Anatase TiO2 nanoparticles with tuning size and aspect ratio were successfully prepared by a simple solvothermal method, using ethanol as a solvent, titanium butoxide as a precursor, and oleic acid and oleylamine as anionic and cationic capping agents, respectively. The average size and aspect ratio of these nanoparticles can be greatly regulated by varying the oleic acid/oleylamine molar ratio while keeping their total molar content constant and finely adjusted by increasing the total capping agents molar concentration in solvent at constant molar ratio (oleic acid/oleylamine molar ratio = 1:1). The variation of molar ratio or molar concentration enables a manipulation of the growth rate along different facets of TiO2 nanoparticles and, consequently, a control of the aspect ratio of these nanoparticles. Moreover, the photocatalytic degradation rate of methyl blue for sample prepared with molar ratio of oleic acid to oleylamine at 6:24 is over 11% higher than that for the other samples.