Magnetic nanoparticles are becoming increasingly important for several biomedical applications. For example, superparamagnetic magnetite nanoparticles with suitable bio-compatible coatings are useful in magnetic resonance imaging, tissue engineering, and drug delivery, etc. In this study we report the synthesis of magnetite nanoparticles and the further coating of these particles by several types of protective layers. Thermodynamic modeling of the chemical system has been adopted as a rational approach to establish routes to better synthesis conditions for pure phase magnetite. Quantitative analysis of different reaction equilibria involved in the precipitation of magnetite from aqueous solutions has been used to determine optimum synthesis conditions. Superparamagnetic magnetite nanoparticles (SPION) with diameters of 6 and 12 nm have been prepared by controlled chemical coprecipitation of magnetite phase from aqueous solutions containing suitable salts of Fe2+ and Fe3+ under inert atmosphere. Pure magnetite phase SPION could be observed from X-ray diffraction. Magnetic colloid suspensions containing particles with three different types of coatings (sodium oleate (NaOl), starch, and methoxypoly(ethylene glycol) (MPEG)) have been prepared by using different stabilization methods. SPION coatings were studied by determining the change of the surface charge by electrokinetic sonic amplitude (ESA) measurements, as a function of varying NaOl in the solution, where the amount of NaOl needed to form a stable suspension was determined. For stable suspension, the optimum concentration of sodium oleate (NaOl) chemisorbed at 2.5 g of SPION surface is 5.2 × 10-7 M NaOl which shows maximum ESA value of 0.034 mPa·M/V. SPION coating by starch results in the formation of agglomerate. The agglomeration size of starch-coated SPION can be decreased by introducing H2O2 as an oxidizing agent; the resulting particle size is 42 nm as determined by dynamic light scattering (DLS). For the modification of SPION surfaces with MPEG, the surface was first silanized by 3-aminopropyltrimethoxy silane (APTMS) as a coupling agent with a thickness of two or three molecular layers. AFM image shows that each cluster includes several magnetite single particles with the cluster size around 120 nm. SPION, both coated and uncoated, have been characterized by several techniques. AFM was used to image the MPEG-coated SPION. FTIR study indicated that the different coating agents cover the SPION surface. Magnetic characterization was carried out using SQUID and Mössbauer spectroscopy.
Superparamagnetic iron oxide nanoparticles (SPION) with an average particle diameter of 6 nm are prepared by controlled chemical coprecipitations. Colloidal suspensions of noninteracting SPION, where the surface has been modified with three different types of biocompatible substances, namely, starch, gold (Au), and methoxypoly(ethylene glycol) (MPEG) have been fabricated via three different techniques. Starch-coated SPION are prepared by coprecipitation in a polymeric matrix, Au-coated SPION are fabricated by the microemulsion method, and MPEG-coated SPION are prepared using the self-assembly approach. The magnetic nanoparticles form a core-shell structure, and the magnetic dipole-dipole interactions are screened by a layer of coating agents. The amounts of coating agents and SPION are indirectly calculated from the thermogravimetric analysis and superconducting quantum interference device measurements by assuming passive oxidation on the surface of the SPION, and the other conditions do not influence the measurements. The dependency of the spectral characteristics of Mössbauer spectroscopy as a function of an external magnetic field Hext is measured to investigate the effect of dipole-dipole screening of the different coating layers on the SPION. Uncoated SPION show a stable magnetic moment under Hext, and the superparamagnetic (SPM) fraction transforms to a ferrimagnetic state. Starch and Au-coated SPION retain the SPM fraction according to Mössbauer spectroscopy and magnetization measurements. MPEG-coated SPION show hyperfine magnetic structure without the quadrupole effect with increasing the value of the blocking temperature.
The magnetic properties of maghemite (gamma-Fe2O3) cubic and spherical nanoparticles of similar sizes have been experimentally and theoretically studied. The blocking temperature, T(B), of the nanoparticles depends on their shape, with the spherical ones exhibiting larger T(B). Other low temperature properties such as saturation magnetization, coercivity, loop shift or spin canting are rather similar. The experimental effective anisotropy and the Monte Carlo simulations indicate that the different random surface anisotropy of the two morphologies combined with the low magnetocrystalline anisotropy of gamma-Fe2O3 is the origin of these effects.
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