We report the use of X-rays absorption technique, detected in total reflection mode, to obtain structural information on new materials. After a brief description of the ReflEXAFS technique, we present the results obtained in the study of two very peculiar solid-state problem: a) the effect of the Sb as surfactant in the Si/Ge multilayers and b) the understanding of the very early stage of the spinel formation. We show that the use of a Sb film is not enough to completely stop the interdiffusion process and the quality of the interface is quantify in terms of the interdiffusion of Ge in Si. The second case deals with the structural study of the very earl stage of the NiAl_2O_4 spinel formation; this solid-state reaction requires high temperature and long time of exposition in O_2 atmosphere. The progresses of the reaction have been followed by several ReflEXAFS measurement, taken after each thermal treatment.
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