A combination of ion beam sputtering and in situ x-ray diffraction as a method for depth-resolved phase analysis using nitrogen-implanted austenitic stainless steel as an example

Abstract

In situ x-ray diffraction (XRD) during ion implantation or thin film deposition is a powerful method to follow the time evolution of diffusion and phase transition processes in thin films, even as the depth resolution is still dominated by the information depth of the x rays. However, in the case of sputter etching with energetic ions at moderate temperatures, where no diffusion or phase transformation processes are active, this limitation is no longer of concern. Here, thin surface layers which are removed by sputtering can be identified with a depth resolution of 25 nm or better—while information from the substrate—despite overlayers of several micrometers—is accessible. However, considerable mathematical operations are necessary to convert the time series of diffractograms measured by XRD into a depth series. In this paper, a method is highlighted describing which depth-resolved properties of thin films can be accessed using such in situ measurements during ion beam sputtering in the model system austenitic stainless steel + nitrogen: (i) the influence of concentration gradients on the peak shape and peak width for conventional XRD scans in Bragg–Brentano geometry is determined; (ii) correlations between the local nitrogen concentration and the local lattice expansion can be established; and (iii) the evolution of the scattering intensity with depth becomes accessible, thus depth-resolved information on defect densities or grain size (normal to the surface) can be extracted without resorting to transmission or scanning electron microscopy.