Transition metal-doped spinel cathode materials of LiM0.1Mn1.9O4 (M: Co, Ni, Cr) were prepared by solid-state reaction. The structure and morphology of the products were investigated by X-ray photoelectron spectroscopy, X-ray diffraction, Rietveld refinement and SEM-EDX. The oxidation states of Mn, Co, Ni and Cr were found to be 3+/4+, 2+, 2+ and 3+, respectively as revealed by X-ray photoelectron spectroscopy. SEM-EDX shows uniform particles and the particle size was about 200-700 nm ranges. The diffraction peaks of the prepared solids corresponded to a single phase of cubic spinel structure with a space group Fd3m. Doping of Co, Ni and Cr causes lattice parameters to decrease. The prepared materials have ionic conductivity where LiCo0.10Mn1.90O4 has the highest capacitance. Asian Journal of Chemistry; Vol. 29, No. 7 (2017), 1466-1470 We mainly focus on analysis of physico-chemical properties of LiM0.1Mn1.9O4 cathodes by X-ray photoelectron microscopic measurement, X-ray diffraction, SEM-EDX and AC impedance measurement.
EXPERIMENTALSynthesis of MnO2 and LiMxMn2-xO4: An analytical grade of Mn(CH3COO)2 and Na2S2O8 (Aldrich) were used to prepare MnO2 nanorods by reflux technique. All other chemicals were used without as they were received. In a typical synthesis, Mn(CH3COO)2 and Na2S2O8 were dissolved at room temperature with a molar ratio of 1:1 in 80 mL deionized distilled water by magnetic stirring to form a clear homogeneous solution. The mixed solution was transferred into boiling flask and heated at 120 °C for 12 h. The obtained powder was subsequently dried at 110 °C for 12 h in air [19].A typical synthesis of LiM0.10M1.90O4 is as the following. 1 mole of LiOH, 0.10 moles of Co(CH3COO)2 and 1.90 mol of as-synthesized MnO2 were dispersed into high purity ethanol to form a thick slurry, stirred to form fine mixture for several hours and dried at room temperature. The above process was repeated two to three times to produce a well-mixed powder. The LiMn2O4 powder was then ignited at 750 °C for 10 h. The same procedure was used for synthesis LiMn0.10Mn1.90O4, LiNi0.10Mn1.90O4 and LiCr0.10Mn1.90O4 [20,21].Characterization of LiM0.10Mn1.90O4 microstructure: The cathode material underwent X-ray photoelectron