The evolution of desirable physico-chemical properties in high performance photocatalyst materials involves steps that must be carefully designed, controlled, and optimized. This study investigated the role of key parameter in the preparation and photocatalytic activity analysis of the mixed phase of anatase/rutile TiO2 nanoparticles, prepared via sol-gel method containing titanium-n-butoxide Ti(OBu)4 as a precursor material, nitric acid as catalyst, and isopropanol as solvent. The prepared TiO2 nanoparticles were characterized by means of XRD, SEM, and BET analyses, and UV-Vis-NIR spectroscopy. The results indicated that the calcination temperature play an important role in the physico-chemical properties and photocatalytic activity of the resulting TiO2 nanoparticles. Different calcination temperatures would result in different composition of anatase and rutile. The photocatalytic activity of the prepared mixed phase of anatase/rutile TiO2 nanoparticles was measured by photodegradation of 50 ppm phenol in an aqueous solution. The commercial anatase from Sigma-Aldrich and Degussa P25 were used for comparison purpose. The mixed phase of anatase/rutile TiO2 nanoparticles (consists of 38.3% anatase and 61.7% rutile) that was prepared at 400°C exhibited the highest photocatalytic activity of 84.88% degradation of phenol. The result was comparable with photocatalytic activity demonstrated by Degussa P25 by 1.54% difference in phenol degradation. The results also suggested that the mixed phase of anatase/rutile TiO2 nanoparticles is a promising candidate for the phenol degradation process. The high performance of photocatalyst materials may be obtained by adopting a judicious combination of anatase/rutile and optimized calcination conditions.