Abstract
Background: In the last decade, Fe3O4 nanoparticles have been intensively investigated for medical applications. Up now, various chemical methods have been applied for their preparation. Although, these methods have been improved in the recent years, however, higher temperature (100–300 oC), toxic and expensive precursors and limited controllability of particle morphology and size still the challenges. As an alternative method, cathodic electrochemical deposition can be effectively applied for the preparation of metal oxides and hydroxides nanoparticles. However, this electrochemical route has been rarely applied into the synthesis of iron oxide nanoparticles, and surface coating of these NPs has not been reported through this method.
Methods: A two- electrode electrochemical set up was used in all the electrodeposition experiments, which includes a cathodic stainless-steel substrate centered between two parallel graphite anodes. Naked Fe3O4NPs were prepared by galvanostatic electrodeposition from both electrolytes with applying the current density of 5 mAcm-2 for 1h. For preparation of PEI coated NPs, composition of electrolyte was just changed, and PEI polymer with value of 1 g L–1 was added to the electrolyte solution. The prepared NPs were characterized through FE-SEM, TEM, XRD, DLS and VSM techniques. Results: The XRD patterns have the well-defined and relative broad diffraction peaks which is indexed as spinal structure of magnetite. The Scherrer calculations revealed that the naked and PEI coated samples have sizes of 9.2 and 8.7 nm, respectively. FE-SEM images clearly revealed that both samples have well-defined particle shape and no obvious aggregation is observed for polymer coated NPs. The sizes of 10 nm and 15 nm were measured for the naked and PEI coated Fe3O4 nanoparticles, respectively. This size increase proves the possibility of adlayer formation on the Fe3O4 particles during their formation on the cathode surface. The IR vibrations qualitatively confirmed the successful coating of PEI on the surface of Fe3O4 NPs. DSC curve of coated NPs exhibits two main endothermic peaks at 250 and 285 ºC, and TG curves showed two regions of maximum rate of mass loss located at these temperatures with total weight loss of 29.3%. This weight loss in the TG profile proofed the presence of PEI onto the surface of NPs. For the naked NPs, the mean hydrodynamic diameter was measured to be 16 nm. For the PEI coated NPs, DLS profile exhibits mean size of 50 nm. This size is some larger than that of observed for the naked particles (i.e. 16 nm) and completely implicates the presence of polymer layer on the surface of deposited Fe3O4 NPs. The VSM data confirmed the proper superparamagnetic behavior of the prepared magnetite NPs. Conclusion: An efficient and simple platform was proposed to fabricate naked and polyethyleneimine coated Fe3O4 nanoparticles. The FE-SEM and TEM observations indicated that the deposited coated NPs have spherical shape with size about 10nm. confirmed that the pure magnetite crystal phase of the obtained nanoparticles. VSM analysis of the prepared Fe3O4 NPs showed their superparamagnetic characters. The XRD and IR data specified that the prepared nanoparticles have favorable size and suitable magnetic properties for biomedical applications. It was stated that our applied method is efficient platform for in situ preparation of PEI coated Fe3O4NPs from ethanol medium.Keywords: Cathodic electrosynthesis, Fe3O4, magnetic properties, nanoparticles, polymer coating., Cathodic electrosynthesis, Fe3O4, magnetic properties, nanoparticles, polymer coating.
Graphical Abstract
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