Title:Effective Preparation, Characterization and In Situ Surface Coating of Superparamagnetic Fe3O4 Nanoparticles with Polyethyleneimine Through Cathodic Electrochemical Deposition (CED)
VOLUME: 13 ISSUE: 2
Author(s):Isa Karimzadeh, Mustafa Aghazadeh, Taher Doroudi, Mohammad Reza Ganjali, Peir Hossein Kolivand, Isa Karimzadeh, Mustafa Aghazadeh, Taher Doroudi, Mohammad Reza Ganjali and Peir Hossein Kolivand
Affiliation:Department of Physics, Faculty of Science, Islamic Azad University,, Nuclear Science and Technology Research Institute (NSTRI), P.O. Box 14395-834, Tehran,, Shefa Neuroscience Research Center, Khatam ol Anbia Hospital, Tehran,, Biosensor Research Center, Endocrinology and Metabolism Molecular-Cellular Sciences Institute, Tehran University of Medical Sciences, Tehran,, Shefa Neuroscience Research Center, Khatam ol Anbia Hospital, Tehran,, Department of Physics, Faculty of Science, Islamic Azad University,, Nuclear Science and Technology Research Institute (NSTRI), P.O. Box 14395-834, Tehran,, Shefa Neuroscience Research Center, Khatam ol Anbia Hospital, Tehran,, Biosensor Research Center, Endocrinology and Metabolism Molecular-Cellular Sciences Institute, Tehran University of Medical Sciences, Tehran,, Shefa Neuroscience Research Center, Khatam ol Anbia Hospital, Tehran
Keywords:Cathodic electrosynthesis, Fe3O4, magnetic properties, nanoparticles, polymer coating., Cathodic electrosynthesis, Fe3O4, magnetic properties, nanoparticles, polymer coating.
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.
