Ductility evaluation of nitrided Zircaloy-4 cladding by ring compression testing

This study evaluated the embrittlement of Zircaloy-4 cladding by dry air and dry nitrogen environments as a function of process temperature and duration of exposure. A Netzsch thermogravimetric analyzer was used to measure the mass gain of cladding sections over time with specified temperature and gas flow programs. Oxidation of Zircaloy in dry air produced a brittle ZrO₂ layer with ductile unreacted metal. In contrast, nitridation of Zircaloy had a slower reaction rate but produced a brittle cladding that was more easily breached during ring compression tests. The ring compression tests demonstrated that ductility of Zircaloy cladding decreases as nitrogen pickup increases; a ductile-to-brittle transition occurs near a mass gain of 2.1 wt %. Nitridation showed minimal temperature dependency in ductility degradation, whereas oxidation showed significant temperature dependency in ductility degradation, with severe embrittlement occurring at 1200 °C. Optical micrographs confirmed the formation of uniform ZrN layers (approximately 12 µm thick) on the cladding surface, indicating that cladding embrittlement is primarily the result of nitrogen diffusion rather than metal layer thinning.