Nano-crystalline ZnM2O4, M= (Al, Fe, Cr, Mn) particles have been prepared by different methods such as combustion, hydrothermal and sol-gel methods. The samples were characterized by X-ray diffraction (XRD) analysis, Fourier transform infrared spectroscopy (FTIR) and Transmission Electron Microscope (TEM). The XRD analysis showed that the samples exhibit different crystal phases depending on the preparation route. It showed that pure spinel phases formed only by combustion method with crystallite sizes lie in the range of 6 – 37 nm. The particulate and morphological properties have been investigated using TEM techniques.