Journal of Chemical Engineering of Japan, Vol.48, No.4, 292-299, 2015
Effects of Annealing on the Morphology and Porosity of Porous TiO2 Films Fabricated by Deposition of Aerosol Nanoparticles
The present study investigates the impact of post annealing of TiO2 nanoparticulate films on their crystallinity, mechanical strength, and morphology. Non-agglomerated and amorphous TiO2 nanoparticles of 46 nm diameter were synthesized in a plasma field, and were subsequently deposited on substrates to form nanoparticulate films. The films were annealed at various temperatures in the range of 100-1,200 degrees C. Phase transformations from amorphous-to-anatase and from anatase-to-rutile were observed at 400 degrees C and at 1,000 degrees C, respectively. The high rutile transformation temperature was considered to be due to a tensile field induced by shrinkage of the film. The as-deposited film and the films annealed at below 400 degrees C had poor mechanical strength. Conversely, the films annealed at over 500 degrees C were strengthened by necking of the nanoparticles. The size of nanoparticles changed with increasing temperature. Annealing at 100-300 degrees C caused the nanoparticles to shrink to approximately 30 nm. The nanoparticle diameters changed only slightly when annealed at 400-600 degrees C because the annealing time was insu efficient for changes to manifest. Annealing at 700-900 degrees C caused the nanoparticle diameter to increase to approximately 50 nm because of sintering and coalescence of the nanoparticles. The diameter of the nanoparticles annealed at over 1,000 degrees C became approximately 200 nm because of densification during the anatase-to-rutile transformation. The porosities of the films annealed at below 900 degrees C were over 80%. However, the porosities of the films annealed at over 1,000 degrees C decreased significantly due to densification.