In Situ Sample Environment for Studying Corrosion of Nuclear Materials
Currently there is lack of fundamental understanding of kinetics and reaction mechanisms that occur at nuclear cladding-steam interface under extreme environments in the nuclear reactors. Such understanding is vital to design and develop advanced cladding materials for more economical and safer nuclear power. We present advanced in situ sample environment for probing solid-fluid interfaces using high resolution synchrotron methods for studying early stages of corrosion including development of oxide layer as corrosion proceeds. Both X-ray diffraction and X-ray fluorescence methods will be discussed to probe structural and elemental composition changes under steam environment using corrosion resistant cell at high temperatures. High intensity and brightness of synchrotron coupled with advanced in situ sample environment developed, presents an opportunity to understand the fundamental interfacial processes involved in degradation of materials. The in situ sample environment is optimized for XRD and XRF data collection at NSLS-II and will be available to all users through the proposal process. The in situ sample environment is built to study the interfacial interactions at temperatures and pressures up to 400 deg. C and 1500 psi. It consists of three main parts; the distribution manifold, the pressure vessel, and the reaction cell as shown in Figure 1. Water is allowed to heat up to 350 deg. C inside the pressure vessel to produce steam which is delivered to reaction cell using insulated delivery system. The cell design is adapted from J. Diefenbacher, et. al. However, it is modified for corrosion applications in steam environments. The reaction cell and sample holder are made from hastelloy due to its high corrosion resistance. The reaction cell is surrounded by copper heating block to control its temperature independently from the rest of the system. Lab view based platform is developed for remote monitoring of pressure and temperature. The sample environment was commissioned at 6-IDD beamline in the Advanced Photon Source, for grazing incidence XRD corrosion studies. Metallic Zr sample (200 μm thickness) was used due to its faster oxidation kinetics as compared to Zircaloy. Sample was exposed to steam at 350 deg. C and 50 psi for a total time of 64 hours. Results showed the presence of α-Zr as the dominant phase. After 32 hours of exposure to steam, three oxide peaks in the low diffraction angle side started to develop with time. These peaks are attributed to the growth of substoichiometric zirconium oxide phases (Zr{sub 3}O and Zr{sub 3}O{sub 1-x}). (authors)