ABSTRACT
High magnetization Fe3O4/OA-FeCo/Al2O3 nanocomposite magnetic clusters have been obtained using a modified oil-in-water miniemulsion method. These nanocomposite clusters dispersed in a ferrofluid carrier result in a magnetorheological fluid with improved characteristics. The magnetic clusters have a magnetic core consisting of a mixture of magnetite nanoparticles of about 6 nm average size, stabilized with oleic acid (Fe3O4/OA) and FeCo/Al2O3 particles of about 50 nm average size, compactly packed in the form of spherical clusters with a diameter distribution in the range 100-300 nm and a hydrophilic coating of sodium lauryl sulphate surfactant. The surface chemical composition of the Fe3O4/OA-FeCo/Al2O3 clusters investigated by XPS indicates the presence of the Co2+ and Co3+ oxidation states of cobalt and the components of Fe2+ and Fe3+ characteristic to both an enhanced oxidation state at the surface of the FeCo particles and to the presence of magnetic nanoparticles of spinel structure which are decorating the supporting FeCo. This specific decorating morphology is also indicated by TEM images. Advanced characterization of the Fe3O4/OA-FeCo/Al2O3 magnetic clusters has been performed using Mössbauer spectroscopy and magnetization measurements at various temperatures between 6 K and 200 K. The unexpected formation of Co ferrite decorating nanoparticles was supported by Mössbauer spectroscopy. The dispersion of magnetic clusters in the ferrofluid carrier highly influences the flow properties in the absence of the field (shear thinning for low and moderate shear rates) and especially in applied magnetic field, when significant magnetoviscous effect and shear thinning was observed for the whole range of shear rate values. Detailed analysis of the magnetorheological behavior of the nanocomposite magnetic clusters dispersed in a ferrofluid carrier evidence significantly higher normalized dynamic yield stress values in comparison with the magnetite nanocluster suspensions of the same mass concentration, a promising result for this new type of nanocomposite magnetorheological fluid.
ABSTRACT
Zn-Fe-O nanoparticle systems (Z3F, Z20F and Z60F) were produced by changing the Zn:Fe ratio (0.97 : 0.03, 0.8 : 0.2 and 0.4 : 0.6 in at%, respectively) in Zn(ii)-Fe(iii)-carboxylate precursors. According to X-ray diffraction, Z60F is nearly single-phase ZnFe2O4 (5.9 nm crystallite size), Z20F is a ZnO/ZnFe2O4 nanocomposite consisting of 48.8% ZnFe2O4 (4.7 nm crystallite size), and Z3F is apparently pure ZnO (9.5 nm). We found evidence for a ZnFe2O4 spinel of high inversion degree (80-100%) and with superparamagnetic (SPM) behaviour at room temperature in all three samples by a remarkable correlation between HRTEM, FTIR, XPS, Mössbauer and magnetization analyses. Iron modifies the decomposition process of the precursor and enhances its viscosity, which appears to favour the separation of Zn- and Fe-rich phases. As a consequence, two-phase systems of individual nanocrystals/nanoparticles (ZnO and ZnFe2O4) are formed. The large anisotropy constant, 106-107 erg cm-3, of the ZnFe2O4 nanoparticles and the concentration dependence of their magnetic energy barrier are explained in terms of interparticle interactions interlinked with finite size effects and high inversion degree; these factors also control the other parameters of importance for applications, including the blocking temperature (13-111 K), saturation magnetization (1.08-17.7 emu g-1 at 300 K, 4.6-44.8 emu g-1 at 5 K) and coercivity (85.4-491 Oe at 5 K). Magnetic dynamic results, particularly modelled by the Néel-Brown and Vogel-Fulcher laws, yield fitting parameters which validate the presence of concentration-dependent dipole-like interactions between ZnFe2O4 nanoparticles. A fraction of iron was found in the Fe2+ state, presumably substituting for Zn2+ in zinc oxide; however, the samples behave like ZnFe2O4 SPM nanoclusters/nanoparticles dispersed in a nonmagnetic ZnO particle assembly, rather than Zn(Fe)O dilute magnetic semiconductors. The relevance of the properties of the investigated material for specific applications is highlighted throughout the manuscript.
ABSTRACT
The aim of this paper is to present a reliable procedure for the experimental determination of the specific absorption rate (SAR) in case of superparamagnetic Fe oxide nanoparticles dispersed in liquid environments. It is based on the acquisition of consecutive steps of time-temperature dependences along of both heating and cooling processes. Linear fitting of these recorded steps provides the heating and cooling speeds at different temperatures, which finally allow the determination of the heating profile in adiabatic-like conditions over a broad temperature range. The presented methodology represents on one hand, a useful alternative tool for the experimental evaluation of the heating capability of nanoparticulate systems for magnetic hyperthermia applications and on the other hand, gives support for a more accurate modeling of bio-heat transfer phenomena.
