• Fröhlich, Katja
• Trifonova, Atanaska
• Bärhold, Frank
• Legotin, Evgeny

Abstract

The spray roasting process is recently applied for production of catalysts and single metal oxides. In our study, it was adapted for large-scale manufacturing of a more complex mixed oxide system, in particular symmetric lithium nickel manganese cobalt oxide (LiNi1/3Co1/3Mn1/3O2-NMC), which is already used as cathode material in lithium-ion batteries. An additional lithiation step was coupled with the main process in order to obtain the desired layered structure. Thermogravimetric analysis and high-temperature X-ray diffractometry built the basis for determining suitable synthesis temperature regions for the used chloride precursors and the post-treatment step. The optimized process was proven on an industrial pilot line where a setup for minimum production capacity of 12 kg h−1 was possible. The powder obtained directly after roasting had a very striking morphology compared to the final lithiated product. Hollow aggregates (≥250 μm) with overall 10.926 m2 g−1 surface area and a pore diameter of 3.396 nm were observed. Their well-faceted primary particles were converted into nanosized spheres after lithiation, building a few micrometer big high-porous agglomerates. Actual composition was verified by inductively coupled plasma atomic emission spectroscopy analysis, and the crystal structure and corresponding unit cell parameters were identified and confirmed by Rietveld fit of the derived X-ray diffraction pattern. The initial electrochemical measurements show a 149-mAh g−1discharge capacity, as determined from cyclic voltammetry.

Topics

• porous
• impedance spectroscopy
• pore
• surface
• nickel
• x-ray diffraction
• layered
• thermogravimetry
• cobalt
• Lithium
• Manganese
• cyclic voltammetry
• atomic emission spectroscopy