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Volume 113
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Morphological changes and migration accumulation of fluorine during the thermal reduction process of high-nickel ternary electrode materials
Xueying He a, Wenzhe Wang a, Bu Chu a, Weining Xie a b *, Jie Wang a, Linhan Ge c *, Tao Zhang d, Shuai Wang a b, Yi Feng e
a School of Chemical Engineering, China University of Mining and Technology, Xuzhou, 221116, China
b Advanced Analysis & Compuration, Center, China University of Mining and Technology, Xuzhou, 221116, China
c Institute of Nuclear and New Energy Technology, Tsinghua University, Beijing, 100084, China
d Beichen Advanced Recycling Technology (Qingdao) Co., Ltd, Qingdao, 266041, China
e School of Minerals Processing and Bioengineering, Central South University, Changsha, 410083, China
10.1016/j.partic.2026.02.030
Volume 113, June 2026, Pages 12-21
Received 7 January 2026, Revised 6 February 2026, Accepted 18 February 2026, Available online 14 March 2026, Version of Record 31 March 2026.
E-mail: 5718@cumt.edu.cn; linhan.ge@hotmail.com
Highlights

• Fluorine migration and accumulation during crushing, screening and thermal reduction of high-nickel mixed electrodes.

• Fluorine in binders and electrolytes is quantified to show its migration in particles.

• Fluorine distribution and evolution are characterized to clarify its transformation during thermal reduction.

• Fluorine distribution and elemental states were analyzed by XPS and SEM-EDS for raw and optimally reduced samples.


Abstract

This study investigates the migration and distribution of fluorine in high-nickel cathode and anode mixed materials during crushing, screening, and thermal reduction. Crushing and screening results show that 78.76% of the particles are smaller than 0.125 mm, where fluorine (mainly from LiPF6 decomposition) and cathode materials are concentrated. Thermal reduction experiments indicate that 650 °C is the optimal temperature, at which cathode materials are deeply reduced to form water-soluble Li2CO3, and the lithium leaching efficiency reaches 75.6%. Lower temperatures result in insufficient reduction, while higher temperatures cause Li2CO3 decomposition and LiF formation, thus reducing lithium leaching efficiency. XPS and thermogravimetric analyses reveal that fluorine-containing intermediates react with metal oxides to form metal fluorides, which enrich in fine particles and increase fluorine content. Thermal reduction breaks P–F bonds and raises the proportion of Li–F, but only removes surface fluorine pollutants rather than internal fluorides.

Graphical abstract
Keywords
High-nickel lithium-ion batteries; Thermal reduction; Migration law of fluorine elements; Lithium leaching efficiency
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