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Materials (Basel). 2015 Mar 19;8(3):1249-1263. doi: 10.3390/ma8031249.

Gas-Phase Deposition of Ultrathin Aluminium Oxide Films on Nanoparticles at Ambient Conditions.

Author information

1
Department of Chemical Engineering, Delft University of Technology, 2628 BL Delft, The Netherlands. d.valdesueiro@tudelft.nl.
2
Department of Chemical Engineering, Delft University of Technology, 2628 BL Delft, The Netherlands. G.M.H.Meesters@tudelft.nl.
3
Department of Chemical Engineering, Delft University of Technology, 2628 BL Delft, The Netherlands. M.T.Kreutzer@tudelft.nl.
4
Department of Chemical Engineering, Delft University of Technology, 2628 BL Delft, The Netherlands. j.r.vanommen@tudelft.nl.

Abstract

We have deposited aluminium oxide films by atomic layer deposition on titanium oxide nanoparticles in a fluidized bed reactor at 27 ± 3 °C and atmospheric pressure. Working at room temperature allows coating heat-sensitive materials, while working at atmospheric pressure would simplify the scale-up of this process. We performed 4, 7 and 15 cycles by dosing a predefined amount of precursors, i.e., trimethyl aluminium and water. We obtained a growth per cycle of 0.14-0.15 nm determined by transmission electron microscopy (TEM), similar to atomic layer deposition (ALD) experiments at a few millibars and ~180 °C. We also increased the amount of precursors dosed by a factor of 2, 4 and 6 compared to the base case, maintaining the same purging time. The growth per cycle (GPC) increased, although not linearly, with the dosing time. In addition, we performed an experiment at 170 °C and 1 bar using the dosing times increased by factor 6, and obtained a growth per cycle of 0.16 nm. These results were verified with elemental analysis, which showed a good agreement with the results from TEM pictures. Thermal gravimetric analysis (TGA) showed a negligible amount of unreacted molecules inside the alumina films. Overall, the dosage of the precursors is crucial to control precisely the growth of the alumina films at atmospheric pressure and room temperature. Dosing excess of precursor provokes a chemical vapour deposition type of growth due to the physisorption of molecules on the particles, but this can be avoided by working at high temperatures.

KEYWORDS:

aluminium oxide; ambient conditions; atmospheric pressure; atomic layer deposition (ALD); coating; fluidized bed reactor; nanoparticles; room temperature; thin films

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