Texture, residual stress and structural analysis of thin films using a combined X-ray analysis

• Published in: Thin solid films Vol. 450; no. 1; pp. 34 - 41
• Main Authors: Lutterotti, L., Chateigner, D., Ferrari, S., Ricote, J.
• Format: Journal Article Conference Proceeding
• Language: English
• Published: Lausanne Elsevier B.V 22-02-2004; Elsevier Science
• Subjects: Condensed matter: structure, mechanical and thermal properties; Diffraction; Exact sciences and technology; Multilayer; Physics; Reflectivity; Residual stress; Rietveld method; Single-crystal and powder diffraction; Structure and morphology; thickness; Structure of solids and liquids; crystallography; Surfaces and interfaces; thin films and whiskers (structure and nonelectronic properties); Texture; Thin film structure and morphology; Thin films; X-Ray; X-ray diffraction and scattering; X-ray reflectometry; Thin films; Reflectivity; Rietveld method; Diffraction; Multilayer; X-Ray; Texture; Residual stress; Cubic lattices; Inorganic compounds; Tetragonal lattices; Lead titanates; Transition element compounds; Roughness; Calcium Titanates; X-ray reflection; Residual stresses; XRD; Experimental study; Inclination; Thickness; Zirconia; Pole figures
• ISSN: 0040-6090; 1879-2731
• DOI: 10.1016/j.tsf.2003.10.150

Advanced thin films for today's industrial and research needs require highly specialized methodologies for a successful quantitative characterization. In particular, in the case of multilayer and/or unknown phases a global approach is necessary to obtain some or all the required information. A full approach has been developed integrating novel texture and residual stress methodologies with the Rietveld method (Acta Cryst. 22 (1967) 151) (for crystal structure analysis) and it has been coupled with the reflectivity analysis. The complete analysis can be done at once and offers several benefits: the thicknesses obtained from reflectivity can be used to correct the diffraction spectra, the phase analysis help to identify the layers and to determine the electron density profile for reflectivity; quantitative texture is needed for quantitative phase and residual stress analyses; crystal structure determination benefits of the previous. To achieve this result, it was necessary to develop some new methods, especially for texture and residual stresses. So it was possible to integrate them in the Rietveld, full profile fitting of the patterns. The measurement of these spectra required a special reflectometer/diffractometer that combines a thin parallel beam (for reflectivity) and a texture/stress goniometer with a curved large position sensitive detector. This new diffraction/reflectivity X-ray machine has been used to test the combined approach. Several spectra and the reflectivity patterns have been collected at different tilting angles and processed at once by the special software incorporating the aforementioned methodologies. Some analysis examples will be given to show the possibilities offered by the method.