Abstract

The influence of variable reaction time (tr) on surface/textural properties (surface area, total pore volume, and pore diameter) of carbon-encapsulated magnetite (Fe3O4@C) nanocomposites fabricated by a hydrothermal process at 190 °C for 3, 4, and 5 h was studied. The properties were calculated using the Brunauer–Emmett–Teller (BET) isotherms data. The nanocomposites were characterised using Fourier transform infrared spectroscopy, X-ray diffraction analysis, thermogravimetry, and scanning and transmission electron microscopies. Analysis of variance shows tr has the largest effect on pore volume (F value = 1117.6, p value < 0.0001), followed by the surface area (F value = 54.8, p value < 0.0001) and pore diameter (F value = 10.4, p value < 0.001) with R2-adjusted values of 99.5%, 88.5% and 63.1%, respectively. Tukey and Fisher tests confirmed tr rise to have caused increased variations in mean particle sizes (11–91 nm), crystallite sizes (5–21 nm), pore diameters (9–16 nm), pore volume (0.017–0.089 cm3 g−1) and surface area (7.6–22.4 m2 g−1) of the nanocomposites with individual and simultaneous confidence limits of 97.9 and 84.4 (p-adj < 0.05). The nanocomposites’ retained Fe–O vibrations at octahedral (436 cm−1) and tetrahedral (570 cm−1) cubic ferrite sites, modest thermal stability (37–60 % weight loss), and large volume-specific surface area with potential for catalytic application in advanced oxidation processes.

Highlights

  • Accepted: 13 October 2021In recent years, concerted efforts have been made to develop magnetite (Fe3 O4 )nanocomposite materials with improved surface properties suitable for specific applications in diverse fields

  • The results show that the mean particle diameter (DTEM ) for the nanocomposites Fe3 O4 @C-T190 t3, Fe3 O4 @C-T190 t4 and Fe3 O4 @C-T190 t5 were 67 ± 19, 16 ± 5, and 77 ± 14 nm, respectively, in contrast to the mean diameter of 30 ± 9 nm recorded for the parent Fe3 O4 NPs (Figure 5l)

  • The results show that Fe3 O4 @C-T190 t4 has the highest surface area, total pore volumes and pore diameters and the smallest crystallite grain size and particle size among the three Fe3 O4 @C nanocomposites

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Summary

Introduction

Accepted: 13 October 2021In recent years, concerted efforts have been made to develop magnetite (Fe3 O4 )nanocomposite materials with improved surface properties suitable for specific applications in diverse fields. NPs from agglomeration and deterioration in chemical stability, thereby maintaining their effective surface properties, making them compatible for applications in both inorganic and organic processes It involves synthesising Fe3 O4 @C nanostructures by heating at reaction temperatures and pressures above the ambient conditions of boiling water for a given reaction time, with the mixture of precursors in aqueous media as reported in the literature [14,15]. The method depends on precursor concentrations, the nature of the aqueous solvent, the stabilising agent, the type of precursor, the heating temperature, and the reaction time, which considerably influence the final products. It gives relatively low Published: 16 October 2021

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