Gadolinium orthoferrite (GdFeO 3) seems to have potential as a dual-modal contrast agent for magnetic resonance imaging (MRI), thus its preparation in the form of ultrafine superparamagnetic nanoparticles is currently of great interest. In this work, nanocrystalline GdFeO 3 was successfully synthesized by the heat treatment (750 • C, 4 h) of gadolinium and iron(III) hydroxides reversely co-precipitated at low temperature (0 • C). Initial and resulting powders were analyzed by EDX, SEM, PXRD, Mössbauer spectroscopy, vibration magnetometry, etc. Gadolinium orthoferrite was formed as isometric nanocrystals with an average size of 23±3 nm, which were strongly agglomerated into clusters of about 200 nm in diameter. It was shown that the individual GdFeO 3 nanocrystals are superparamagnetic, but in the cluster form, they exhibit a collective weak ferromagnetic behavior. After ultrasonic-assisted disintegration of GdFeO 3 to a colloidal solution form, these clusters remained stable due to their strong agglomeration and low zeta potential value of 1 mV. Thus, it is concluded that the further use of the synthesized GdFeO 3 nanoparticles as a basis of MRI contrast agents will be possible only after the suppression of their clustering.

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Nanocrystals of gadolinium orthoferrite (GdFeO3) with morphology close to isometric and superparamagnetic behavior were successfully synthesized using direct, reverse and microreactor co-precipitation of gadolinium and iron(III) hydroxides with their subsequent heat treatment in the air. The obtained samples were investigated by PXRD, FTIR, low-temperature nitrogen adsorption-desorption measurements, HRTEM, SAED, DRS and vibration magnetometry. According to the X-ray diffraction patterns, the GdFeO3 nanocrystals obtained using direct co-precipitation have the smallest average size, while the GdFeO3 nanocrystals obtained using reverse and microreactor co-precipitation have approximately the same average size. It was shown that the characteristic particle size values are much larger than the corresponding values of the average crystallite size, which indicates the aggregation of the obtained GdFeO3 nanocrystals. The GdFeO3 nanocrystals obtained using direct co-precipitation aggregate more than the GdFeO3 nanocrystals obtained using reverse co-precipitation, which, in turn, tend to aggregate more strongly than the GdFeO3 nanocrystals obtained using microreactor co-precipitation. The bandgap of the obtained GdFeO3 nanocrystals decreases with decreasing crystallite size, which is apparently due to their aggregation. The colloidal solutions of the obtained GdFeO3 nanocrystals with different concentrations were investigated by 1H NMR to measure the T1 and T2 relaxation times. Based on the obtained r2/r1 ratios, the GdFeO3 nanocrystals obtained using microreactor, direct and reverse co-precipitation may be classified as T1, T2 and T1–T2 dual-modal MRI contrast agents, respectively.