Titanium Dioxide (TiO2) has been extensively studied as it can be applied to many different applications. TiO2 nanomaterials have several unique properties that makes it desirable for many applications as such producing TiO2 nanomaterials is very important. Multitude of methods and processes are available to synthesize nanomaterials. The ability to manipulate and control the method is the key in producing nanomaterials with specific properties for the desired applications. Hydrothermal method is very flexible and cost-effective method that has been employed to produce TiO2 nanomaterials. This study presents the experimental study on method to produce Titanium Dioxide (TiO2) aggregates composed of nanocrystallites. This type of surface morphology is known to introduce the light scattering effect which can enhance the performance of dye sensitized solar cells (DSSC). Various synthesis parameters were investigated focusing on the autoclaving temperature to obtain desired surface morphology. Titanium alkoxides was used with ethanol and 2-propanol as solvents using hydrothermal method. Characterization and analysis were conducted using Scanning electron microscope (SEM) and X-ray Diffraction (XRD). SEM analysis indicates the formation of TiO2 aggregates estimated to be 2-6 microns composed of 1 -2 nm crystallites. XRD analysis confirms that anatase TiO2 is produced as expected. Furthermore, autoclaving at higher temperature (220°C) produces larger TiO2 particles compared to lower autoclaving temperature (150°C). Subsequently, autoclave treatment at high temperature causes the deformation of large aggregates. As such the autoclaving temperature is a predominant factor in controlling the growth of TiO2 aggregates. © 2011 Asian Network for Scientific Information.