Sample Preparation and Determination of Trace Elements in High-Entropy Alloys by Total Reflection X-Ray Fluorescence (TXRF)

Abstract

High-entropy alloys (HEAs) have attracted significant attention in recent years owing to their exceptional material properties; however, trace impurities in these alloys can significantly affect their strength, toughness, and radiation resistance. This study employs total reflection X-ray fluorescence (TXRF) to determine the trace impurities in three common HEA powders prepared via suspension techniques. High-Z (Ca and Mn) and low-Z (Mg and Al) elements were quantified using the internal standard and calibration curve methods, respectively. The levels of high-Z elements are consistent with those determined using inductively coupled plasma – optical emission spectrometry (ICP-OES). Although the physical mechanisms exerted various effects on low-Z elements, qualitative and semi-quantitative analyses remained feasible, demonstrating the effectiveness of TXRF for impurities in HEAs. Additionally, the combination of suspension sample preparation and TXRF affords a nondestructive, rapid, and cost-effective methodology that requires minimal sample quantities. Consequently, TXRF is well suited for the rapid determination of impurities in HEAs.