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Starting from the seminal work of De Wolff , we have developed a structural description, based on two kinds of defects, which accounts for the scattering function of all γand ε-MnO2. Using numerical simulation results, we propose simple methods to estimate the parameters which characterize real manganese dioxide samples. Real time neutron powder diffraction has been used to investigate in situ the transformations undergone by γ-MnO2 during thermal annealing and electrochemical reduction in alkaline solutions. We have found that thermally induced transformation from MnO2 to ∝-Mn2O3 can involve up to seven different steps and that electrochemical reduction of γ-MnO2 in KOD electrolyte proceeds through three stages, the final one leading in most cases to a breakdown of the initial crystal lattice.
We have performed electrochemical studies of proton intercalation in several varieties of γ/ε-MnO2 using an original method which combines linear sweep voltammetry and potentiostatic intermittent titration technique. This technique gave for the first time a direct evidence of a two step intercalation process in the ramsdellite units of these compounds. Either 0.5 or 1 proton per manganese are accommodated in the 1×2 channels, as previously suggested by Maskell. The reversibility of these steps has been studied and is discussed in relation to the structural modifications induced by the proton intercalation.
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