X‐ray reflectivity measurement of interdiffusion in metallic multilayers during rapid heating

• Published in: Journal of synchrotron radiation Vol. 24; no. 4; pp. 796 - 801
• Main Authors: Liu, J. P., Kirchhoff, J., Zhou, L., Zhao, M., Grapes, M. D., Dale, D. S., Tate, M. D., Philipp, H. T., Gruner, S. M., Weihs, T. P., Hufnagel, T. C.
• Format: Journal Article
• Language: English
• Published: 5 Abbey Square, Chester, Cheshire CH1 2HU, England International Union of Crystallography 01.07.2017
• Subjects: interdiffusion; multilayer; NUCLEAR PHYSICS AND RADIATION PHYSICS; Research Papers; X-ray reflectivity; interdiffusion; X-ray reflectivity; multilayer
• ISSN: 1600-5775; 0909-0495; 1600-5775
• DOI: 10.1107/S1600577517008013

A technique for measuring interdiffusion in multilayer materials during rapid heating using X‐ray reflectivity is described. In this technique the sample is bent to achieve a range of incident angles simultaneously, and the scattered intensity is recorded on a fast high‐dynamic‐range mixed‐mode pixel array detector. Heating of the multilayer is achieved by electrical resistive heating of the silicon substrate, monitored by an infrared pyrometer. As an example, reflectivity data from Al/Ni heated at rates up to 200 K s−1 are presented. At short times the interdiffusion coefficient can be determined from the rate of decay of the reflectivity peaks, and it is shown that the activation energy for interdiffusion is consistent with a grain boundary diffusion mechanism. At longer times the simple analysis no longer applies because the evolution of the reflectivity pattern is complicated by other processes, such as nucleation and growth of intermetallic phases. A method for in situ X‐ray reflectivity measurements on the millisecond time scale is described, and its use for measuring interdiffusion in metallic multilayers is illustrated.