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Journal of Polymer & Composites Original Research

Fabrication, Interfacial Characterization, and Superparamagnetic Properties of Fe₃O₄@γ-Fe₂O₃ Core/Shell Nanoparticle-Reinforced Chitosan Biopolymer Composites

  1. Rajeshwar Rai Department of Chemistry, MIT Muzaffarpur, Department of Science, Technology and Technical Education, Bihar Engineering University, Patna
  2. Anup Kumar Mishra M.I.T Muzaffarpur, Department of Science, Technology and Technical Education, Bihar Engineering University, Patna
  3. Dhananjai Singh Department of Chemistry, Nalanda College of Engineering, Chandi, Nalanda
  4. Rajnish Kumar Singh Department of Chemistry, Government Polytechnic Chapra, DSTTE

Abstract

Magnetite/maghemite core/shell nanoparticles were prepared by alkaline co-precipitation of Fe(II) and Fe(III) precursors followed by controlled thermal oxidation at 350 °C and subsequently incorporated into chitosan at 1, 3, and 5 wt% loadings by solution casting. The resulting films were evaluated by X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), high-resolution transmission electron microscopy (HR-TEM), vibrating-sample magnetometry (VSM), thermogravimetric analysis (TGA), and tensile testing. XRD showed the characteristic cubic spinel reflections at 2θ ≈ 30.15°, 35.48°, 43.12°, 53.45°, 57.02°, and 62.61°, with an apparent crystallite size of approximately 13.8 nm and a lattice parameter of 0.8362 nm. HR-TEM showed approximately spherical particles in the 12-16 nm range; contrast analysis gave a magnetite-rich inner region of about 9.5 nm and an oxidized outer region of about 2.2 nm, yielding an overall dimension consistent with the XRD-derived size. FT-IR bands shifted from approximately 3420 to 3385 cm⁻¹ and from 1592 to 1585 cm⁻¹ after filler incorporation, while an Fe-O vibration appeared near 582 cm⁻¹, supporting interfacial interaction between chitosan functional groups and the iron-oxide surface. At 300 K, the composite films displayed negligible remanence and coercivity under the reported measurement conditions, consistent with a highly reversible superparamagnetic-like response. The 5 wt% film exhibited the strongest combined property enhancement: tensile strength increased from 32.4 to 53.1 MPa (≈64%), Young's modulus from 1.15 to 2.38 GPa, and the reported TGA degradation onset from 225 to 258 °C. These results support the use of low-loading Fe₃O₄@γ-Fe₂O₃/chitosan films as magnetically responsive, mechanically reinforced biopolymer composites for separation, adsorption, sensing, and related functional-material applications.

Keywords

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