Copper-tin (CuSn) nanomaterials have been receiving substantial attention due to their excellent thermal, electrical, and optical properties. However, how such properties are affected based on heat treatment temperature and chemical composition of copper and tin is still not very well understood. In this paper, CuSn nanofibers were fabricated by electrospinning a precursor solution of polyacrylonitrile, copper, and tin. Calcination temperatures were selected using thermogravimetric/differential thermal analysis (TG/DTA) and Fourier transform infrared (FT-IR) results. Analytical techniques such as scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and ultraviolet photoelectron spectroscopy (UPS) were employed to investigate the physicochemical properties of the CuSn nanofibers. SEM images and EDS revealed the formation of pores on the nanofibers and high concentrations of tin were in the core, while copper was located on the surface. XRD results confirmed the monoclinic phase of Cu 6 Sn 5 for the CuSn nanofibers because peaks for diffraction angles at 27.6°, 53.4°, and 60.0°were observed. XPS results showed that Cu-C and Sn-C bonds occur at binding energies around 932 and 484 eV, respectively. The work function of the CuSn NF heat treated at 150°C was calculated from the UPS spectra, and the value was 4.19 eV.