Mechanisms of high-entropy carbide formation (TiVTaNbW)C via high-energy milling: structural, chemical, and spectroscopic analysis

Materials Science and Engineering B-Advanced Functional Solid-State Materials

2026-01

High-entropy carbide powder

High-energy milling

Intermetallic Laves phases

Metallic powders

High-entropy alloy powder

This study reports a two-step high-energy milling (HEM) route for synthesizing equimolar high-entropy carbide (TiVTaNbW)C powders directly from elemental metals and graphite, without post-milling heat treatments. In the first stage, equiatomic Ti0.2V0.2Ta0.2Nb0.2W0.2 alloys were produced by milling for 6, 12, and 18 h; in the second stage, the alloys were milled with graphite (1:1 M ratio) for 6 and 12 h at 500 rpm. The powders were characterized by SEM/EDS, XRD, FTIR, and TOC analysis. XRD confirmed the presence of the high-entropy carbide phase along with minor intermetallic and binary carbide residues. FTIR revealed metal–carbon bonding and surface hydroxyl/carbonate species, consistent with mild surface oxidation during milling. TOC quantified 6.549 wt% C versus the theoretical 9.74 wt%, evidencing a carbon deficit that may contribute to the residual phases. Prolonged milling enhanced elemental homogeneity and reduced crystallite size. These findings confirm the successful formation of a high-entropy carbide phase, demonstrating the potential of this synthesis method for producing homogeneous carbide powders