Synthetic control of composition and crystallite size of silver hollandite, Ag _xMn ₈O ₁₆: Impact on electrochemistry

Synthetic control of the silver content in silver hollandite, Ag _xMn ₈O ₁₆, where the silver content ranges from 1.0 ≥ x ≥ 1.8 is demonstrated. This level of compositional control was enabled by the development of a lower temperature reflux based synthesis compared to the more commonly reported hydrothermal approach. Notably, the synthetic variance of the silver content was accompanied by a concomitant variance in crystallite size as well as surface area and particle size. To verify the retention of the hollandite structure, the first Rietveld analysis of silver hollandite was conducted on samples of varying composition. The impacts of silver content, crystallite size, surface area, and particle size on electrochemical reversibility were examined under cyclic voltammetry and battery testing.