Quantitative analysis of radiation-induced grain-boundary segregation measurements

Abstract

Radiation-induced and precipitation-induced grain-boundary segregation profiles are routinely measured by scanning-transmission electron microscopy using energy-dispersive X-ray spectroscopy (STEM-EDS). However, radiation-induced grain-boundary segregation (RIS) profiles achieved at low and moderate temperatures are exceedingly narrow, typically less than 10 nm full width at half maximum. Since the instrumental spatial resolution can be a significant fraction of this value, the determination of grain boundary compositions poses a formidable challenge. STEM-EDS and Auger electron spectroscopy (AES) measurements are reported, performed on controlled-purity alloys of type 304L stainless steel irradiated with 3.4 MeV protons to 1 displacement per atom at 400°C. Because of statistical noise and the practical lower limit on the step size in STEM, deconvolution of the measured data does not yield physical results. An alternative analysis of STEM data is presented. Numerical calculations of RIS profiles are convoluted with the instrumental broadening function and modified iteratively to fit the data, yielding a “best estimate” profile. This “best estimate” is convoluted with the Auger intensity profile to yield a simulated AES measurement, which is compared with the actual AES measurement to provide an independent test of the validity of the “best estimate”. For impurities with a narrow segregation profile and an Auger electron escape depth of one monolayer, a combination of STEM and AES data allows a determination of the width of the segregated layer. It is found that, in an ultrahigh-purity alloy doped with P, the latter is essentially contained in a single monolayer.