We report a new synthesis method to obtain palladium nano-crystals by sol-gel polymerized with acrylamide. From thermogravimetric analysis (TGA) studies, we found PdO and Pd compounds in the xerogel sample, at 550 °C, and over 900 °C we detected only metallic Pd. These results were corroborated by powder X-Ray Diffraction (XRD), High Resolution Scanning Electron Microscopy (HRSEM), and Transmission Electron Microscopy (TEM). XRD studies exhibit the lines from the tetragonal structure (PDF 41-1107) of PdO compound and from the cubic structure (PDF 46-1043) of Pd metallic. HRSEM micrographs show morphologies from the sample very sensitive to heat treatment. Finally, TEM images show crystals of ~8 nm in diameter.