Synthesis of nanostructured LiM_0.15Mn_1.85 5O₄ (M = Mn, Co, Al, and Fe) particles by spray pyrolysis in a fluidized bed reactor

A novel technique has been developed to directly produce fine ceramic powders from liquid solution via spray pyrolysis in a fluidized bed reactor (SPFBR). Using this technique the preparation of LiM_0.15Mn_1.85O₄ (M = Mn, Co, Al, and Fe), which are the most promising cathode materials for lithium-ion batteries, has been carried out at a superficial velocity U₀ of 0.71 m/s, a reactor temperature T of 800°C, and a static bed height Ls of 100 mm. The as-prepared powders were spherical nanostructured particles that comprised primary particles of a few tens of nanometers in size, and they exhibited a pure cubic spinel structure without any impurities in the XRD patterns. The chemical composition of as-prepared samples showed good agreement with the theoretical values that proved stoichiometric formulae of the compounds. The specific surface area of as-prepared LiM_0.15Mn_1.85 O₄ (M = Mn, Co, Al, and Fe) powders decreases with increasing the static bed height in each doping metal, while the crystallite size increases with the static bed height. As a result, the as-prepared powders showed larger crystallite size and smaller specific surface area than those prepared by conventional spray pyrolysis.