The polymeric alumina sol was prepared by partial hydrolysis of aluminum sec-butoxide reacted with acetylacetone and its characteristics was investigated. The effects of alcohol solvent, acetylacetone, and acid concentration to the sol were investigated. FT-IR and Al27-MASNMR were used to study hydrolysis and polymerization reaction of aluminum complex. Synthesized sol showed the characteristics of polymeric alumina sol. To make a clear polymeric alumina sol, the optimum contents of acetylacetone, H2O and alcohol solvent were 0.4-0.6 mole, 0.25-1.25 mole, 3-5 mole per one mole alkoxide respectively. As a result of the Al27-MASNMR analysis, it was noted that hexa-penta-coordinated Al were main structure.