In recently years, the many alluring methods to prepare the inorganic-organic hybrid nanomaterials have garnered great interest. The in-situ growth phenomenon is the most straightforward way to from these compounds with multiply dimensions. Here in, we demonstrate the in-situ synthesis of noble metal nanoparticles-polyacrylonitrile nanofibers (M NPs-PAN NFs) using electrospinning route. Synthesis includes two main paths in the presence of DMF. In the first path, the M NPs were prepared from the precursor solution using in-situ reduction route in the presence of ultrasound irradiation and DMF (as solvent and weak reducing agent) at 60 °C for 9 min. The mechanism of our second path exhibited that the polymer matrix solution (PAN/DMF) acts as an appropriate host solution for the MNPs, due to possessing high contents of effectiveness groups. These groups not only anchor NM NPs tightly in PAN fibers via dipole-induced dipole interactions but also they stabilize metal nanoparticles by good bonding interaction with their surface atoms. After preparing all nanofibers, TEM images revealed that both M NPs and their related nanofibers have particular and unique shape without agglomerated particles with different sizes. Field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDS) with SEM-mapping images, and Fourier-transform infrared (FT-IR) were also applied to verify the formation all samples. In this report, we tried to present a preparative synthesis strategy to preparation of nanofibers.