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

IF 4.6 3区材料科学 Q2 MATERIALS SCIENCE, MULTIDISCIPLINARY

Materials Science and Engineering: B Pub Date : 2025-09-22 DOI:10.1016/j.mseb.2025.118787

Anderson C. Marques , Thalita Q. Silva , Pâmala S. Vieira , Celmo Hudson Reis Paula , Maria J.S. Lima , Rubens M. Nascimento , Marcello Filgueira , Uílame U. Gomes , Meysam Mashhadikarimi

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Abstract

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 Ti_0.2V_0.2Ta_0.2Nb_0.2W_0.2 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.

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高能铣削形成高熵碳化物（TiVTaNbW）C的机理：结构、化学和光谱分析

本研究报告了一种两步高能铣削（HEM）路线，用于直接从元素金属和石墨合成等摩尔高熵碳化物（TiVTaNbW）C粉末，而无需铣削后热处理。第一阶段分别铣削6、12、18 h制备等原子Ti0.2V0.2Ta0.2Nb0.2W0.2合金；在第二阶段，合金与石墨（1:1 M比）在500 rpm下铣削6和12 h。采用SEM/EDS、XRD、FTIR和TOC分析对粉末进行了表征。XRD证实了高熵碳化物相的存在以及少量的金属间化合物和二元碳化物残留。FTIR显示金属-碳键和表面羟基/碳酸盐物种，与铣削过程中轻微的表面氧化一致。TOC量化的碳含量为6.549 wt%，而理论的碳含量为9.74 wt%，这表明碳亏缺可能导致剩余相的形成。延长磨矿时间提高了元素均匀性，减小了晶粒尺寸。这些发现证实了高熵碳化物相的成功形成，证明了这种合成方法在制备均匀碳化物粉末方面的潜力。

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来源期刊

Materials Science and Engineering: B 工程技术-材料科学：综合

CiteScore

5.60

自引率

2.80%

发文量

481

审稿时长

3.5 months

期刊介绍： The journal provides an international medium for the publication of theoretical and experimental studies and reviews related to the electronic, electrochemical, ionic, magnetic, optical, and biosensing properties of solid state materials in bulk, thin film and particulate forms. Papers dealing with synthesis, processing, characterization, structure, physical properties and computational aspects of nano-crystalline, crystalline, amorphous and glassy forms of ceramics, semiconductors, layered insertion compounds, low-dimensional compounds and systems, fast-ion conductors, polymers and dielectrics are viewed as suitable for publication. Articles focused on nano-structured aspects of these advanced solid-state materials will also be considered suitable.