Fluidized-bed atomic layer deposition reactor for the synthesis of core-shell nanoparticles

Arjen P Didden; Joost Middelkoop; Wim F A Besling; Diana E Nanu; Roel van de Krol

doi:10.1063/1.4863099

Fluidized-bed atomic layer deposition reactor for the synthesis of core-shell nanoparticles

Rev Sci Instrum. 2014 Jan;85(1):013905. doi: 10.1063/1.4863099.

Authors

Arjen P Didden¹, Joost Middelkoop¹, Wim F A Besling², Diana E Nanu³, Roel van de Krol¹

Affiliations

¹ Delft University of Technology, Faculty of Applied Sciences, Department of Chemical Engineering, P.O. Box 5045, 2600 GA Delft, The Netherlands.
² NXP Semiconductors, High Tech Campus 32, 5656 AE Eindhoven, The Netherlands.
³ Thin Film Factory B.V., Hemma Oddastrjitte 5, 8927 AA Leeuwarden, The Netherlands.

PMID: 24517780
DOI: 10.1063/1.4863099

Abstract

The design of a fluidized bed atomic layer deposition (ALD) reactor is described in detail. The reactor consists of three parts that have all been placed in one protective cabinet: precursor dosing, reactor, and residual gas treatment section. In the precursor dosing section, the chemicals needed for the ALD reaction are injected into the carrier gas using different methods for different precursors. The reactor section is designed in such a way that a homogeneous fluidized bed can be obtained with a constant, actively controlled, reactor pressure. Furthermore, no filters are required inside the reactor chamber, minimizing the risk of pressure increase due to fouling. The residual gas treatment section consists of a decomposition furnace to remove residual precursor and a particle filter and is installed to protect the pump. In order to demonstrate the performance of the reactor, SiO2 particles have been coated with TiO2 using tetrakis-dimethylamino titanium (TDMAT) and H2O as precursors. Experiments with varying pulse times show that saturated growth can be obtained with TDMAT pulse times larger than 600 s. Analysis of the powder with High-Angle Annular Dark-Field Scanning Transmission Electron Microscopy (HAADF-STEM) and energy dispersive X-ray spectroscopy confirmed that after 50 cycles, all SiO2 particles were coated with a 1.6 nm homogenous shell of TiO2.