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In Situ Studies of Solvothermal Synthesis of Energy Materials

DOI: 10.1002/cssc.201301042 DOI Help

Authors: Kirsten M. Ø. Jensen (Aarhus University) , Christoffer Tyrsted (Aarhus University) , Martin Bremholm (Aarhus University) , Bo B. Iversen (Aarhus University)
Co-authored by industrial partner: No

Type: Journal Paper
Journal: Chemsuschem , VOL 7 (6) , PAGES 1594 - 1611

State: Published (Approved)
Published: June 2014

Open Access Open Access

Abstract: Solvothermal and hydrothermal synthesis, that is, synthesis taking place in a solvent at elevated temperature and pressure, is a powerful technique for the production of advanced energy materials as it is versatile, cheap, and environmentally friendly. However, the fundamental reaction mechanisms dictating particle formation and growth under solvothermal conditions are not well understood. In order to produce tailor-made materials with specific properties for advanced energy technologies, it is essential to obtain an improved understanding of these processes and, in this context, in?situ studies are an important tool as they provide real time information on the reactions taking place. Here, we present a review of the use of powder diffraction and total scattering methods for in?situ studies of synthesis taking place under solvothermal and hydrothermal conditions. The experimental setups used for in?situ X-ray and neutron studies are presented, and methods of data analysis are described. Special attention is given to the methods used to extract structural information from the data, for example, Rietveld refinement, whole powder pattern modelling and pair distribution function analysis. Examples of in?situ studies are presented to illustrate the types of chemical insight that can be obtained.

Journal Keywords: Energy Materials;Hydrothermal;In Situ;Powder Diffraction;Solvothermal

Subject Areas: Materials

Instruments: I12-JEEP: Joint Engineering, Environmental and Processing

Other Facilities: ESRF; Soleil; Desy