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D. Đeorđić, M. Bošković, M. Perović, E. Illés

The presented experimental research focuses on obtaining iron oxide nanoparticles with high efficiency for magnetic hyperthermia treatments. They were prepared by two different synthesis methods. The first sample was prepared in the modified process of thermal decomposition of Fe precursor in a polyol solution. The second sample was prepared by coprecipitation based on mixing iron salts solution with NaOH solution. Samples were characterized by X-ray powder diffraction, SQUID measurements, transmission electron microscopy and Zetasizer Nano series. The results derived from two systems obtained by different synthesis methods represent valuable knowledge in the fundamental research on magnetic behavior of nanoparticle systems and also a significant contribution in the developing field of application of magnetic hyperthermia.

S. Krehula, M. Ristić, Ivana Mitar, Chuchu Wu, Xuning Li, Luhua Jiang, Junhu Wang, Gongquan Sun et al.

Ni-doped goethite (α-FeOOH) nanorods were synthesized from mixed Fe(III)-Ni(II) nitrate solutions with various Ni/(Ni+Fe) ratios (0, 5, 10, 20, 33 and 50 mol % Ni) by hydrothermal precipitation in a highly alkaline medium using the strong organic alkali, tetramethyl¬ammonium hydroxide (TMAH). Ni-doped hematite (α-Fe2O3) nanorods were obtained by calcination of Ni- doped goethite nanorods at 400 °C. The Ni2+- for-Fe3+ substitution in goethite and hematite was confirmed by determination of the unit cell expansion (due to the difference in the ionic radii of Fe3+ and Ni2+) using XRPD and determination of the reduction of a hyperfine magnetic field (due to the difference in magnetic moments of Fe3+ and Ni2+) using Mossbauer spectroscopy. Single- phase goethite nanorods were found in samples containing 0 or 5 mol % Ni. A higher Ni content in the precipitation system (10 mol % or more) resulted in a higher Ni2+-for-Fe3+ substitution in goethite, and larger Ni-doped goethite nanorods, though with the presence of low crystalline Ni-containing ferrihydrite and Ni ferrite (NiFe2O4) as additional phases. Significant changes in FT-IR and UV-Vis-NIR spectra of prepared samples were observed with increasing Ni content. Electrochemical measurements of samples showed a strong increase in oxygen evolution reaction (OER) electrocatalytic activity with increasing Ni content.

B. Antić, M. Bošković, J. Nikodinović-Runić, Y. Ming, Hongguo Zhang, E. Bozin, D. Janković, V. Spasojević et al.

Magnetic nanoparticles (MNPs) are of immense interest for diagnostic and therapeutic applications in medicine. Design and development of new iron oxide-based MNPs for such applications is of rather limited breadth without reliable and sensitive methods to determine their levels in body tissues. Commonly used methods, such as ICP, are quite problematic, due to the inability to decipher the origin of the detected iron, i.e. whether it originates from the MNPs or endogenous from tissues and bodily fluids. One of the approaches to overcome this problem and to increase reliability of tracing MNPs is to partially substitute iron ions in the MNPs with Er. Here, we report on the development of citric acid coated (Fe,Er)3O4 nanoparticles and characterization of their physico-chemical and biological properties by utilization of various complementary approaches. The synthesized MNPs had a narrow (6-7nm) size distribution, as consistently seen in atomic pair distribution function, transmission electron microscopy, and DC magnetization measurements. The particles were found to be superparamagnetic, with a pronounced maximum in measured zero-field cooled magnetization at around 90K. Reduction in saturation magnetization due to incorporation of 1.7% Er3+ into the Fe3O4 matrix was clearly observed. From the biological standpoint, citric acid coated (Fe,Er)3O4 NPs were found to induce low toxicity both in human cell fibroblasts and in zebrafish (Danio rerio) embryos. Biodistribution pattern of the MNPs after intravenous administration in healthy Wistar rats was followed by the radiotracer method, revealing that 90Y-labeled MNPs were predominantly found in liver (75.33% ID), followed by lungs (16.70% ID) and spleen (2.83% ID). Quantitative agreement with these observations was obtained by ICP-MS elemental analysis using Er as the detected tracer. Based on the favorable physical, chemical and biological characteristics, citric acid coated (Fe,Er)3O4 MNPs could be further considered for the potential application as a diagnostic and/or therapeutic agent. This work also demonstrates that combined application of these techniques is a promising tool for studies of pharmacokinetics of the new MNPs in complex biological systems.

M. Bošković, G. Goya, Sanja D. Vranješ-Djurić, N. Jović, B. Jaňcar, B. Antić

Herein we present the results of specific loss power (SLP) analysis of polydisperse water based ferrofluids, Fe3O4/PEG200 and Fe3O4/PEG6000, with average Fe3O4 particle size of 9 nm and 11 nm, respectively. Specific loss power was measured in alternating magnetic field of various amplitudes and at fixed frequency of 580.5 kHz. Maximum SLP values acquired were 195 W/g for Fe3O4/PEG200 and 60 W/g for Fe3O4/PEG6000 samples. The samples were labeled as superparamagnetic by magnetization measurements, but SLP field dependence showed deviation from the behavior predicted by the commonly employed linear response theory. The scope of this theory for both samples with wide particle size distribution is discussed. Deviation from the expected behavior is explained by referring to polydisperse nature of the samples and field dependent relaxation rates.

M. Vučinić-Vasić, M. Bošković, Aleksandar Antić, G. Stojanović, M. Radovanović, M. Fabián, Č. Jovalekić, M. Pavlovič et al.

Abstract Nickel ferrite nanoparticles were annealed in order to find dependence of electric/magnetic properties on crystallite size. The following correlations of crystallite size with physical parameters were found: (a) lattice parameter decreases with the increase in size and it reaches value for bulk counterpart approximately for crystallites bigger than 7 nm, (b) ac electrical resistivity at room temperature increases with the increase in crystallite size, (c) for crystallites of ~7 nm or smaller electrical resistivity have maximum value at 50 °C, (d) the real part of permittivity at selected frequency generally decreases with the increase in crystallite size and (e) magnetization increases with the increase in crystallite size. Deviation of stoichiometry, cation polyvalence, and cation redistribution with annealing are the main factors that influence physical properties of Nickel ferrite nanoparticles.

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