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Examples of Hydrothermal Titration and Real Time X-Ray Diffraction in the Synthesis of Open Frameworks

Published online by Cambridge University Press:  15 February 2011

J. B. Parise ,
K. Tan ,
P. Norby ,
Y. Ko  and
C. Cahill
J. B. Parise
Affiliation:
Earth and Space Sciences, State University of New York, StonyBrook, NY11794–2100 Department of Chemistry, State University of New York, StonyBrook, NY11794–2100
K. Tan
Affiliation:
Earth and Space Sciences, State University of New York, StonyBrook, NY11794–2100
P. Norby
Affiliation:
Department of Chemistry, Brookhaven National Laboratory, Upton, NY11973
Y. Ko
Affiliation:
Earth and Space Sciences, State University of New York, StonyBrook, NY11794–2100
C. Cahill
Affiliation:
Department of Chemistry, State University of New York, StonyBrook, NY11794–2100
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Abstract

Hydrothermal titration (HTT) techniques represent a new synthetic strategy for the production of open frameworks. As an example, initial digestion of amorphous GeS2 in the presence of tetraethyl ammonium hydroxide (TEAOH) at 100°C is followed by injection of Ag+ into this mixture to condense the [Ge4S10]4− clusters and form a framework consisting of 8-ring channels bounded by alternating GeS-clusters and Ag+. The rational use of this apparatus depends upon determining the timing of injection. Insight into the changes occurring during reactant digestion is provided by real time synchrotron X-ray powder diffraction. Changes in the the system dimethylamine-Sb-S have been followed in real time at different temperatures. The transformation from mixtures of DMA, Sb and S to the known open phase DMA-SbS-SB8 was followed by observing monochromatic X-ray scattering detected on an imaging plates over a 8 hr period with one continuous exposure.

Type
Research Article
Information
MRS Online Proceedings Library (OPL) , Volume 453: Symposium R – Solid State Chemistry of Inorganic Materials , 1996 , 103
Copyright
Copyright © Materials Research Society 1997

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