Magnetite particles with an average size of 39 nm and good monodispersity have been synthesized by
coprecipitation at 70 °C from ferrous Fe2+ and ferric Fe3+ ions by a (N(CH3)4OH) solution, followed by
hydrothermal treatment at 250 °C. The magnetite nanoparticles before the hydrothermal step display an
average size of 12 nm and are highly oxidized when they are in contact with air. Complementary
microstructural and magnetic characterizations of nanoparticles after hydrothermal treatment show
unambiguously that they consist of magnetite with only a slight deviation from stoichiometry (δ ≈ 0.05),
leading to Fe2.95O4.
Magnetite nanoparticles of 40 nm in size have been phosphated in orthophosphoric acid. Large
phosphatation rates, equivalent to goethite capacity, have been pointed out, and the possibility of
phosphatation−dephosphatation cycles has been proved. Phosphatation occurs rapidly, inhibits the
dissolution of magnetite and does not modify the structure and the magnetization of magnetite. IR
spectroscopy, X-ray photoelectron spectroscopy (XPS) analysis, and Mössbauer spectrometry have shown
that phosphatation occurs by interaction with both positively charged groups and hydroxyl sites at the
surface of magnetite and more precisely with Fe3+ in octahedral sites. The main surface species would
be a protonated binuclear species and the top layer would be in the (111) plane. The chemical stability
of magnetite during cycling and its magnetic macroscopic moment allowing an easy recycling are promising
for technological uses.
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