In this work, the precursors zinc nitrate hexahydrate and zinc chloride were used to synthesize zinc oxide (ZnO) nanocrystals, applying a simple solochemical technique. ZnO rod-like nanostructures were successfully obtained by chemical reaction between NaOH and zinc nitrate hexahydrate at 90 °C. The sample formed by chemical reaction between NaOH and zinc chloride at 90 °C showed the ZnO phase mixed with the Zn5(OH)8Cl2•H2O phase. Only after thermal treatment at 500 °C for 3 hours, the conversion of Zn5(OH)8Cl2•H2O in ZnO was achieved. The samples prepared with different precursors were characterized by X-ray diffraction, Raman spectroscopy and transmission electron microscopy. Rietveld analysis to the X-ray diffraction data indicated that ZnO nanocrystals obtained have hexagonal wurtzite structure and nanometric-sized crystallites.