Precipitation Study in a High Temperature Austenitic Stainless Steel using Low Voltage Energy Dispersive X-ray Spectroscopy

Abstract: Precipitation of second phase particles is a key factor dominating the mechanical properties of high temperature alloys. In order to control and optimize the precipitation effect it is of great importance to study the role of alloying elements in the formation and stability of precipitates. As a favored family of corrosion and creep resistant austenitic stainless steels the 20Cr-25Ni alloy was modified by addition of copper, molybdenum, nitrogen, niobium and vanadium. A set of alloys with similar matrix but varying contents of niobium, vanadium and nitrogen were prepared. Sample preparation process included melting, hot forging, solution annealing and finally aging for 500 h at 700, 800 and 850 ºC.Light optical and scanning electron microscopy revealed micron-scale precipitates on grain and twin boundaries as well as sub-micron intragranular precipitates in all samples. Characterization of precipitates was carried out by means of energy dispersive X-ray spectroscopy (EDS). Among micron-scale precipitates M23C6 carbide was the dominant phase at 700 ºC aging temperature; whereas silicon-rich eta phase (M5SiC) was the main precipitate in samples aged at 800 and 850 ºC. A few sigma phase particles were found in one of the niobium containing samples aged at 700 and 800 ºC. Sub-micron intragranular precipitates were analyzed using low voltage EDS. The spatial resolution of EDS microanalysis at 5 kV accelerating voltage was estimated as almost 100 nm which was at least eight times better than that using the ordinary 20 kV voltage. Also, low voltage EDS revealed the presence of light elements (carbon, nitrogen and boron) in the composition of sub-micron particles thanks to the less matrix effect in absorption of low energy X-rays of light elements. In samples aged at 700 ºC niobium-rich and vanadium-rich carbonitrides were found as the dominant precipitates; whereas they contained much less carbon in samples aged at 800 ºC and mostly became carbon-free nitrides with well-defined cuboidal shapes at 850 ºC aging temperature. This showed that niobium/vanadium-rich nitride phases are stable precipitates at aging temperatures above 700 ºC.The drawbacks of low voltage EDS were indicated as high detection limit (no detection of low- content elements), poor accuracy of quantitative analysis and high sensitivity to surface contamination. Some possible ways to improve the accuracy of low voltage EDS, e.g. longer acquisition time were examined and some other suggestions are proposed for future works.