Strains in Thermally Growing Alumina Films Measured In-Situ Using Synchrotron X-Rays

Abstract

Strains in thermally grown oxides have been measured in-situ, as the oxides develop and evolve. Extensive data have been acquired from oxides grown in air at elevated temperatures on different model alloys that form Al2O3. Using synchrotron x-rays at the Advanced Photon Source (Beamline 12BM, Argonne National Laboratory), Debye-Scherrer diffraction patterns from the oxidizing specimen were recorded every 5 minutes during oxidation and subsequent cooling. The diffraction patterns were analyzed to determine strains in the oxides, as well as phase changes and the degree of texture. To study a specimen's response to stress perturbation, the oxidizing temperature was quickly cooled from 1100 to 950oC to impose a compressive thermal stress in the scale. This paper describes this new experimental approach and gives examples from oxidized β-NiAl, Fe-20Cr-10Al, Fe-28Al-5Cr and H2- annealed Fe-28Al-5Cr (all at. %) alloys to illustrate some current understanding of the development and relaxation of growth stresses in Al2O3.