Single-pass flow-through reaction cell for high-temperature and high-pressurein situneutron diffraction studies of hydrothermal crystallization processes

F. Xia; J. Brugger; G. Qian; Y. Ngothai; B. O'Neill; J. Zhao; S. Pullen; S. Olsen; A. Pring

doi:10.1107/S0021889812002300

$Single-pass flow-through reaction cell for high-temperature and high-pressurein situneutron diffraction studies of hydrothermal crystallization processes$

Journal article

Open access

Peer reviewed

Single-pass flow-through reaction cell for high-temperature and high-pressurein situneutron diffraction studies of hydrothermal crystallization processes

F. Xia, J. Brugger, G. Qian, Y. Ngothai, B. O'Neill, J. Zhao, S. Pullen, S. Olsen and A. Pring

Journal of Applied Crystallography, Vol.45(2), pp.166-173

2012

DOI: https://doi.org/10.1107/S0021889812002300

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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 ([greater-than or equal to]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 SrSO4 (celestine) to SrCO3 (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.

Details

Title: Single-pass flow-through reaction cell for high-temperature and high-pressurein situneutron diffraction studies of hydrothermal crystallization processes
Authors/Creators: F. Xia (Author/Creator)
J. Brugger (Author/Creator)
G. Qian (Author/Creator)
Y. Ngothai (Author/Creator)
B. O'Neill (Author/Creator)
J. Zhao (Author/Creator)
S. Pullen (Author/Creator)
S. Olsen (Author/Creator)
A. Pring (Author/Creator)
Publication Details: Journal of Applied Crystallography, Vol.45(2), pp.166-173
Publisher: International Union of Crystallography
Identifiers: 991005545356607891
Copyright: © 2012 International Union of Crystallography
Murdoch Affiliation: Murdoch University
Language: English
Resource Type: Journal article

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Collaboration types: Domestic collaboration
Citation topics: 2 Chemistry; 2.165 Nanofibers, Scaffolds & Fabrication; 2.165.1082 Calcium Carbonate Crystallization
Web Of Science research areas: Chemistry, Multidisciplinary; Crystallography
ESI research areas: Chemistry