Abstract
In this study, we developed a convenient one-pot method with sodium oleate as both the surfactant and precipitant to synthesize pure magnetite nanoparticles in the water/ethanol/toluene system. The initial molar ratio of [Fe3+]/[Fe2+] and the concentration of iron salts were changed in order to systematically investigate their influences on the chemical and physical properties of nanoparticles, such as the crystal structure, morphology, particle sizes, dispersion and magnetism. Samples were determined by XRD, XPS, FTIR, DLS, and VSM. The oleate coating steadily existed on the surface of the nanoparticles to profit them of excellent monodispersibility and stability in non-polar solvents with very narrow size distribution and extremely approximate mean diameters of ~7 nm. Particles consisted mainly of magnetite with a little or no maghemite phase with the molar ratio of [Fe3+]/[Fe2+] decreasing from 2:1 to 1:1, but they all exhibited superparamagnetism at room temperature. After the optimization, pure magnetite nanoparticles could be prepared with the saturation magnetization successfully increasing to 75 emu/g(Fe), when the molar ratio of [Fe3+]/[Fe2+] was 1.5:1 and the concentration of iron precursors was 95 mM.
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Arruebo M, Fernandez-Pacheco R, Ibarra MR, Santamaria J (2007) Magnetic nanoparticles for drug delivery. Nano Today 2(3):22–32. doi:10.1016/S1748-0132(07)70084-1
Blinov AV, Ramazanova AG, Korolev VV (2002) Heats of adsorption of sodium oleate from aqueous solutions on the surface of magnetite. Russ J Phys Chem 76(5):806–808
Bronstein LM, Huang XL, Retrum J, Schmucker A, Pink M, Stein BD, Dragnea B (2007) Influence of iron oleate complex structure on iron oxide nanoparticle formation. Chem Mater 19(15):3624–3632. doi:10.1021/cm062948j
Buzea C, Pacheco II, Robbie K (2007) Nanomaterials and nanoparticles: sources and toxicity. Biointerphases 2(4):MR17–MR71
Chandrappa KG, Venkatesha TV, Vathsala K, Shivakumara C (2010) A hybrid electrochemical-thermal method for the preparation of large ZnO nanoparticles. J Nanopart Res 12(7):2667–2678
De Palma R, Peeters S, Van Bael MJ, Van den Rul H, Bonroy K, Laureyn W, Mullens J, Borghs G, Maes G (2007) Silane ligand exchange to make hydrophobic superparamagnetic nanoparticles water-dispersible. Chem Mater 19(7):1821–1831. doi:10.1021/Cm0628000
Fan QL, Neoh KG, Kang ET, Shuter B, Wang SC (2007) Solvent-free atom transfer radical polymerization for the preparation of poly(poly(ethyleneglycol) monomethacrylate)-grafted Fe3O4 nanoparticles: synthesis, characterization and cellular uptake. Biomaterials 28(36):5426–5436. doi:10.1016/j.biomaterials.2007.08.039
Gupta AK, Gupta M (2005) Synthesis and surface engineering of iron oxide nanoparticles for biomedical applications. Biomaterials 26(18):3995–4021. doi:10.1016/j.biomaterials.2004.10.012
Jeong U, Teng XW, Wang Y, Yang H, Xia YN (2007) Superparamagnetic colloids: controlled synthesis and niche applications. Adv Mater 19(1):33–60. doi:10.1002/adma.200600674
Jiang W, Wu Y, He B, Zeng XB, Lai KL, Gu ZW (2010) Effect of sodium oleate as a buffer on the synthesis of superparamagnetic magnetite colloids. J Colloid Interface Sci 347(1):1–7. doi:10.1016/j.jcis.2010.02.055
Jun YW, Seo JW, Cheon A (2008) Nanoscaling laws of magnetic nanoparticles and their applicabilities in biomedical sciences. Acc Chem Res 41(2):179–189. doi:10.1021/ar700121f
Kim DK, Zhang Y, Voit W, Rao KV, Muhammed M (2001) Synthesis and characterization of surfactant-coated superparamagnetic monodispersed iron oxide nanoparticles. J Magn Magn Mater 225(1–2):30–36. doi:10.1016/S0304-8853(00)01224-5
Laurent S, Forge D, Port M, Roch A, Robic C, Elst LV, Muller RN (2008) Magnetic iron oxide nanoparticles: synthesis, stabilization, vectorization, physicochemical characterizations, and biological applications. Chem Rev 108(6):2064–2110. doi:10.1021/Cr068445e
Liu XQ, Kaminski MD, Guan YP, Chen HT, Liu HZ, Rosengart AJ (2006) Preparation and characterization of hydrophobic superparamagnetic magnetite gel. J Magn Magn Mater 306(2):248–253. doi:10.1016/j.jmmm.2006.03.049
