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<p>This study aims to evaluate how solvent composition and the presence of a reducing agent influence the morphology and crystallinity of tungsten-based structures synthesized via a microwave-assisted solvothermal method. The goal is to understand how these variables affect particle shape, size and phase formation in sulfur-enriched tungsten compounds. Four experimental conditions were tested, two focused on the effect of solvent composition, comparing pure ethylene glycol (EG) with a water–ethylene glycol mixture (WEG, while the other two explored the influence of sodium borohydride (NaBH<sub>4</sub>) as a reducing agent. In all cases, ammonium tetrathiotungstate (ATT) was used as the tungsten precursor, with an excess of elemental sulfur added to promote the formation of sulfur-rich phases. Synthesis reactions were carried out under microwave irradiation at 1200 W and 2.64&#xa0;GHz for one minute. The resulting materials were systematically characterized using Scanning Electron Microscopy (SEM), High Resolution Transmission Electron Microscopy (HR-TEM), Fourier-Transform Infrared Spectroscopy (FTIR), UV–Vis Diffuse Reflectance Spectroscopy (UV–Vis DRS) and X-ray Diffraction (XRD). SEM revealed distinct differences in morphology and particle, ranging from 0.01 to 6.5&#xa0;µm. Observed morphologies included tetragonal prisms, flakes, irregular agglomerates, and flower-like structures with solvent composition being the dominant factor influencing these features. HR-TEM provided further insights into nanoscale shape, size distribution, and internal structure XRD confirmed the formation of well-defined crystalline phases, identifying tungsten trioxide (WO<sub>3</sub>) in three samples and tungsten disulfide (WS<sub>2</sub>) in one.</p> Graphical abstract <p></p>

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Microwave-assisted synthesis of tungsten-based structures: effect of reaction medium composition on morphology and crystallinity

  • 期刊论文

  • 发表日期：

    2025年11月19日

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  • T. Guzmán-Barba,
  • M. Estrada-Flores,
  • C. M. Reza-SanGermán,
  • M. E. Manríquez-Ramírez,
  • O. G. Rojas-Valencia,
  • C. Encarnación-Gómez,
  • M. G. Hernández-Cruz

摘要

This study aims to evaluate how solvent composition and the presence of a reducing agent influence the morphology and crystallinity of tungsten-based structures synthesized via a microwave-assisted solvothermal method. The goal is to understand how these variables affect particle shape, size and phase formation in sulfur-enriched tungsten compounds. Four experimental conditions were tested, two focused on the effect of solvent composition, comparing pure ethylene glycol (EG) with a water–ethylene glycol mixture (WEG, while the other two explored the influence of sodium borohydride (NaBH4) as a reducing agent. In all cases, ammonium tetrathiotungstate (ATT) was used as the tungsten precursor, with an excess of elemental sulfur added to promote the formation of sulfur-rich phases. Synthesis reactions were carried out under microwave irradiation at 1200 W and 2.64 GHz for one minute. The resulting materials were systematically characterized using Scanning Electron Microscopy (SEM), High Resolution Transmission Electron Microscopy (HR-TEM), Fourier-Transform Infrared Spectroscopy (FTIR), UV–Vis Diffuse Reflectance Spectroscopy (UV–Vis DRS) and X-ray Diffraction (XRD). SEM revealed distinct differences in morphology and particle, ranging from 0.01 to 6.5 µm. Observed morphologies included tetragonal prisms, flakes, irregular agglomerates, and flower-like structures with solvent composition being the dominant factor influencing these features. HR-TEM provided further insights into nanoscale shape, size distribution, and internal structure XRD confirmed the formation of well-defined crystalline phases, identifying tungsten trioxide (WO3) in three samples and tungsten disulfide (WS2) in one.

Graphical abstract