Silver, nickel, nickel oxide and silver-nickel alloys have been produced from their inexpensive liquid precursors using CO2 and Nd-YAG lasers. Ethylene glycol, diethylene glycol and 2-ethoxyethanol were used as reductants in the synthesis reactions. Spherical and faceted silver particles of high purity were formed by laser interaction between the precursor solution and a rotating substrate, while porous dual phase nickel and nickel oxide particles were produced when nickel nitrate was used as a precursor. The composition and morphology of the alloy particles was dependent on laser parameters and chemical composition of the precursor solution. The product composition was dependent only upon the chemistry of the precursors used. The mean particle size was dependent upon the temperature generated by irradition and the duration of exposure to the laser beam. The synthesis of nano-particles and metastable alloys is proposed to occur primarily at the laser-liquid-solid interface by a nucleation and growth mechanism.