Maity D, Agrawal DC (2007) Synthesis of iron oxide nanoparticles under oxidizing environment and their stabilization in aqueous and non-aqueous media. J Magn Magn Mater 308(1):46–55. doi:10.1016/j.jmmm.2006.05.001
Mialon G, Gohin M, Gacoin T, Boilot JP (2008) High temperature strategy for oxide nanoparticle synthesis. Acs Nano 2(12):2505–2512. doi:10.1021/Nn8005784
Mikhaylova M, Kim DK, Bobrysheva N, Osmolowsky M, Semenov V, Tsakalakos T, Muhammed M (2004) Superparamagnetism of magnetite nanoparticles: Dependence on surface modification. Langmuir 20(6):2472–2477. doi:10.1021/La035648e
Namduri H, Nasrazadani S (2008) Quantitative analysis of iron oxides using Fourier transform infrared spectrophotometry. Corros Sci 50(9):2493–2497. doi:10.1016/j.corsci.2008.06.034
Prakash R, Choudhary RJ, Chandra LSS, Lakshmi N, Phase DM (2007) Electrical and magnetic transport properties of Fe3O4 thin films on a GaAs(100) substrate. J Phys Condens Mater 19: 486212. doi:10.1088/0953-8984/19/48/486212
Ruby C, Humbert B, Fusy J (2000) Surface and interface properties of epitaxial iron oxide thin films deposited on MgO(001) studied by XPS and Raman spectroscopy. Surf Interface Anal 29(6):377–380. doi:10.1002/1096-9918(200006)
Salazar JS, Perez L, de Abril O, Lai TP, Ihiawakrim D, Vazquez M, Greneche JM, Begin-Colin S, Pourroy G (2011) Magnetic iron oxide nanoparticles in 10–40 nm range: composition in terms of magnetite/maghemite ratio and effect on the magnetic properties. Chem Mater 23(6):1379–1386
Sun SH, Zeng H, Robinson DB, Raoux S, Rice PM, Wang SX, Li GX (2004) Monodisperse MFe2O4 (M = Fe, Co, Mn) nanoparticles. J Am Chem Soc 126(1):273–279. doi:10.1021/Ja0380852
Teng XW, Yang H (2004) Effects of surfactants and synthetic conditions on the sizes and self-assembly of monodisperse iron oxide nanoparticles. J Mater Chem 14(4):774–779. doi:10.1039/B311610g
Vidal–Vidal J, Rivas J, Lopez-Quintela MA (2006) Synthesis of monodisperse maghemite nanoparticles by the microemulsion method. Colloid Surface A 288(1–3):44–51. doi:10.1016/j.colsurfa.2006.04.027
Wang X, Zhuang J, Peng Q, Li YD (2005) A general strategy for nanocrystal synthesis. Nature 437(7055):121–124. doi:10.1038/Nature03968
Wen XT, Yang JX, He B, Gu ZW (2008) Preparation of monodisperse magnetite nanoparticles under mild conditions. Curr Appl Phys 8(5):535–541. doi:10.1016/j.cap.2007.09.003
Woo K, Hong J, Choi S, Lee HW, Ahn JP, Kim CS, Lee SW (2004) Easy synthesis and magnetic properties of iron oxide nanoparticles. Chem Mater 16(14):2814–2818. doi:10.1021/Cm049552x
Wu SYH, Tseng CL, Lin FH (2010) A newly developed Fe-doped calcium sulfide nanoparticles with magnetic property for cancer hyperthermia. J Nanopart Res 12(4):1173–1185
Xu CJ, Sun SH (2009) Superparamagnetic nanoparticles as targeted probes for diagnostic and therapeutic applications. Dalton Trans 29:5583–5591. doi:10.1039/B900272n
Yamashita T, Hayes P (2008) Analysis of XPS spectra of Fe2+ and Fe3+ ions in oxide materials. Appl Surf Sci 254(8):2441–2449. doi:10.1016/j.apsusc.2007.09.063
Zhang L, He R, Gu HC (2006) Oleic acid coating on the monodisperse magnetite nanoparticles. Appl Surf Sci 253(5):2611–2617. doi:10.1016/j.apsusc.2006.05.023
Zhou HF, Yi R, Li JH, Su Y, Liu XH (2010) Microwave-assisted synthesis and characterization of hexagonal Fe3O4 nanoplates. Solid State Sci 12(1):99–104. doi:10.1016/j.solidstatesciences.2009.10.012
Acknowledgments
The authors would like to thank National Basic Research Program of China (National 973 program, No. 2011CB606206), the National Natural Science Foundation of China (31070849, 50830105), the Department of Science and Technology of Sichuan Province (2009HH0001, 2009SZ0137) and the Ministry of Science and Technology (2010DFA51550).
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Jiang, W., Lai, KL., Hu, H. et al. The effect of [Fe3+]/[Fe2+] molar ratio and iron salts concentration on the properties of superparamagnetic iron oxide nanoparticles in the water/ethanol/toluene system. J Nanopart Res 13, 5135–5145 (2011). https://doi.org/10.1007/s11051-011-0495-8
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DOI: https://doi.org/10.1007/s11051-011-0495-8