Hybrid Nanocomposites of Fe3O4/SiO2-EDTA: Holistic Comparison of One-Step and Two-Step Modification Methods

Fe3O4/SiO2-EDTA materials have been used for diverse applications and they have been modification by different methods, but a comparison is lacking between their physicochemical characteristics. This work aimed to compare the physicochemical characteristics of the Fe3O4/SiO2-EDTA nanocomposite obtained by four methods, whose modification of the Fe3O4 surface with SiO2-EDTA occurs in one or two steps, with not hazardous chemicals. In the one-step methods (M1 and M2), Fe3O4 particles were coated and functionalized in consecutive steps (by sonication in M1 and mechanical stirring in M2). In the two-step methods (M3 and M4), the Fe3O4 particles were primarily coated with silica and then functionalized with TMS-EDTA (by sonication in M3 and mechanical stirring in M4). The Fe3O4/SiO2-EDTA nanocomposites were characterized by XRD, TEM, EDX, BET, SQUID magnetometry, FTIR, XPS, and zeta potential. The TEM highlighted that the nanocomposites from methods M1 and M2 there is the simultaneous presence of magnetite particles coated and uncoated with silica, while those from M3 and M4 were totally coated, besides the nanocomposites from M2 and M3 showed to be more aggregated than those from the other methods. The presence of EDTA on the surface of the nanocomposites was evidenced by the carboxyl groups in the FTIR spectra and by the nitrogen in the XPS spectra. The nanocomposites from M3 and M4 presented a higher content of nitrogen than those from M1 and M2, and those from M4 also presented a higher content of carbon than those from M3. Overall, the Fe3O4/SiO2-EDTA nanocomposites from two-step methods showed better SiO2 coating and EDTA functionalization than those from one-step methods, and those from M4 presented the best physicochemical characteristics, being this method recommended for their modification for future applications.