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    Wang, Xiqu Liu, Lumei and Jacobson, Allan J. 2000. Hydrothermal Synthesis and Crystal Structures of [(CH3NH3)0.5(NH4)1.5]Sb8S13·2.8H2O and Rb2Sb8S13 ·3.3H2O. Journal of Solid State Chemistry, Vol. 155, Issue. 2, p. 409.


    Wang, Xiqu Jacobson, Allan J and Liebau, Friedrich 1998. Hydrothermal Synthesis and Crystal Structure of [(CH3NH3)1.03K2.97]Sb12S20·1.34H2O. Journal of Solid State Chemistry, Vol. 140, Issue. 2, p. 387.


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

  • J. B. Parise (a1) (a2), K. Tan (a1), P. Norby (a3), Y. Ko (a1) and C. Cahill (a2)
  • DOI: http://dx.doi.org/10.1557/PROC-453-103
  • Published online: 01 February 2011
Abstract
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.

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