 (R-LFP) using recycled FePO 4 and Li 2 CO 3 exhibits superior electrochemical performance compared to those with unused LiFePO 4 , including a higher discharge specific capacity (140.7 mAhg −1 at 0.1C) and excellent cycle life, with a capacity retention of 98.6% over 500cycles at 1.0C. The LSR method provides a green and sustainable closed-loop recovery strategy for S-LFP cathode materials, which reduces the number of processing steps and chemical consumption, promotes resource conservation and environmental protection, and facilitates the sustainable industrial development of S-LFP batteries.

研究领域: 材料科学 · 环境科学 · 化学工程
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JOURNAL OF POWER SOURCES · 2024 · IF 8.1

Value-added recycling of spent LiFePO4 by a FeCl3 leaching-spray pyrolysis approach

Zhao Zhao,Yan Li,Ziyu Chen,Chengzong Li,Haibin Zeng,Chengming Du,Tao Li

Traditional recycling technologies for spent lithium iron phosphate (LiFePO 4 , LFP) usually suffer from issues such as complex procedures, heavy chemical consumption, and limited economic viability. Herein, we propose a method combining FeCl 3 leaching and spray pyrolysis for the high-value-added recycling of spent LFP. Using FeCl 3 as leaching agent, over 99 % of Li is selectively leached out within 30 min with a solid-liquid ratio up to 300 g L −1 . The resulting leaching residue (FePO 4 ) serves as a precursor for the synthesis of new LFP. Subsequently, the Li and Fe-containing leachate undergoes a spray pyrolysis process, yielding a pyrolysis powder comprising LiCl and Fe 2 O 3 . Through a water-leaching procedure, the separation of LiCl and Fe 2 O 3 is achieved based on their distinct solubility in water. The resulting high-purity LiCl solution and Fe 2 O 3 residue are directly utilizable for producing battery-grade Li 2 CO 3 and LFP cathodes, respectively. LFP/C cathodes, synthesized using the recovered Li 2 CO 3 and FePO 4 precursor, exhibit an impressive 99.8 % capacity retention after 200 cycles at a 1C rate. This method holds great economic and environmental benefits by producing high-value-added products while avoiding the consumption of acids or alkalis.

研究领域: 材料科学 · 环境工程 · 化学工程
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International Journal of Applied Ceramic Technology · 2019 ·Vol. 17 ·期 3 ·1231-1240 · IF 1.074

Application of the factorial design of experiments to hydrothermal synthesis of lithium iron phosphate

Zuolin Liu,Yongming Zhu,Peng Gao,Zhizhou Zhang

The mathematical model of lithium iron phosphate prepared by hydrothermal method was established by factor experimental design. The effect of individual variables and their interactions were studied by the main effects plot and Interaction plot. The influence of ascorbic acid dosage on the discharge specific capacity was greater than the hydrothermal time and the hydrothermal temperature, and the influence degree of the latter two was equivalent and the interaction effect of hydrothermal time and ascorbic acid dosage has the greatest influence on the discharge specific capacity in three interaction effects. The optimized hydrothermal condition was hydrothermal time of 9 hours, hydrothermal temperature of 210°C and ascorbic acid dosage of 1.5 mmol in the experimental design range, with the initial discharge specific capacity of 0.1 C as 152.5 mAh g −1 . The corresponding characterization was performed using electrochemical methods, XRD, SEM, and TEM. This study provided a protocol to factorially design better experiments to achieve excellent battery criterion in the context of lithium iron phosphate preparation.

研究领域: 材料科学 · 电化学
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IONICS · 2017 ·Vol. 24 ·期 3 ·671-679 · IF 2.062

An efficient process to fabricate spherical hierarchical LiFePO4/C cathode composites with controllable coating thickness

Yan Yinglin,Li Qiaole,Ren Bing,Yang Rong,Xu Yunhua,Zhong Lisheng,Wu Hong

Hierarchical lithium iron phosphate/carbon (LiFePO 4 /C) microspheres were fabricated successfully using a facile spray drying-assisted coprecipitation method. A relatively short calcination time and a relatively low calcination temperature were adopted to prepare the hierarchical LiFePO 4 /C microspheres. The hierarchical microspheres consisted of nanoparticles with a uniform coating of amorphous carbon. The thickness of the carbon layer was controlled by the addition of glucose. The hierarchical LiFePO 4 /C microspheres exhibited a high tap density and a large specific surface area. The electrochemical properties of the sample were investigated. The sample exhibited a better rate capability and a better cyclability than the coral-like LiFePO 4 /C cathode material, and these were ascribed to the highly uniform carbon coating and the self-assembled nanoparticles.

