Spherical alumina powders were prepared by the controlled hydrolysis of aluminum iso-propoxide, aluminum sec-butoxide and aluminum tri-ethoxide in a solution consisting of various alcohol and acetonitrile. The reagent concentration influenced on the particle size, size distribution, and morphology. Sub-micro-sized alumina particles grew with increasing the concentration of hydroxypropylcellulose. Particle size increased when alkoxide concentration was increased and decreased when amount of H₂O was increased. The prepared particle morphology was not spherical when alcohol/acetonitrile volume fraction was decreased over than 1 and when ethanol was used as a solvent. When aluminum tri-ethoxide was used as aluminum source, size and distribution of spherical alumina powders were decreased and sharped more than aluminum iso-prpoxide, and aluminum sec-butoxide used as an aluminum source. As amorphous powders were crystallized into γ-alumina at 1000℃ and converted into α-alumina at 1150℃. The particle morphology was retained after crystallization α-alumina.