Al2O3 and NiO-doped Al2O3 powders were prepared from the ethanol solution of Al (NO3)3$.$9H2O and Ni(NO3)2$.$6H2O by spray pylolysis method using two-fluid nozzle. As a result of spraying test with 0.3 mol/{{{{ iota }} concentration starting solution, mean droplet sizes varied with 8.99∼9.69$mu extrm{m}$ and those standard deviation were 4.57∼5.12. As-prepared powders which were synthesized at 1000$^{circ}C$ have spherical shape, sizes of 0.1∼3.0$mu extrm{m}$ and specific surface area of 22.34∼24.20㎡/g. Most powders consisted of {{{{ gamma }}-Al2O3 phase and transforned into ${alpha}$-A;2O3 phase by calcination at 1100$^{circ}C$ for 1 hr. NiO-doped Al2O3 sintered bodies had better sinterability than those of pure Al2O3 and 0.3 wt% NiO-doped Al2O3 had near theoretical density and dense microstructure.