CAS / MDL: 1310-66-3
研究领域: 材料科学 · 电化学
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ACS Sustainable Chemistry & Engineering · 2023 · IF 8.4

Simplifying and Optimizing Li4SiO4 Preparation from Spent LiFePO4 Batteries with Enhanced CO2 Adsorption

Jiaqi Ruan,Yichao Tong,Jingyu Ran,Changlei Qin

A large amount of spent lithium batteries, especially lithium iron phosphate (LiFePO4), is discarded due to their limited lifespan and poses a great threat to the environment. At the same time, the potential application of Li4SiO4, an efficient high-temperature CO2 sorbent, is largely limited by the high cost of lithium resources. Thus, the preparation of Li4SiO4 from spent LiFePO4 batteries has great potential for achieving waste recycling and reducing CO2 capture costs. However, the process of recycling spent LiFePO4 batteries to synthesize Li4SiO4 sorbents still needs to be well investigated. This work proposes to simplify the preparation scheme by combing precipitation, Na doping, and synthesis processes and further optimizing the key variables of pH, Na2CO3 ratio, and heating rate. An optimal condition is determined to be pH = 9, Na2CO3 ratio = 11 wt %, and heating rate = 5 °C/min, and the sorbent prepared shows a superior stable CO2 capacity of 0.24 g/g in 80 adsorption/desorption cycles. The work develops an effective Li4SiO4 preparation scheme from spent LiFePO4 batteries with largely enhanced CO2 adsorption performance and reduced cost and could achieve a win–win situation in waste recycling and CO2 mitigation.

研究领域: 材料科学 · 环境科学
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ACS Sustainable Chemistry & Engineering · 2024 · IF 7.1

Potassium Pyrosulfate-Assisted Roasting and Water Leaching for Selectively Li and Fe Recycling from Spent LiFePO4 Batteries

Haozheng Hu,Xianghao Meng,Yin Li,Yusong Yang,Yanqiu Xu,Junxian Hu,Yaochun Yao

In the era of extensive deployment of LiFePO4 batteries in energy storage and electric vehicle domains, the recycling of lithium from spent LiFePO4 (SLFP) batteries has emerged as a focus, which helps in alleviating environmental pollution and resource shortages. Traditional recycling techniques, encompassing pyrometallurgical and hydrometallurgical methods, are often marred by low selectivity and extraction efficiency. Herein, an eco-friendly and low-consumption recycling strategy involving potassium pyrosulfate (K2S2O7)-assisted low-temperature roasting and subsequent water leaching has been developed for selectively recycling Fe and Li from SLFP batteries. The proposed strategy, compared to the conventional inorganic acid leaching method, mitigates the environmental hazards caused by acidic wastewater generation and reduces the costs associated with wastewater treatment. Investigations of thermal performance characterization and thermodynamic calculation analyses have revealed that K2S2O7 plays a pivotal role in extracting lithium from the Fe–P–O framework, converting lithium into a soluble sulfate variant and iron into insoluble compounds. This process culminates in the segregation of a lithium-rich leachate and an iron-enriched residue, which are further processed to synthesize Li2CO3 and FePO4. The effects on Li leaching of the mass ratio of K2S2O7 to SLFP, roasting time, roasting temperature, and water leaching time are systematically studied and 95.87% Li was leached in water under optimal conditions. In addition, the feasibility of the strategy was further illustrated by the regeneration of LiFePO4 produced by the recycled Li2CO3 and FePO4. Overall, this recovery strategy stands out for its effective lithium-iron segregation, environmental sustainability, and economic viability, which provide some inspiration for high-efficiency and environmentally friendly recovery metal from spent lithium-ion batteries.

