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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:
tompsett@ecs.umass.edu, University of Massachusetts, Chemical Engineering, 159 Goessmann Lab, Amherst, MA, 01003, United States, 413-577-0139
Bernard Panzarella
Affiliation:
bpanzare@ecs.umass.edu, University of Massachusetts, Chemical Engineering, United States
W. Curt Conner
Affiliation:
wconner@ecs.umass.edu, University of Massachusetts, Chemical Engineering, United States
Keith W Jones
Affiliation:
jones@bnl.gov, Brookhaven National Lab, Environmental Science, United States
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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

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