Phone: þ351 234 378 117, Fax: þ351 234 378 197Nanosized single-phase powders of the ferrimagnetic double perovskite Sr 2 FeMoO 6-d (SFMO) with various degrees of the superstructural ordering of the Fe 3þ and Mo 5þ cations have been synthesized by the citrate-gel method at pH ¼ 4, 6, 9 (samples SFMO 4,6,and 9). According to the results of the X-ray photoelectron spectroscopy, a mixed valence state of the iron and molybdenum cations is realized in the obtained SFMO powders, whereby the concentration of Fe 2þ increases and that of Fe 3þ decreases with increasing pH. The charge state of iron and the redistribution of the electron density in SFMO has been studied by means of the M€ ossbauer spectroscopy. The charge disproportionation for the powders obtained at pH ¼ 6 and 9 facilitates the segregation of a-Fe. The temperature dependences of the magnetization measured in the field cooling and zero-field cooling regimes indicate the existence of superparamagnetism in the nanosized grains of SFMO 4, 6, and 9 at T < 19 K. The superparamagnetism is metastable up to a temperature Т S . The applied magnetic field stimulates the transition in nanosized grains from the metastable superparamagnetic state into the stable one, above some value of the magnetic field induction exceeding the minimal anisotropy field.
57Fe M€ ossbauer spectra taken at 20 K of Sr 2 FeMoO 6-d prepared at pH ¼ 6.