This Book provides in depth details of synthesis Nano Crystalline Zinc Oxide (ZnO) by Solution Combustion Process. Starting from the chemicals required, chemical solution balancing, how to take particular amount of compound in grams, how to change oxidizer to fuel ratio, how it effects the result by changing oxidizer to fuel ratio. Characterization of different products through X-Ray Diffractometer (XRD), Raman Spectroscopy, FTIR Spectroscopy, TG/DT Analysis and Scanning Electron Microscopy. Through XRD we find crystal structure, crystallite size. FTIR provides characteristic frequency of Zn-O bond. TG/DT Analysis gives information about stability of ZnO up to a temperature of 1000 degree Celsius. Scanning Electron Microscopy reveals the presence of ZnO nanoparticles and also it indicate the spherical morphology of the particles.