Materials Chemistry and Physics, Vol.90, No.1, 116-122, 2005
Template removal from polycrystalline silicalite-1 self-supporting layer
The extent of thermal template (tetra-propyl-ammonium: TPA(+)) removal from a silicalite-1 layer by heating in air was investigated. While a temperature of 330degreesC was sufficient to eliminate all N-containing template species from the surface region of the layer (i.e., within a depth of 10 nm), their complete elimination from the bulk even at 550degreesC was not achieved. This was caused by a series of reactions proceeding at high temperatures, involving the products of TPA(+) thermal degradation. A substantial amount of C-containing template species remained in the sample even after a thermal treatment at 550degreesC. A role the SiO2 phase of low organization present in the silicalite-1 layer plays in the retention of the products of thermal degradation has been proposed. Additionally, the stability of TPA(+) irradiated by microwaves was examined. Only minor morphological changes of the layer upon thermal template removal were revealed by atomic force microscopy. (C) 2004 Elsevier B.V. All rights reserved.
Keywords:microporous materials;surface properties;X-ray photoelectron spectroscopy;atomic force microscopy;silicalite-1