Synthesis of Li-ion battery cathode materials via freeze granulation

Keivan Amiri Kasvayee
Department of Materials and Manufacturing Technology
Chalmers University of Technology

Göteborg, Sweden

Synthesis of Li-ion battery cathode materials via freeze granulation


Recently, enormous efforts have been done within the development of Li-ion batteries for use in portable electric devices from small scale applications such as mobile phones, digital cameras, laptop computers, to large scale applications like electrical vehicles (EVs) and hybrid electric vehicles (HEVs). LiFePO4 as an active material in cathode materials in Li-ion batteries has shown outstanding advantages compare to other cathode materials such as low cost, low toxicity and environmental compatibility, good thermal stability, high theoretical specific capacity of 170 mAh/g and operating reversibility at 3.4V. Still, it is a need to develop the manufacture of the cathode material to achieve improved performance reliability by using  environmental sustainable processes in order to meet future demands in large scale production and uses of Li-ion batteries.
The aim of this work was to develop a non-toxic, cheap, efficient and environmentally friendly process for synthesis of high quality active cathode material based on LiFePO4 for Li-ion batteries. Water based suspensions/solutions containing various reactant constituents have been homogenized, granulated and calcined. Freeze granulation was applied as the key tool for the synthesis of LiFePO4 with integrated carbon in order to produce granules with high degree of homogeneity prior to calcination. The resulting powder materials have been evaluated by XRD, carbon and conductivity measurements and characterization of other physical properties such as density and specific surface area. The promising version was used for manufacture of cathode material by tape casting, cell assembling and evaluation of the performance by charge/discharge cycling of the cells.
For the best sample in our experiment the XRD results revealed a high degree of purity, homogeneity and crystallinity of LiFePO4. The produced LiFePO4/C composite also had a high specific surface area and, therefore, considered as a promising material for cathode manufacturing and cell assembly. A discharge capacity of 155 and 140 mAh/g was achieved at the fifth cycle at 0.1C rate at room temperature for the cathodes which were made with NMP (solvent based) and water system, respectively. The long-term stability test indicated good result with no loss in capacity for at least 390 cycles. The satisfactory discharge capacity should be attributed to the homogenous nano-sized particles with a conductive porous carbon structure that was provided by the freeze granulation process and adapted calcination process.


Li-ion batteries, LiFePO4, cathode active material, specific capacity, freeze
granulation, calcination, LiFePO4/C composite, cell assembly.

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