In this paper, we report on the preparation of bare and Mg-doped Li(Mg x Co 1-x )O 2 (x = 0, 0.03, 0.05) phases by a molten salt method and their electrochemical properties. They were prepared at 800 °C for 6 h in air. Rietveld refined X-Ray Diffraction data of bare (x = 0) and charge capacity values at the 60 th cycle to be: 147 (±3) mAh g -1 (x = 0), 127 (±3) mAh g -1 (x = 0.03), and 131 (±3) mAh g -1 (x=0.05) cycled at a current density of 30 mA g -1 . Capacity retention is also favourable at 98.5 %.
Oxygen non-stoichiometry in layered rock salt structure cathodes can have a major deleterious effect on their performance in Li batteries. The effect of preparation conditions - temperature, atmosphere and cooling rate - on oxygen non-stoichiometry and consequent interlayer cation mixing in the layered rock salt material LiNi0.8Mn0.1Co0.1O2-δ has been investigated using a combination of X-Ray powder diffraction, including Rietveld refinement and thermogravimetry. Oxygen content varies over the approximate range ∼0≤ δ ≤ ∼ 0.23; oxygen deficiency is greatest in samples fired at high temperatures in N2. Interlayer mixing occurs as a direct consequence of oxygen deficiency and leads to reduced cathode capacity and performance; samples with least oxygen deficiency and most cation order were obtained on firing in O2 at ∼900–950°C. Attention to the optimisation of oxygen stoichiometry should be an important generic consideration during cathode preparation.
This paper discussed refinement strategy that been used to reveal crystallographic properties of lithium-based complex oxides with layered rock salt structure. Rietveld analysis using XRD data was used to determine the amount of interlayer mixing and estimate oxygen contents. The structural model and refinement methodology was controlled and validated initially using a standard sample. Thus, this paper summarized structure refinement strategy that been used to quantify the degree of cation order associated with interlayer mixing and investigate the sensitivity of laboratory XRD data to oxygen non-stoichiometry that recently published elsewhere [.
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