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Quantification Problems in Depth Profiling of PWR Steels Using Ar+ Ion Sputtering and XPS Analysis

Published online by Cambridge University Press:  23 August 2006

Velislava A. Ignatova ,
Sven Van Den Berghe ,
Steven Van Dyck  and
Vladimir N. Popok
Velislava A. Ignatova
Affiliation:
SCK.CEN Reactor Materials Research (LHMA), Boeretang 200, 2400 Mol, Belgium Velislava Ignatova is now at the Fraunhofer Center for Nanotechnologies, Koenigsbruecker Strasse 180, 01099 Dresden, Germany
Sven Van Den Berghe
Affiliation:
SCK.CEN Reactor Materials Research (LHMA), Boeretang 200, 2400 Mol, Belgium
Steven Van Dyck
Affiliation:
SCK.CEN Reactor Materials Research (LHMA), Boeretang 200, 2400 Mol, Belgium
Vladimir N. Popok
Affiliation:
Department of Physics, Gothenburg University, 41296 Gothenburg, Sweden
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Abstract

The oxide scales of AISI 304 formed in boric acid solutions at 300°C and pH = 4.5 have been studied using X-ray photoelectron spectroscopy (XPS) depth profiling. The present focus is depth profile quantification both in depth and chemical composition on a molecular level. The roughness of the samples is studied by atomic force microscopy before and after sputtering, and the erosion rate is determined by measuring the crater depth with a surface profilometer and vertical scanning interferometry. The resulting roughness (20–30 nm), being an order of magnitude lower than the crater depth (0.2–0.5 μm), allows layer-by-layer profiling, although the ion-induced effects result in an uncertainty of the depth calibration of a factor of 2. The XPS spectrum deconvolution and data evaluation applying target factor analysis allows chemical speciation on a molecular level. The elemental distribution as a function of the sputtering time is obtained, and the formation of two layers is observed—one hydroxide (mainly iron–nickel based) on top and a second one deeper, mainly consisting of iron–chromium oxides.

Keywords

PWR steelsXPS depth profilingXPS quantificationerosion rate calibration
Type
MICROANALYSIS
Information
Microscopy and Microanalysis , Volume 12 , Issue 5 , October 2006 , pp. 432 - 437
Copyright
© 2006 Microscopy Society of America

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References

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