Combined XRD and XPS analysis of ex-situ and in-situ plasma hydrogenated magnetron sputtered Mg films

Abstract

Contrary to traditional methods including top layer catalyst deposition and ex-situ hydrogenation in current study Mg–H films were synthesized using magnetron sputtering in Ar+ atmosphere and their in-situ hydrogenation in magnetron induced hydrogen plasma. XRD analysis of hydrogenated Mg–H films revealed changes of preferred crystallographic orientation. After 1–3 h of in-situ plasma hydrogenation XRD does not indicate presence of any crystalline MgH2 phase but it is observed after 5 h. The appearance of significant amount of crystalline MgH2 phase after prolonged time of in-situ hydrogenation presupposed that samples without clear expression of MgH2 crystal phase might still have hydrogen rich amorphous Mg phase which is not observable by XRD. The analysis of predicted hydrogen containing phase was performed using combination of conventional SEM; AFM, Θ-Θ XRD, GI-XRD and XPS analysis techniques. The obtained data of hydrogen containing phase distribution at the surface of the samples and its distribution depth profiles are presented together with considerations related to the efficiency of the proposed in-situ hydrogenation approach and combined analysis methods.