Synthesis of nanosized phases with a garnet structure using supercritical СО2 fluid

Solid State Sciences. 2024. Vol. 157 . Article 107710.

Kolobanov A. I., Fomichev V. V., Sigov A. S., Kumskov A. S., Ionov A. M., Mozhchil R. N.

A method was developed for the production of nanosized complex oxides and oxysulfides. The first stage uses supercritical СО2 fluid (SAS – supercritical antisolvent method). This approach makes it possible to obtain precursor-free complex oxides in a narrow nanoscale range. Nanosized rare-earth iron garnets with the general formula R3Fe5O12, where R is a rare earth element, were obtained and studied by physicochemical methods. The resulting samples have a size of less than 100 nm, exhibit ferromagnetic ordering, and can be used as soft magnetic materials. The multi-stage method for the preparation of complex oxysulfides was not previously demonstrated anywhere in the literature. The method involves three stages. At the first stage, a nanosized X-ray amorphous solid solution of the original salts is obtained using the SAS method. Then a nanosized X-ray amorphous component – the oxide phase – is obtained by annealing in a furnace. After this, the resulting oxide phase is mixed with the disulfide of a transition element (Nb, Mo), and high-temperature annealing is performed in an evacuated quartz ampoule. As a result, compact and nanosized phases of the composition Eu3Fe5-3/ 2xMox□1/2xO12-2xS2x and Eu3Fe5-3/2xNbx□1/2xO12-2xS2x, where x = 0.15, were obtained for the first time. The introduction of the sulfide component, namely NbS2, into the garnet structure increases its magnetic parameters by the factor of 1.5.

Keywords: наноматериалы, Supercritical fluid, Nanomaterials, Complex oxysulfides, сверхкритическая жидкость, сложные оксисульфиды