The raw materials namely, 99.9% purity La2O3 and Co3O4 from Fluka were metered in the stoichiometric ratio to lead to the formation of LaCoO3. The mix was homogenized by mechanical activation in a Fritsch Pulverisette 5 planetary mill (150 rpm) with a 10:1 ball:mix ratio. The BIM 23042 duration varied from 2 to 20 h, and alcohol was employed as wetting agent. Upon grinding, the alcohol was exhausted after oven-heating at 60 °C. The particle size distribution upon grinding and drying was determined using a Brookhaven 90 Plus particle size analyzer. The morphology of the powders was determined using scanning electron microscopy on a FEG–SEM–FIB Auriga Workstation at 5 kV. Thermal analysis to determine the behavior of the powders at thermal treatment was carried out on a STA 449 F3 Jupiter machine. The phase composition of the raw materials and the powders after drying was determined by X-ray diffraction in the 2θ=20–70° range by using a Shimadzu 6100 diffractometer with a CuKα (λ=1.5402 Å) radiation source. The mechanically activated powders were Ø 10 mm uniaxially pelleted at 100 MPa in a Meyer SPA43-25/350 press. The pellets were thermally treated from 1000 °C to 1250 °C for 2 h at the higher temperature. The pellets were burned in a Nabertherm GmbH laboratory furnace. The phase composition of the pellets was determined by X-ray diffraction.