AbstractThe lattice parameter of Bi/BiSb superlattice nanowire (SLNW) has been measured using in situ high-temperature X-ray diffraction method. The single crystalline Bi/BiSb SLNW arrays with different bilayer thicknesses have been fabricated within the porous anodic alumina membranes (AAMs) by a charge-controlled pulse electrodeposition. Different temperature dependences of the lattice parameter and thermal expansion coefficient were found for the SLNWs. It was found that the thermal expansion coefficient of the SLNWs with a large bilayer thickness has weak temperature dependence, and the interface stress and defect are the main factors responsible for the thermal contraction of the SLNWs.