Abstract

The novel wet-chemical method for the analysis of the concentration and the distribution of constituent(s) at a higher oxidation state, [CuO] +, in superconducting La 2− x Sr x CuO y was developed. The sample pellet was dissolved in a flow of acid solution containing Fe 2+, and the solution was introduced continuously into a flow-coulometric system composed of two-step column electrodes of glassy carbon fibers as working electrodes. Fe 3+ generated in the solution through the stoichiometric redox between [CuO] + and Fe 2+ was detected at the first column electrode, and Cu 2+ in the dissolving solution was detected at the second column. It was obvious that the [CuO] + concentration in the surface region of ca. 200 μm in depth from the surface was lower than that of the bulk pellet and the distribution of [CuO] + near the surface was dependent on such sample-preparation parameters as sintering time, annealing atmosphere and storage time of the pellets, etc.

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