A large volume cell for in situ neutron diffraction studies of hydrothermal crystallizations

Fang Xia, Gujie Qian, Joel Brugger, A Studer, Scott Olsen, Allan Pring

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    5 Citations (Scopus)

    Abstract

    A hydrothermal cell with 320 ml internal volume has been designed and constructed for in situ neutron diffraction studies of hydrothermal crystallizations. The cell design adopts a dumbbell configuration assembled with standard commercial stainless steel components and a zero-scattering Ti-Zr alloy sample compartment. The fluid movement and heat transfer are simply driven by natural convection due to the natural temperature gradient along the fluid path, so that the temperature at the sample compartment can be stably sustained by heating the fluid in the bottom fluid reservoir. The cell can operate at temperatures up to 300 °C and pressures up to 90 bars and is suitable for studying reactions requiring a large volume of hydrothermal fluid to damp out the negative effect from the change of fluid composition during the course of the reactions. The capability of the cell was demonstrated by a hydrothermal phase transformation investigation from leucite (KAlSi2 O 6) to analcime (NaAlSi2O6 H2O) at 210 °C on the high intensity powder diffractometer Wombat in ANSTO. The kinetics of the transformation has been resolved by collecting diffraction patterns every 10 min followed by Rietveld quantitative phase analysis. The classical Avrami/Arrhenius analysis gives an activation energy of 82.3±1.1 kJ mol-1. Estimations of the reaction rate under natural environments by extrapolations agree well with petrological observations.

    Original languageEnglish
    Article number105107
    Pages (from-to)105107
    Number of pages6
    JournalReview of Scientific Instruments
    Volume81
    Issue number10
    DOIs
    Publication statusPublished - Oct 2010

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