Rajeshwar Rai,
Anup Kumar Mishra,
Dhananjai Singh,
Rajnish Kumar Singh,
- Assistant Professor, Department of Chemistry, MIT Muzaffarpur, Department of Science, Technology and Technical Education, Bihar Engineering University, Patna, Bihar, India
- Assistant Professor, Department of Chemistry, M.I.T Muzaffarpur, Technology and Technical Education, Bihar Engineering University, Patna, Bihar, India
- Assistant Professor, Department of Chemistry, Nalanda College of Engineering, Chandi, Nalanda, Bihar, India
- Lecturer, Department of Chemistry, Government Polytechnic Chapra, DSTTE, Bihar, India
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 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: Fe₃O₄@γ-Fe₂O₃, chitosan, core/shell nanoparticles, magnetic nanocomposites, interfacial interaction, superparamagnetic-like response, XRD, thermal stability.
[This article belongs to Special Issue under section in Journal of Polymer & Composites (jopc)]
References
1. Laurent S, Forge D, Port M, Roch A, Robic C, Vander Elst L, et al. Magnetic iron oxide nanoparticles: Synthesis, stabilization, vectorization, physicochemical characterizations, and biological applications. Chem Rev. 2008;108(6):2064–2110.
2. Tartaj P, Morales MP, Veintemillas-Verdaguer S, González-Carreño T, Serna CJ. The preparation of magnetic nanoparticles for applications in biomedicine. J Phys D Appl Phys. 2003;36(13):R182–R197.
3. Gupta AK, Gupta M. Synthesis and surface engineering of iron oxide nanoparticles for biomedical applications. Biomaterials. 2005;26(18):3995–4021.
4. Ali A, Zafar H, Zia M, Ul Haq I, Phull AR, Ali JS, et al. Synthesis, characterization, applications, and challenges of iron oxide nanoparticles. Nanotechnol Sci Appl. 2016;9:49–67.
5. Cornell RM, Schwertmann U. The Iron Oxides: Structure, Properties, Reactions, Occurrences and Uses. 2nd ed. Weinheim: Wiley-VCH; 2003.
6. Chikazumi S. Physics of Ferromagnetism. 2nd ed. Oxford: Clarendon Press; 1997.
7. Nguyen MD, Tran HV, Xu S, Lee TR. Fe₃O₄ nanoparticles: Structures, synthesis, magnetic properties, surface functionalization, and emerging applications. Appl Sci. 2021;11(23):11301.
8. Dave PN, Kalaniya RY. Synthesis and magnetic properties of Fe₃O₄@γ-Fe₂O₃ core/shell nanoparticles. J Indian Chem Soc. 2012;89(6):853–856.
9. Massart R. Preparation of aqueous magnetic liquids in alkaline and acidic media. IEEE Trans Magn. 1981;17(2):1247–1248.
10. Kim DK, Zhang Y, Voit W, Rao KV, Muhammed M. Synthesis and characterization of surfactant-coated superparamagnetic monodispersed iron oxide nanoparticles. J Magn Magn Mater. 2001;225(1–2):30–36.
11. Dash M, Chiellini F, Ottenbrite RM, Chiellini E. Chitosan – A versatile semi-synthetic polymer in biomedical applications. Prog Polym Sci. 2011;36(8):981–1012.
12. Bhattarai N, Gunn J, Zhang M. Chitosan-based hydrogels for controlled, localized drug delivery. Adv Drug Deliv Rev. 2010;62(1):83–99.
13. Vaewbundit S, Siriphannon P. Soft solution in situ synthesis of chitosan/iron oxide nanocomposites and their magnetic properties. Soft Matter. 2021;17(25):6238–6247.
14. Soares PIP, Machado D, Laia C, Pereira LCJ, Coutinho JT, Ferreira IMM, et al. Thermal and magnetic properties of chitosan-iron oxide nanoparticles. Carbohydr Polym. 2016;149:382–390.
15. Kadam AA, Lee DS. Glutaraldehyde cross-linked magnetic chitosan nanocomposites: Reduction precipitation synthesis, characterization, and application for removal of hazardous textile dyes. Bioresour Technol. 2015;193:563–567.
16. Pospiskova K, Safarik I. Low-cost, easy-to-prepare magnetic chitosan microparticles for enzymes immobilization. Carbohydr Polym. 2013;96(2):545–548.
17. Bae KH, Park M, Do MJ, Lee N, Ryu JH, Kim GW, et al. Chitosan oligosaccharide-stabilized ferrimagnetic iron oxide nanocubes for magnetically modulated cancer hyperthermia. ACS Nano. 2012;6(6):5266–5273.
18. Singh N, Riyajuddin S, Ghosh K, Mehta SK, Dan A. Chitosan-graphene oxide hydrogels with embedded magnetic iron oxide nanoparticles for dye removal. ACS Appl Nano Mater. 2019;2(11):7379–7392.
19. Mistral J, Ve Koon KT, Cotica LF, Dias GS, Santos IA, Alcouffe P, et al. Chitosan-coated superparamagnetic Fe₃O₄ nanoparticles for magnetic resonance imaging, magnetic hyperthermia, and drug delivery. ACS Appl Nano Mater. 2024;7(7):7097–7110.
20. Hall BD, Zanchet D, Ugarte D. Estimating nanoparticle size from diffraction measurements. J Appl Crystallogr. 2000;33(6):1335–1341.
21. Wu Y, Wang Y, Luo G, Dai Y. In situ preparation of magnetic Fe₃O₄-chitosan nanoparticles for lipase immobilization by cross-linking and oxidation in aqueous solution. Bioresour Technol. 2009;100(14):3459–3464.

Journal of Polymer & Composites
| Volume | 14 | |
| Special Issue | 04 | |
| Received | 16/08/2026 | |
| Accepted | 08/09/2026 | |
| Published | 10/09/2026 | |
| Publication Time | 25 Days |
