Finally, the insets to Figure show representative SEM images of a secondary particle of approximately 10 µm in diameter and several primary particles of approximately 200 nm diameter. Note the secondary particle morphology is not spherical. These characterizations establish the baseline for observing changes to structure, oxidation state, and morphology during calcination. The evolution of the TM precursor with temperature competes with lithiation. To deconvolute TM precursor evolution from lithiation, we compare TGA of the isolated TM (oxy)hydroxide precursor with that of the TM (oxy)hydroxide precursor-Li 2 CO 3 mixture (Figure and) . Note we employed size-controlled Li 2 CO 3 to improve reaction homogeneity, limited to a particle size <20 µm via sieving, to improve reaction homogeneity; this is the "small-Li LMR" (SL-LMR) case discussed later. 20 µm was selected to keep all precursor particle sizes within 1 order of magnitude in diameter. In both the normal-ized and differential TGA curves, the curve for the isolated precursor and the mixture are nearly identical until approximately 330°C (marked with a teal arrow in Figure and), indicating that the reaction up to this point proceeds independent of the Li source. We attribute this mass loss to the continued dehydration and oxidation of the precursor. Past this temperature, when the two TGA curves diverge, lithiation begins.