Synchrotron X-ray diffraction investigations of two single crystals of
Na_xCoO_2 from different batches with composition x = 0.525-0.530 reveal
homogeneous incommensurate sodium ordering with propagation vector (0.53 0.53
0) at room-temperature. The incommensurate (qq0) superstructure exists between
220 K and 430 K. The value of q varies between q = 0.514 and 0.529, showing a
broad plateau at the latter value between 260 K and 360 K. On cooling, unusual
reversible phase segregation into two volume fractions is observed. Below 220
K, one volume fraction shows the well-known commensurate orthorhombic x = 0.50
superstructure, while a second volume fraction with x = 0.55 exhibits another
commensurate superstructure, presumably with a 6a x 6a x c hexagonal supercell.
We argue that the commensurate-to-incommensurate transition is an intrinsic
feature of samples with Na concentrations x = 0.5 + d with d ~ 0.03.Comment: Corrected/improved versio
