Structure and Bonding Volume 119, 2006, pp 161-192

Mechanistic and Kinetic Studies of Guest Ion Intercalation into Layered Double Hydroxides Using Time-resolved, In-situ X-ray Powder Diffraction

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Abstract

In recent years, a tremendous increase in our understanding of intercalation reactions has been attained through the use of in-situ techniques. In such studies, a non-invasive probe is employed, allowing the collection of large amounts of data on a reaction process. A non-invasive probe is preferred, rather than arresting the reaction and analysing the product thereby obtained (quenching). This is because the quenching process often affects the reaction product, and hence what is isolated can never be guaranteed to be typical of the reaction matrix. In the study of crystalline solids, one of the most useful non-invasive probes is X-ray diffraction, since this technique can provide evidence on the nature of the species present in the reaction and their concentrations. Through the use of synchrotron radiation, X-ray diffraction patterns may be collected on timescales as short as seconds, allowing accurate quantitative information about an intercalation process to be acquired. In this review, the application of this technique to a variety of intercalation processes relating to layered double hydroxides is surveyed.