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Synthesis of Porous Transition Metal Oxides by the Salt-Gel Method

Published online by Cambridge University Press:  28 February 2011

Andreas Stein ,
Mark Fendorf ,
Thomas P. Jarvie ,
Karl T. Mueller ,
Maurie E. Garcia  and
Thomas E. Mallouk
Andreas Stein
Affiliation:
Department of Chemistry, University of Minnesota, Minneapolis, MN 55455
Mark Fendorf
Affiliation:
Department of Chemistry, University of California, Berkeley, CA 94720
Thomas P. Jarvie
Affiliation:
Department of Chemistry, Pennsylvania State University, University Park, PA 16802
Karl T. Mueller
Affiliation:
Department of Chemistry, Pennsylvania State University, University Park, PA 16802
Maurie E. Garcia
Affiliation:
Department of Chemistry, Pennsylvania State University, University Park, PA 16802
Thomas E. Mallouk
Affiliation:
Department of Chemistry, Pennsylvania State University, University Park, PA 16802
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Abstract

Composites of surfactants with certain transition metal oxides can be arranged into periodic arrays with giant tunnel structures. Transmission electron micrographs of these structures resemble images of mesoporous silicate molecular sieves synthesized in the presence of surfactants. However, data in this study lead to the conclusion that Keggin-ions of the type (H2W12O40)6- are formed during the hydrothermal synthesis of a cetyltrimethylammonium/tungstate composite. These cluster anions are not connected to each other. Removal of the organic template therefore results in the collapse of the tunnel structures.

A strategy has been developed which uses pre-arranged surfactant-salt structures as precursors for microporous and mesoporous framework materials. Transition metal silicates with long-range structural order have been synthesized by reacting surfactant salts of niobotungstate clusters with tetraethylorthosilicate to form a salt-gel. Infrared and solid-state NMR double resonance spectra indicate that, in addition to linkages between silicate tetrahedra, niobium-oxygen-silicon linkages have been formed in this reaction. Removal of the cationic surfactants by acid-extraction has resulted in porous structures with surface areas up to 265 m2/g.

Type
Research Article
Information
MRS Online Proceedings Library (OPL) , Volume 371: Symposium W1 – Advances in Porous Materials , 1994 , 69
Copyright
Copyright © Materials Research Society 1995

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