Investigation of Oxide Thickness on Technical Aluminium Alloys—A Comparison of Characterization Methods

In this study the oxide layer of technical 6xxx aluminium surfaces, pickled as well as passivated, were comparatively investigated by means of transmission electron microscopy (TEM), Auger electron and X-ray photoelectron spectroscopy (AES, XPS), the latter in two different operating modes, standard and angle resolved mode. In addition, confocal microscopy and focused ion beam cutting were used for structural studies of the surfaces and for specimen preparation. The results illustrate in detail the strengths and weaknesses of each measurement technique. TEM offers a direct way to reliably quantify the thickness of the oxide layer, which is in the range of 5 nm, however, on a laterally restricted area of the surface. In comparison, for AES, the destructiveness of the electron beam did not allow to achieve comparable results for the thickness determination. XPS was proven to be the most reliable method to reproducibly quantify the average oxide thickness. By evaluating the angle resolved XPS data, additional information on the average depth distribution of the individual elements on the surface could be obtained. The findings obtained in this study were then successfully used for the investigation of the increase in the aluminium oxide thickness on technical samples during an aging test of 12 months under standard storage conditions.