In this thesis, Gold-Iron (Au/Fe) core-shell binary nanoparticles () were synthesized using Nd:YAG pulsed laser ablation in different reactive liquid environment of Iron III chloride (FeCl 3 ) solutions. The different reactive aqueous solutions were prepared with equal amount of FeCl 3 .6H 2 O and Hydrochloric acid (HCl) for each solution, but in different order of dissolving the components in water. So different order in dissolving of the solutes yielded the different solutions in chemical properties. Laser ablation of gold target in pure water and in each mentioned reactive solutions was done. Physical and chemical properties of the synthesized characterized by ICP, XRD, UV-Vis spectrophotometry, XPS, TEM, HRTEM-EDS and STEM-HAADF. XRD results showed that Au well crystalized in simple cubic lattice and Akaganéite formed in tetragonal phase. Optical properties by UV-Vis spectrophotometry exhibited different behavior for Surface Plasmon Resonance (SPR) of gold in each solution. More width and wavelength of SPR was related to bigger size and wider size distribution of while less width and wavelength of SPR was related to smaller size and sharper size distribution of . Also, less colloidal stability of and SPR peak damping during time indicated interaction between the gold surface and Akaganéite as a shell. Surface chemical properties of by XPS didn't revealed any binding energy band related to Au4f, indicating surface covered gold by a Fe component shell. Investigating binding energy of Fe2p and O1s showed a large fraction of Iron Hydroxide. TEM images confirmed formation of a shell. Gold weren't spherical in the reactive solutions. Measuring planar d-spacing by HRTEM, Z-contrast and chemical analysis by STEM-HAADF and EDS system revealed the different shell composition, Akaganéite and Iron Oxide, regarding different solutions.