Ammonium perchlorate is one of the most important oxidants being used in the production of composite solid propellant whose shape and particle size have a great impact on its characteristics. In this research, in order to produce the nano-particles, the micro-emulsion of ammonium perchlorate salt in the presence of active surfactant materials has been produced and frozen in the liquid nitrogen before finally turned in the nano-particles using the freeze drying technique. The experiment results show that the parameters such as the emulsion stability, the type of active surfactant material, co-activator, type of oil, the mass ratio of the components in the emulsion, mixing rate, freezing method, and the temperature have a great influence on the particles’ shape and size. Having considered and examined all the above mentioned parameters, the nano-particles with the average diameter of 40-150 nm with spherical shape have been finally produced.