A novel facile, fast, and efficient microwave-assisted method was developed to synthesize a number of diverse nanostructured motifs (ranging from nanorods to nanoflowers) of VS₄ along with its associated composite heterostructures, VS₄/multi-walled carbon nanotube (MWNT; i.e., multi-walled carbon nanotubes). In particular, we have probed and correlated the effects of a number of specific experimental variables, including primarily precursor, solvent, temperature, and time. We noted that nanorods formed more readily with VO(acac)₂ as the vanadium precursor and n-methyl-2-pyrrolidone (NMP) as a polar reaction solvent. By contrast, we determined that hierarchical three-dimensional (3D) nanoflower-like assemblies, ranging in size from 100 to 200 nm in average diameter, could be controllably synthesized by using Na₃VO₄ as the vanadium precursor and an aqueous water: polar solvent mixture as the reaction medium. We also observed that VS₄ disintegrates, when in the presence of either air, solution, or a combination of these environments, and established that the extent of VS₄ nanorod decomposition could be almost fully prevented by storage under nitrogen. From an application’s perspective, our VS₄ is electrochemically active and shows behavior, consistent with the literature. In particular, as compared with pristine VS₄ nanorods alone, we observed enhanced electrochemical activity with (i) 3D hierarchical flower-like motifs, (ii) unique necklace-like VS₄ nanorod–MWNT composites, and (iii) samples in which as-prepared VS₄ nanorods had been annealed. Moreover, we found that the rational application of specific physical and chemical processing treatments, such as (i) thermal annealing to improve crystallinity, (ii) the addition of MWNTs to form conductive composites, and (iii) the evolution of morphology from one-dimensional (1D) nanorods to more complex 3D nanoflowers, was favorable to the resulting electrochemical performance with respect to increasing stability and reversibility.

Matthew Licht

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