Comprehensive structural, morphological, chemical, and vibrational characterization of VSi₂ intermetallic alloy synthesized by spark plasma sintering

This study presents a comprehensive investigation of the structural, microstructural, chemical, surface, and vibrational properties of a VSi₂ intermetallic alloy synthesized by Spark Plasma Sintering (SPS) at 1415 °C under a pressure of 50 MPa. The phase and crystal structure, microstructure, elemental composition, surface topography, and vibrational characteristics were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), atomic force microscopy (AFM), Fourier-transform infrared (FTIR) spectroscopy, and Raman spectroscopy, respectively. The sintered sample exhibited a relative density of 95%. XRD analysis identified hexagonal VSi₂ as the primary phase, with an average coherent crystallite size of 56 ± 18 nm and an estimated dislocation density of 3.2 × 10 ¹ ⁴ m⁻² , after accounting for instrumental broadening. SEM analysis revealed morphological grain sizes ranging from 194 to 823 nm, while no large open pores or macroscopic cracks were observed in the analyzed regions. AFM measurements indicated a relatively uniform surface topography, with a maximum surface relief height of 195 nm. EDS analysis showed a V/Si composition close to the nominal stoichiometry of VSi₂. The Si–O-related features observed in the FTIR spectrum suggest possible partial surface oxidation due to atmospheric exposure, whereas the V–Si-related bands are consistent with the vibrational characteristics of the VSi₂ phase. The Raman spectrum exhibited the main vibrational features associated with VSi₂. Overall, the results demonstrate the formation of a polycrystalline VSi₂ material with a relative density of 95%, a hexagonal VSi₂ primary phase, and submicrometer-scale morphological grains under the applied SPS conditions. This comprehensive characterization provides an experimental basis for evaluating the structural characteristics of VSi₂ and for further investigation of its functional properties.

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