The miscibility gap of La2CUO4+delta was investigated by studying thre
e electrochemically oxygenated samples with different oxygen contents,
using variable-temperature neutron powder diffraction. The low-temper
ature lattice parameters of the two coexisting orthorhombic phases (an
tiferromagnetic, Bmab and superconducting, Fmmm) were found to be in g
ood agreement with those determined for high-pressure annealed samples
, indicating that the two techniques yield essentially identical sampl
es, at least in this concentration range. A sample with delta almost-e
qual-to 0.032 remained phase separated up to 415 K and, above this tem
perature, was found to be single-phase tetragonal (F4/mmm). The phase
separation temperature and the orthorhombic-to-tetragonal phase transi
tion temperature were obtained for all samples, allowing the shape of
the miscibility gap to be determined.