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<p>This study reports the efficient synthesis of multi-walled carbon nanotubes (MWCNTs) decorated with zirconia (ZrO<sub>2</sub>) nanoparticles using a rapid microwave-assisted method. High-resolution transmission electron microscopy (HR-TEM) and X-ray diffraction (XRD) confirmed the formation of a uniform coating of crystalline cubic zirconia on the MWCNT surfaces. Raman spectroscopy revealed that the structural integrity of the nanotubes was preserved during the functionalization and deposition processes, maintaining a constant I<sub><i>D</i></sub>/I<sub><i>G</i></sub> ratio of 0.30. Thermogravimetric analysis (TGA) quantified a significant zirconia loading of 22.0% and demonstrated high thermal stability for the resulting hybrid material. The ZrO<sub>2</sub>/MWCNT composite was evaluated as an adsorbent for the removal of methylene blue (MB) from aqueous solutions. Under optimized conditions (pH 7.5 and 0.025&#xa0;g dosage), the composite achieved a maximum removal efficiency of 98.04%, significantly outperforming pristine MWCNTs (56.7%). Kinetic studies showed that the adsorption process followed a pseudo-second-order model (<i>R</i><sup>2</sup> = 0.9998), indicating a rate-limiting step governed by chemisorption. Equilibrium data were best described by the Langmuir isotherm model, with a maximum monolayer adsorption capacity (<i>q</i><sub>m</sub>) that increased from 208.3 to 238.1&#xa0;mg/g as the temperature rose from 283 to 313&#xa0;K, confirming the endothermic nature of the process. Furthermore, the composite exhibited remarkable performance across a wide pH range (2.5–12.0) and temperature fluctuations. These results demonstrate that ZrO<sub>2</sub>/MWCNT hybrids are robust, high capacity, and versatile adsorbents for the treatment of industrial wastewater contaminated with organic dyes.</p>

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Microwave-assisted synthesis of ZrO2/MWCNT nanocomposites for the efficient removal of methylene blue

  • 期刊论文

  • 发表日期：

    2026年7月22日

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  • Alexis Pérez Gasquez y Marín,
  • Julián López-Tinoco,
  • Ricardo Rangel,
  • Javier Lara-Romero,
  • Andrés Alejandro Damian-Reyna,
  • Nicolas Cayetano-Castro

摘要

This study reports the efficient synthesis of multi-walled carbon nanotubes (MWCNTs) decorated with zirconia (ZrO2) nanoparticles using a rapid microwave-assisted method. High-resolution transmission electron microscopy (HR-TEM) and X-ray diffraction (XRD) confirmed the formation of a uniform coating of crystalline cubic zirconia on the MWCNT surfaces. Raman spectroscopy revealed that the structural integrity of the nanotubes was preserved during the functionalization and deposition processes, maintaining a constant ID/IG ratio of 0.30. Thermogravimetric analysis (TGA) quantified a significant zirconia loading of 22.0% and demonstrated high thermal stability for the resulting hybrid material. The ZrO2/MWCNT composite was evaluated as an adsorbent for the removal of methylene blue (MB) from aqueous solutions. Under optimized conditions (pH 7.5 and 0.025 g dosage), the composite achieved a maximum removal efficiency of 98.04%, significantly outperforming pristine MWCNTs (56.7%). Kinetic studies showed that the adsorption process followed a pseudo-second-order model (R2 = 0.9998), indicating a rate-limiting step governed by chemisorption. Equilibrium data were best described by the Langmuir isotherm model, with a maximum monolayer adsorption capacity (qm) that increased from 208.3 to 238.1 mg/g as the temperature rose from 283 to 313 K, confirming the endothermic nature of the process. Furthermore, the composite exhibited remarkable performance across a wide pH range (2.5–12.0) and temperature fluctuations. These results demonstrate that ZrO2/MWCNT hybrids are robust, high capacity, and versatile adsorbents for the treatment of industrial wastewater contaminated with organic dyes.