Nickel oxide nanoparticles have been successfully synthesized by using low combustion synthesis method followed by calcination at 500 oC for 30 minutes. The calcined Nickel oxide nanoparticles were investigated by various tools such as XRD, FT-IR and FE-SEM. The average crystallite size of the calcined Nickel oxide was determined to be 6.5, 8.2 and 16.7 nm according to various fuels. The characteristic absorption peak at 429 corresponds to Ni-O stretching vibration mode of Nickel oxide. The FE-SEM photograph displayed that the calcined Nickel oxide nanoparticles are agglomerated in network shapes and the average agglomerated particle Nickel in the range 1 μm.