401. Controlled Solid-State Synthesis of Mri Effective Superparamagnetic Maghemite Nanoparticles from Iron(II) Acetate
- Author
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Jiri Tucek, Jan Filip, Radek Zboril, Petr Paucek, Roman Kubinek, Katerina Polakova, and Jiri Pechousek
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Materials science ,Biophysics ,Analytical chemistry ,Maghemite ,engineering.material ,Amorphous solid ,chemistry.chemical_compound ,chemistry ,Phase (matter) ,Mössbauer spectroscopy ,engineering ,Iron oxide nanoparticles ,Superparamagnetism ,Magnetite ,Iron(II) acetate - Abstract
Thermally induced oxidative decomposition of iron(II) acetate in air is presented as a simple route towards superparamagnetic maghemite nanoparticles the size of which can be controlled by the reaction temperature in the range of 320-400°C. Decomposition mechanism, the phase composition of the reaction products as well as their structural, magnetic and surface properties were monitored by Mossbauer spectroscopy, XRD, TEM, magnetic and BET surface area measurements. Mossbauer spectra confirm maghemite (gamma-Fe2O3) as the only crystalline decomposition product without any traces of other Fe2O3 polymorphs or magnetite (Fe3O4). On the other hand, the amorphous phase was identified in all samples, which is manifested by the presence of the sextet component with significantly reduced hyperfine magnetic field in the low temperature and in-field Mossbauer spectra. Its content decreases with temperature of synthesis, in accordance with increasing saturation magnetization of the samples. The size of maghemite particles can be controlled by reaction temperature from 4-8 nm at 320 °C to 20-30 nm at 400 °C. This controlled growth is clearly observed by TEM and indirectly demonstrated by narrowing of XRD lines, decreasing surface area (from 147 to 51 m2/g) and increasing blocking and irreversibility temperatures in the FC-ZFC curves. The low intensities of the 2nd and 5th spectral lines in the in-field (5K/5T) Mossbauer spectrum of the sample prepared at 400 °C indicate a low degree of spin frustration of maghemite phase, while the amorphous admixture reveals speromagnetic behavior with unchanged intensities of spectral lines compared to the zero-field spectrum. The sample synthesized at 400 °C exhibits the MRI contrast properties fully comparable with the commercial agent Lumirem as proved by phantom experiments.Key words: Solid-state synthesis, Superaparamagnetic Iron Oxide Nanoparticles, MRI.
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