The process of laser ablation has been adapted to generate nonoparticles from microparticles of the material, referred to as laser ablation of microparticles (LAM). The LAM process has been shown to generate finer nanoparticles than were previously possible through laser ablation of solid targets. In this thesis, a method of generating a 3D nanoparticle network using the LAM process has been proposed using a femtosecond laser. 3D naoparticles were successfully generated through ablation of microparticle samples of lead oxide, nickel oxide and zinc oxide. The size of the nanoparticles in the generated network was significantly reduced in comparison with similar networks generated through laser ablation of solid targets. The method has been further extended to generate a unique alloy nanomaterial through the ablation of the microparticle containing powders of two metals (Aluminum and Nickel Oxide).