PNNL

Abstract

Intergranular (IG) attack regions and stress-corrosion cracks in alloy 600 U-bend samples tested in 330C, pressurized-water-reactor water have been characterized by analytical transmission electron microscopy (ATEM). Observations of cross-sectional samples revealed short oxidized zones preceding crack tips and narrow (10-nm wide), deeply penetrated, oxidized zones along grain boundaries exposed along open cracks. High-resolution TEM imaging and fine-probe analysis were used to determine the local chemistries and structures in these corrosion-affected zones. Matrix areas surrounding the crack tips appeared highly strained, whereas the IG penetrations generally did not. The predominant oxide structure found along crack walls and just ahead of crack tips was NiO with metal-atom ratios similar to the alloy. The attacked grain boundaries off open cracks contained similar fine-grained NiO-structure oxide together with local areas of Cr-rich oxide and Ni-rich metal. In contrast, Cr-rich oxide identified as Cr2O3 predominated at the leading edges of the IG attack. Stereoscopic imaging of these tip structures revealed nm-scale porosity and tunnels within the oxide and pores along the grain-boundary plane ahead of the oxide. The general interpretation of these results is that IG attack and cracking follows local dissolution or oxidation and the formation of pores at grain boundaries. This degradation occurs at the nanometer scale and therefore requires high-resolution ATEM methods to reveal detailed characteristics. Experimental support for several possible IG degradation mechanisms is considered.