Single-pass flow-through reaction cell for high-temperature and high-pressure in situ neutron diffraction studies of hydrothermal crystallization processes

Fang Xia, Joel Brugger, Gujie Qian, Yung Ngothai, Brian O'Neill, Jing Zhao, S. Pullen, Scott Olsen, Allan Pring

Research output: Contribution to journalArticlepeer-review

4 Citations (Scopus)

Abstract

A large-volume single-pass flow-through cell for in situ neutron diffraction investigation of hydrothermal crystallization processes is reported. The cell is much more versatile than previous designs owing to the ability to control independently and precisely temperature (up to 673 K), pressure (up to 46 MPa), flow rate (0.01-10 ml min -1) and reaction-fluid volume (65 ml). Such versatility is realized by an innovative design consisting of a room-temperature and ambient-pressure external fluid supply module, a high-pressure reaction module which includes a high-temperature sample compartment enclosed in a vacuum furnace, and a room-temperature and high-pressure backpressure regulation module for pressure control. The cell provides a new avenue for studying various parameters of hydrothermal crystallizations independently, in situ and in real time at extreme hydrothermal conditions (e.g. supercritical). The cell was successfully commissioned on the high-intensity powder diffractometer beamline, Wombat, at the Australian Nuclear Science and Technology Organisation by investigating the effect of pressure on the hydrothermal pseudomorphic conversion from SrSO 4 (celestine) to SrCO 3 (strontianite) at a constant temperature of 473 K and flow rate of 5 ml min -1. The results show that the increase of pressure exerts a nonlinear effect on the conversion rate, which first increases with increasing pressure from 14 to 20 MPa, and then decreases when pressure further increases to 24 MPa.

Original languageEnglish
Pages (from-to)166-173
Number of pages8
JournalJOURNAL OF APPLIED CRYSTALLOGRAPHY
Volume45
Issue number2
DOIs
Publication statusPublished - 9 Feb 2012

Keywords

  • hydrothermal cells
  • Neutron diffraction
  • vacuum furnaces
  • strontianite (SrCO )
  • celestine (SrS )
  • in situ neutron diffraction
  • mineral replacement reactions

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