Issue 40, 2017

Synchrotron XRD and NMR evidence of germanium redistribution during silylation of BEC-type germanosilicate

Abstract

The localization and distribution of germanium atoms in the framework positions of Ge-BEC zeolite upon silylation have been studied using synchrotron XRD and 19F NMR. The high thermal stability of Ge-BEC material synthesized using 1-benzyl-1,4-diazabicyclo[2.2.2]octane as the structure-directing agent (SDA) has been observed, enabling the preparation of calcined Ge-BEC. Unexpectedly, the inhomogeneous enrichment of double-four membered ring (d4r) subunits in the BEC structure with germanium has been observed. The interaction of germanosilicate with (NH4)2SiF6 led to the selective substitution of germanium atoms in T2 and T3 positions with silicon, while fluoride anions preferably occupy positions inside d4r subunits.

Graphical abstract: Synchrotron XRD and NMR evidence of germanium redistribution during silylation of BEC-type germanosilicate

Supplementary files

Article information

Article type
Paper
Submitted
29 Jun 2017
Accepted
23 Aug 2017
First published
07 Sep 2017

CrystEngComm, 2017,19, 5982-5988

Synchrotron XRD and NMR evidence of germanium redistribution during silylation of BEC-type germanosilicate

P. A. Kots, A. V. Kurkin, V. L. Sushkevich, A. N. Fitch, V. V. Chernyshev and I. I. Ivanova, CrystEngComm, 2017, 19, 5982 DOI: 10.1039/C7CE01204G

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