A method for accurate texture determination of thin oxide films by glancing-angle laboratory X-ray diffraction

Abstract

Synopsis A method for accurate measurement of the texture of thin oxide films has been proposed.The method involves the separation of integrated intensities from complex glancing angle diffraction spectra and leads to an improved representation of the preferred orientation present in oxide films. AbstractThe present paper describes a modification to the standard method of glancing angle Xray diffraction for accurate measurement of the texture of thin oxide films. The technique resolves the problems caused by overlapping diffraction peaks originating from multiphase materials with asymmetric unit cells, and the peak broadening associated with sample tilt during glancing angle texture measurement. The entire two-theta range of interest is recorded as a function of sample orientation and the integrated intensities from different crystallographic planes are extracted from fitted diffraction profiles. The technique allows for pole figures to be plotted from diffraction peaks that could otherwise not be resolved and separates contributions from neighbouring peaks, leading to a more accurate representation of the existing oxide texture. The proposed method has been used for determining texture in a 3 µm layer of monoclinic/tetragonal zirconium oxide grown during aqueous corrosion testing and has been verified by additional synchrotron XRD measurements.

Calculation of Oxygen Diffusion Coefficients in Oxide Films Formed on Low-Temperature Annealed Zr Alloys and Their Related Corrosion Behavior

“…Such phenomena indicate an increase in the thickness of Figure 6 shows the GIXRD results of the corroded samples after 3-day and 42-day exposures. It can be seen that the oxide film mainly consists of monoclinic zirconia (m-ZrO 2 ), which is consistent with the results in [5,52,53]. Due to the contribution of the substrate, the diffraction peaks of α-Zr can still be observed on the GIXRD patterns for all samples corroded after a 3-day exposure (Figure 6a).…”

Accommodation of tin in tetragonal ZrO2

“…an outer layer of predominantly columnar monoclinic ZrO 2 , a 50-80 nm layer containing equiaxed tetragonal ZrO 2 , often a 100-200 nm layer of sub-stoichiometric Zr-oxide and finally α-Zr metal (saturated with oxygen close to the metal-oxide interface) [6][7][8].…”

Investigating the Effect of Zirconium Oxide Microstructure on Corrosion Performance: A Comparison between Neutron, Proton, and Nonirradiated Oxides

“…The transitions in corrosion kinetics are often attributed to the interconnectivity of pores and cracks in the oxide, allowing the cathodic reaction to occur closer to the metal oxide interface [4], [10], [11]. The destabilisation of the tetragonal phase during oxide growth has been cited in the literature as a possible cause of the breakdown of the protective oxide and subsequent transition in corrosion kinetics [7], [12]- [15]. The extensive transformation from tetragonal to monoclinic oxide during growth leads to disruption of the protective oxide and the development of extensive networks of transformation twin boundaries [7], [10], [16], [17].…”