doi:10.1016/j.cplett.2003.10.088
Copyright © 2003 Elsevier B.V. All rights reserved.
Ultra-thin zeolite films prepared by spin-coating Silicalite-1 precursor solutions
A. M. Doyle
,
, a, G. Rupprechtera, N. Pfändera, R. Schlögla, C. E. A. Kirschhockb, J. A. Martensb and H. -J. Freunda
a Fritz-Haber-Institut der Max-Planck-Gesellschaft, Faradayweg 4-6, Berlin 14195, Germany
b Centrum voor Oppervlaktechemie en Katalyse, K.U. Leuven, Kasteelpark Arenberg 23, B-3001, Heverlee, Belgium
Received 9 July 2003;
revised 15 September 2003.
Available online 14 November 2003.
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Abstract
A procedure has been developed to prepare ultra-thin zeolite films supported on Si(1 0 0). Films were prepared by spin-coating a solution of Silicalite-1 zeolite precursors diluted in ethanol, followed by hydration in water vapour and heating to 60 °C. High resolution transmission electron microscopy analysis of sample cross-sections shows that the surfaces are both smooth and continuous, and films of approximately 2 and 15 nm thickness were prepared by varying the precursor dilution factor. Electron diffraction analysis shows that the 15 nm film is an amorphous arrangement of Silicalite-1 precursors. Atomic force microscopy measurements confirm that the surface is smooth over a range of several microns.
Fig. 1. TEM images of MFI zeolite nanoslabs spread on a grid [10].
Fig. 2. AFM images of zeolite films, analysis area 70 × 70 μm: (a)–(c) film A, (d)–(f) film B, (a) and (d) are topography images. Scratched films (c) and (f) are presented in CDM and include film thickness measurements.
Fig. 3. TEM cross-section images (a) 2 nm film A and (b) 15 nm film B. The interface area of film A and the atomically resolved substrate of B are shown as insets.
Fig. 4. TEM plan view images and electron diffraction patterns of 15 nm film B. (a) and (b) correspond to the zeolite film only, (c) and (d) correspond to the zeolite film and silicon wafer.
Table 1. AFM topographical data for films A and B
