Zn/ZnO nanoparticles were prepared by Laser heating gas-evaporation method in this paper, with a 150W CW CO₂ laser as light source and Zinc as a target. The effects of process parameters on nanoparticles have been pilot studied. XRD, ED, TEM and EDTA Complexo- metrictitration, were used to characterize the samples. The experimental results showed that the process parameters such as reaction pressure, the sort and rate of airflow affected the sizes and crystal system of nanoparticles. The products were varied with reaction atmospheres. It was also discovered that Zn and ZnO nanoparticles' diameters were between 35nm and 120 nm in inert gases. While pure acicular ZnO nanoparticles, 75nm in length, and 10nm in width were acquired in the oxygen, and Zn nanoparticles were obtained in the hydrogen, whose diameters were about 23nm. This method is expected to have the possibility of wide applications in the industry in the future.