Nanoparticles less than 100nm in size have attracted significant interest over the past 20 years due to their unique properties led by quantum size effect. This chapter evaluates the synthesis methods in liquid phase conducted under operation in high/room temperature and at vacuum/atmospheric environment for nanoparticles and nanostructured materials. We draw attention to the fact that various synthesis methods for formation of colloidally stable matrix-free nanoparticles are available. These methods including chemical stain etching, electrodeposition methods, direct-precipitation methods, sol-gel methods, colloidal synthesis methods, hot-injection synthesis methods, hydrothermal and solvothermal methods, microwave-assisted synthesis methods, ultrasonic synthesis methods, and laser ablation in liquid-phase.