研究领域: 材料科学 · 环境科学
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ELECTROCHIMICA ACTA · 2014 · IF 4.086

Fabrication and characteristics of spherical hierarchical LiFePO4/C cathode material by a facile method

Liang Ni,Jugong Zheng,Cancan Qin,Yanwen Lu,Panxing Liu,Tongfu Wu,Yuefeng Tang,Yanfeng Chen

Spherical hierarchical LiFePO 4 /C cathode material was fabricated by a facile sol spray drying method using FePO 4 •2H 2 O, LiOH, oxalate acid (H 2 C 2 O 4 •2H 2 O) and sucrose as raw materials. A relatively low drying temperature 180   °C was adopted in order to form a uniform and thin carbon layer on the surface. The LiFePO 4 /C sample was characterized by physical and electrochemical measurements and the influence of the specific morphology on the electrochemical property was investigated. This cathode material had a reversible capacity of 160.9   mAh   g −1 at 0.1   C and maintained 105.8   mAh   g −1 at as high as 20   C with superior cycling performance. The excellent electrochemical property should be attributed to the carbon coated nanoparticles and a large specific surface area (36.5   m 2 g −1 ) provived by the spherical hierarchical structure.

研究领域: 材料科学 · 电化学
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IONICS · 2022 ·Vol. 28 ·期 3 ·1073-1080 · IF 2.961

Synthesis of PANI and its application in LiFePO4 cathode material

Han Jia-Jun,Guo Ao-Ran,Wang Yan-Fang

Polyaniline (PANI) was synthesized by adsorption double oxidizer method, and then reduced with N 2 H 4 ·H 2 O (r-PANI), doped with HClO 4 (d-PANI). PANI with different states was combined with lithium iron phosphate (LiFePO 4 ) in water-based slurry to form PANI/LFP composites. Some physical characterization methods (Fourier transform infrared spectroscopy analysis, scanning electron microscope) were used to analyze the morphology and structure of the composites. The electrochemical properties were characterized by cyclic voltammetry, impedance spectroscopy, galvanostatic charge/discharge, and rate capability. The specific capacity of the r-PANI/LFP composite reached 154 mAh/g, which was 4.1% higher than that of pure LFP, and the coulombic efficiency of the battery was close to 100%. Under the higher discharge rate conditions, the r-PANI/LFP composite still released a good reversible capacity. Moreover, the cyclability and rate capability of the r-PANI/LFP composites are better than that of pure LFP.

研究领域: 材料科学 · 电化学
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ELECTROCHIMICA ACTA · 2023 · IF 6.6

Elucidating in-situ heat generation of LiFePO4 semi-solid lithium slurry battery under specific cycling protocols

Siyuan Cheng,Lihua Jiang,Zesen Wei,Xiangdong Meng,Qiangling Duan,Huahua Xiao,Jinhua Sun,Qingsong Wang

Semi-solid lithium slurry battery combines the advantages of the high energy density of lithium-ion battery and the flowability of flow battery electrodes and has attracted attention in energy storage. Elucidating the heat generation during cycling is crucial for evaluating the safety. However, there is a relative lack of research in this field of semi-solid lithium slurry battery. Herein, the heat generation of lithium iron phosphate (LiFePO 4 ) semi-solid lithium slurry battery during cycling under specific cycling protocols is investigated in this work. The results show that the battery has lower heat generation when cycling at an ambient temperature of 35–50 ℃ and a charging cutoff voltage below 4.0 V, meanwhile, it maintains considerable capacity. However, when the charging cutoff voltage exceeds 4.4 V, the cyclic heat generation of the battery increases significantly, and the capacity attenuates significantly. Meanwhile, the classical equation for calculating battery heat generation of lithium-ion battery is no longer reliable. This is mainly because the electrolyte content of the semi-solid lithium slurry battery is too high (over 80 %), and at high charging cutoff voltage, the side decomposition reactions of the electrolyte increase significantly. Subsequent characterization of electrode materials also confirms this inference. This study can provide a clearer understanding of the safety of semi-solid lithium slurry battery and has guiding implications for industrial applications.

研究领域: 能源存储 · 材料科学
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