Grain Boundary Composition and Intergranular Fracture of Steels. Volume 1. Detection of Grain Boundary Segregation in Steels. Final Report

摘要

Several alternative techniques for the measurement of grain boundary composition in iron-base alloys were evaluated, including Secondary Ion Mass Spectroscopy (SIMS), Analytical Electron Microscopy (AEM), and chemical/electrochemical etching. Potential problems in grain boundary composition measurements of CrMoV and NiCrMoV steels by AES were identified as a result of AES, high-resolution AES, and AEM characterization. Significant differences were identified in comparing peak height ratios on identical specimens using PHI 545, 560, and 595 systems. These differences were due to instrument parameters that are generally not known for any particular AES sysyem. Localized ductile tearing regions and the presence of second phase particles on intergranular faces exposed by fracture led to significant point to point composition variations. Phosphorus levels varied by more than 50% across individual grain boundary facets. Copper-tin intermetallics were observed by AEM in the CrMoV steel and nickel-tin intermetallics in the NiCrMoV steel. Much of the tin documented by AES at grain boundaries could be explained by the presence of these small intermetallic precipitates. (ERA citation 10:016538)