New method for the preparation of S doped Fe samples characterized by AES and TOF‐SIMS depth profiling

A new method for the preparation of sulfur (S) doped iron (Fe) samples is presented. The required amount of S in Fe is obtained by allowing the vaporized form of S to diffuse into a Fe sample (10 mm diameter, 0.5 mm thick) kept at a temperature of 750 K. Depth profile analysis using Auger Electron Spectroscopy and Time‐of‐Flight Secondary Ion Mass Spectrometry (TOF‐SIMS) showed that the method is reproducible and can be used for the preparation of samples with different S concentrations. It was also found that S deposited onto Fe forms the desired FeS phase, which will prevent S from evaporating when the sample is annealed. Prepared samples were annealed to obtain homogeneity of S in Fe, after which the amount of S in the respective samples was determined by quantitative TOF‐SIMS. The outcome of the results suggests the application of this method to other high melting point host and low melting point dopant systems. Copyright © 2014 John Wiley & Sons, Ltd.

[1]  M. Madito,et al.  The diffusion doping of Cu crystals with 0.1 at.% In at high annealing temperatures for surface segregation measurements , 2013 .

[2]  Y. Mine,et al.  Strengthening and hydrogen embrittlement of ultrafine-grained Fe–0.01 mass% C alloy processed by high-pressure torsion , 2011 .

[3]  M. Balogh,et al.  Hydrogen environment embrittlement of an ODS RAF steel – Role of irreversible hydrogen trap sites , 2010 .

[4]  O. Vinogradov,et al.  Numerical tensile tests of BCC iron crystal with various amounts of hydrogen near the crack tip , 2006 .

[5]  J. Terblans,et al.  Segregation of Sn and Sb in a ternary Cu(1 0 0)SnSb alloy , 2005 .

[6]  M. F. Pillis,et al.  Microstructural Characterization of Reaction Products on Iron Based Alloys Exposed to H2/H2S Atmospheres at High Temperatures , 2002 .

[7]  Thomas Stephan,et al.  TOF-SIMS in Cosmochemistry , 2001 .

[8]  Jian-Sheng Wang.  The thermodynamics aspects of hydrogen induced embrittlement , 2001 .

[9]  J. Wang,et al.  Kinetics near the discontinuous surface transition in the Cu(Ag)(111) binary segregating system , 1999 .

[10]  P. Castello,et al.  The sulfidation of two FeCe alloys in H2H2S mixtures at 600–800 °C , 1997 .

[11]  J. Cabané,et al.  Thermodynamics of sulphur adsorption on iron , 1993 .

[12]  D. R. Penn,et al.  Calculations of electron inelastic mean free paths. III. Data for 15 inorganic compounds over the 50–2000 eV range , 1991 .

[13]  Lawrence H. Bennett,et al.  Binary alloy phase diagrams , 1986 .

[14]  Ryuichi Shimizu,et al.  Quantitative Analysis by Auger Electron Spectroscopy , 1983 .