The aim of this work was to study the corrosion behavior of a Fe-Cr-Ni alloy (310 H stainless steel) in water at a supercritical temperature of 550 °C and a pressure of 250 atm for up to 2160 h. At supercritical temperature, water is a highly aggressive environment, and the corrosion of structural materials used in a supercritical water-cooled nuclear reactor (SCWR) is a critical problem. Selecting proper candidate materials is one key issue for the development of SCWRs. After exposure to deaerated supercritical water, the oxides formed on the 310 H SS surface were characterized using a gravimetric analysis, a metallographic analysis, and electrochemical methods. Gravimetric analysis showed that, due to oxidation, all the tested samples gained weight, and oxidation of 310H stainless steel at 550 °C follows parabolic rate, indicating that it is driven by a diffusion process. The data obtained by microscopic metallography concord with those obtained by gravimetric analysis and show that the oxides layer has a growing tendency in time. At the same time, the results obtained by electrochemical impedance spectroscopy (EIS) measurements indicate the best corrosion resistance of Cr, and (Fe, Mn) Cr2O4 oxides developed on the samples surface after 2160 h of oxidation. Based on the results obtained, a strong correlation between gravimetric analysis, metallographic analysis, and electrochemical methods was found.
The paper’s aim is the assessment of corrosion behaviour of a CrNx-coated 310 H stainless steel under simulated supercritical water conditions (550 °C and 25 MPa) for up to 2160 h. The CrNx coating was obtained by the thermionic vacuum arc (TVA) method. The oxides grown on this coating were characterized using metallographic and gravimetric analysis, SEM with EDS, and grazing incidence X-ray diffraction (GIXRD). A diffusion mechanism drives oxidation kinetics because it follows a parabolic law. By XRD analysis, the presence of Cr2O3 and Fe3O4 on the surface of the autoclaved CrNx-coated 310 H samples were highlighted. Corrosion susceptibility assessment was performed by electrochemical impedance spectroscopy (EIS) and linear potentiodynamic polarization. EIS impedance spectra show the presence of two capacitive semicircles in the Nyquist diagram, highlighting both the presence of the CrNx coating and the oxide film formed during autoclaving on the 310 H stainless steel. Very low corrosion rates, with values up to 11 nm × year−1, obtained in the case of autoclaved for 2160 h, CrNx-coated samples indicated that the oxides formed on these samples are protective and provide better corrosion resistance. The determination of micro hardness Vickers completed the above investigation.
The total 14C content and its partition between inorganic and organic species were measured on irradiated Zy-4 samples from a CANDU spent fuel rod transferred from Cernavoda Nuclear Power Plant (NPP). Long-term leaching tests and accelerated corrosion tests were carried out to measure the 14C release and corrosion rate, respectively, in chemical conditions relevant to cementitious environment. Experimentally measured 14C inventory was compared to the theoretically one predicted based on the irradiation history and impurity content of Zy-4 by means of ORIGEN computations. CANDU SF claddings have a 14C content of around 2 × 104 Bq/g of Zy-4, mainly as organic compounds (more than 99%). The total 14C content measured by acid dissolution/wet oxidation method is in good agreement with the value estimated by ORIGEN simulations for an average burn-up of 7 MWd/kgU. The total 14C released as dissolved species after 18 days and 18 months of Zy-4 immersing in alkaline solution are similar, indicating that a small amount of 14C was available as instant release fraction (0.05% from the initial 14C content) followed by a very low release rate that could not be measured by liquid scintillation counting. In alkaline conditions, 14C is released predominantly (∼70%) as soluble species, but also inorganic 14C was measured as gaseous species. From the soluble 14C released during leaching test, more than 60% was found to be as organic species. Generally, corrosion rates values ranging between 46 and 130 nm/yr were measured by the linear polarization resistance method. In addition, defects and cracks were observed on the oxide layer by scanning electron microscopy (SEM) investigation.
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