48
3 Optimization of the Synthesis of Combinatorial Samples
the carbonate precipitator resulted in the formation of lithium stearate on the surface
of the substrate.
The map of lithium loss in Fig. 3.1 shows that samples can be prepared throughout the Gibbs triangle with the exception of samples near the Li corner where the
formation of lithium peroxide vapor prevents coexistence with lithium oxide. Consequently, the issue of lithium loss in the Li–Mn–Ni oxide pseudo-ternary system is
manageable with the methodology developed here and is used throughout the rest of
this thesis for combinatorial synthesis. All other Li–Mn–Ni–O samples were therefore heated at 800
◦ C for 3 h in oxygen. Various cooling rates were used, but the
heating rate was always 5
◦ C/min. The only variation for Li–Co–Mn–O materials
was that they were heated in air in a box furnace since it was found that lithium loss
was much smaller for these samples as discussed in the next chapter.
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