Hostname: page-component-586b7cd67f-t7czq Total loading time: 0 Render date: 2024-11-29T09:51:40.076Z Has data issue: false hasContentIssue false
  • English
  • Français

In situ SAXS/WAXS of Zeolite Microwave Hydrothermal Synthesis

Published online by Cambridge University Press:  01 February 2011

Geoff A. Tompsett ,
Bernard Panzarella ,
W. Curt Conner  and
Keith W Jones
Geoff A. Tompsett
Affiliation:
[email protected], University of Massachusetts, Chemical Engineering, 159 Goessmann Lab, Amherst, MA, 01003, United States, 413-577-0139
Bernard Panzarella
Affiliation:
[email protected], University of Massachusetts, Chemical Engineering, United States
W. Curt Conner
Affiliation:
[email protected], University of Massachusetts, Chemical Engineering, United States
Keith W Jones
Affiliation:
[email protected], Brookhaven National Lab, Environmental Science, United States
Get access

Abstract

The microwave hydrothermal synthesis of silicalite zeolite was monitored in situ using small and wide angle X-ray scattering (SAXS and WAXS). A custom-built waveguide reactor provided the microwave heating at 2.45 GHz frequency. Microwave power up to 300 W was supplied by a SAIREM generator via a coax connection. A sample port in the waveguide section allowed a thin-walled glass sample vessel to be held in the microwave field. The sample vial was sealed with a fiber optic temperature probe used for monitoring the temperature. Silicalite zeolite precursor solutions were heated temperatures between 100 and 130°C for up to 120 minutes. The SAXS or WAXS patterns were simultaneously scanned during the reaction under microwaves via X-ray beam through slots in the side of the waveguide. The progress of silicalite zeolite formation was followed and the analysis of SAXS patterns showed the primary particles of 2 nm shifted to aggregates of 5.8 nm in diameter, in 120 minutes at 130°C.

Keywords

microwave heatingzeolitex-ray diffraction (XRD)
Type
Research Article
Information
MRS Online Proceedings Library (OPL) , Volume 900: Symposium O – Nanoparticles and Nanostructures in Sensors and Catalysis , 2005 , 0900-O12-06
Copyright
Copyright © Materials Research Society 2006

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

1 Whittaker, A. G.et al., Review of Scientific Instruments 72, 173–176. (2001).Google Scholar
2 Harrison, A.et al., Faraday Discussions 122, 363–379 (2002).Google Scholar
3 Robb, G. R., Harrison, A., Whittaker, A. G., PhysChemComm, 135–137 (2002).Google Scholar
4 Dokter, W. H. et al., Journal of Applied Crystallography 27, 901–906 (Dec 1, 1994).Google Scholar
5 Moor, P. P. E. A. de, Beelen, T. P. M., Santen, R. A. van, Beck, L. W., Davis, M. E., Journal of Physical Chemistry B 104, 7600–7611 (Aug 17, 2000).Google Scholar
6 Houssin, C. J. Y.et al., Physical Chemistry Chemical Physics 5, 3518–3524 (2003).Google Scholar
7 Watson, J. N., Brown, A. S., Iton, L. E., White, J. W., Journal of the Chemical Society-Faraday Transactions 94, 2181–2186 (Aug 7, 1998).Google Scholar
8 Yang, S. Y., Navrotsky, A., Chemistry of Materials 16, 3682–3687 (Sep 21, 2004).Google Scholar
9 Dokter, W. H., Beelen, T. P. M., Garderen, H. F. v., Santen, R. A. v., Studies in Surface Science and Catalysis 87 (Characterization of Porous Solids III), 725–34 (1994).Google Scholar
10 Moor, P.-P. E. A. De, Beelen, T. P. M., Komanschek, B. U., Santen, R. A. Van, Microporous and Mesoporous Materials 21, 263–269 (1998).Google Scholar
11 Xomeritakis, G., Nair, S., Tsapatsis, M., Microporous and Mesoporous Materials 38, 61–73 (2000).Google Scholar
12 Tompsett, G.et al., Review of Scientific Instruments In preparation (2005).Google Scholar
13 Dokter, W. H., Garderen, H. F. van, Beelen, T. P. M., Santen, R. A. van, Bras, W., Angewandte Chemie, International Edition in English 34, 73–5 (1995).Google Scholar
14 Moor, P.-P. E. A. De, Beelen, T. P. M., Santen, R. A. Van, Journal of Physical Chemistry B 103, 1639–1650 (1999).Google Scholar