In this study fabrication of Nickel thin filmsbypulsed laser deposition process in vacuum environment was investigated. Nickel thin films were fabricated with different substrate temperatures with Excimer laser KrF 248 nm. By increasing substrate temperature Nickel thin films started to growth at the surface disorderly in which the roughness of thin fimls increased by substrate temperature till 500 ut in 700it decreased and surface of thin films had a regular shape. X-ray diffraction howed that in 700, Ni/Si (100) single crystals start to epitaxial growth in Si direction. Atomic force microscopy howed thatthese single crystals had rectangular parallel sides which revealed the growth direction of single crystals. Ag also were generated by laser ablation in liquid environment with two differen laser appliances:Excimer KrF 248 nm and Nd:YAG1064 nm. Transmission electron microscopy images revealed crystallite nanostructers of Ag. Ag had a beige color after synthesizing. After addingpalladium chloride into product of Ag the color of the Ag changes into milky color which suggested the interattion between Ag and PdCl 2 . The evolution of Ag surface plasmon resonance eaks was traced by optical spectroscopy in 190-1100 nm wavelength range