Developing a solvothermal reaction cell for in situ neutron scattering of crystallisation Mark Crossman 1 , Helen Y. Playford 2 and Richard I. Walton 1 1 University of Warwick, UK, 2 ISIS Facility Rutherford Appleton Laboratory, UK Despite solvothermal synthesis being one of the most versatile methods for the synthesis of metal oxides, little is known of the chemistry that occurs during the process due to the closed nature of a solvothermal reaction. Although a range of X-ray techniques have been used to follow solvothermal crystallisations, the benefits of neutron diffraction have not been exploited in the in-situ study of the formation of materials. This includes the penetration of bulky reaction vessels, sensitivity to low atomic number elements, and, potentially, study of magnetic materials. In this contribution I will explore the potential of a new cell designnull-scattering titanium zirconium alloy (Ti 0676 Zr 0.324 ) with an aim for the cell to be easily transportable and adaptable to a variety of neutron instruments depending on suitability for the reactions being studied. The cell has been deployed in the study of the synthesis of the strontium ruthenate SrRu 2 O6 on POLARIS at ISIS for the real time monitoring of its crystallization at different temperatures. This material is of particular interest for its potential as a new semiconductor material while also possessing antiferromagnetic ordering with a Néel point above the synthesis temperature ( T N = 565 K). It has also been reported that with minor changes to the synthesis conditions of SrRu 2 O 6 , two additional strontium ruthenate phases can be produced. This makes the study of this material ideal to explore the potential of the cell in monitoring synthesis routes, magnetic structure formation in real time and reaction kinetics. The cell has also been used to study the formation of zeolite A (LTA) and its conversion under basic conditions to hydrosodalite (SOD) on NIMROD at ISIS. This allows for studying the impact of temperature on the rate of formation of the zeolite and the rate of conversion to the sodalite with an opportunity to use the cell to study disordered materials and its suitability for PDF analysis in situ.
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© The Author(s), 2023
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