Superconducting samples of LazCu04+& are shown by neutron powder diffraction to consist of two nearly identical orthorhombic phases. The primary phase has a stoichiometry near La2Cu04. The second phase is an oxygen-rich phase that is superconducting.The abundance of the second phase increases with the oxygen pressure at which the samples are annealed. Neutron-diffraction measurements as a function of temperature show that the phase separation occurs reversibly near 320 K.
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