The nonstoichiometric and thermodynamic behavior of the YBa2Cu3Ox system as a function of oxygen partial pressure and temperature is being investigated by means of a coulometric titration technique. The oxygen content of the superconductor can be varied coulometrically by well-defined small amounts and the equilibrium partial pressures determined from the EMF. The oxygen stoichiometry in YBa2Cu3Ox as a function of oxygen partial pressure shows a change of curvature around x = 6.55–6.75 and an inflection around x ≅ 6.65 at temperatures between 400–500°C. These new low temperature data are consistent with the presence of a miscibility gap at lower temperatures, which is similar to that postulated in several theoretical papers.
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