Bi/Tl multilayer nanowires have been successfully fabricated using template-based electordeposition by polycarbonate nanoporous template with 100 nm diameter. The growth Bi/Tl multilayer nanowires was performed using dual-bath system containing Bi and Tl salt, respectively. The electrochemical reduction of ions was explored by cyclic voltammetry (CV). The deposition process was controlled with current–time profiles. X-ray diffraction pattern (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) were employed for characterization of crystalline structure and morphology of nanowires. The XRD spectra showed that the lattice structure of Bi segment is rhombohedral and thallium segment has hexagonal lattice structure. The average nanowires diameter was determined from TEM images. Elemental analysis of nanowires was carried out using energy dispersive X-ray (EDX), Rutherford backscattering spectrometry (RBS), and proton induced X-ray emission (PIXE). The length of nanowires was determined by RBS technique. Elemental concentration and weight percent of sample were measured by PIXE analysis
