David M. King, Xinhua Liang, Yun Zhou, Casey S. Carney, Luis F. Hakim, Peng Li, Alan W. Weimer

Atomic layer deposition of TiO₂ films on particles in a fluidized bed reactor

Powder Technology 183 (2008) 356–363

Atomic layer deposition (ALD) of controlled-thickness TiO₂ films was carried out on particle substrates in a fluidized bed reactor for the first time. Films were deposited on 550 nm SiO₂ spheres and 65 nm ZnO nanoparticles for enhanced optical properties. Nanoparticles were fluidized with the assistance of a magnetically-coupled stirring unit. The metalorganic precursor titanium tetraisopropoxide was used here followed by either H₂O or H₂O₂ to deposit TiO₂ at various substrate temperatures. Growth rates of 0.01 nm/cycle and 0.04 nm/cycle were achieved when using H₂O and H₂O₂ as the oxidizer, respectively. These conformal TiO₂ films were verified using HRTEM, ICP-AES, XPS and UV absorbance measurements. The specific surface area changed appropriately after the particle size increased by the deposition of films with a given density, which showed that primary particles were not agglomerated together due to the coating process. In situ mass spectrometry was used to monitor reaction progress throughout each ALD reaction cycle. Bulk quantities of powder were successfully functionalized by TiO₂ nanofilms without wasting excess precursor.

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