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Contribution

X-ray structural analysis

Study of the reduction process of Co3O4 in supercritical isopropanol using In Situ SR XRD

Speakers

  • Dr. Alexander SHMAKOV

Primary authors

Co-authors

Content

Because of the development of chemical technology, the emergence of new materials and the improvement of engineering solutions, supercritical (SC) fluid technologies become more and more economically attractive for carrying out various chemical processes (extraction, separation, chemical reactions). Approaches using the SC state of the substance, allow the creation of unique functional materials that are difficult, and sometimes impossible to obtain using traditional approaches. It is known that isopropanol in the SC state (Tcrit = 235°C, Pcrit = 53 bar) allows the reduction of cobalt oxide (Co3O4) at temperatures lower than when hydrogen is used as a reducing agent [1]. Thus, it was shown by the ferromagnetic resonance method that this feature of the isopropanol SC avoids the high-temperature sintering of metal particles upon reduction and makes SK isopropanol a promising reducing agent for the preparation of dispersed metallic Co catalysts [2]. This work is dedicated to the studying of the reduction process of Co3O4 cobalt oxide by SK-isopropanol by In Situ Synchrotron Radiation X-ray diffraction (In Situ SR XRD). The experiment was carried out at Beamline No.8 of VEPP-4M storage ring. Since the sample is placed to glass capillary of 1 mm diameter with thick walls of about 0.1-0.15 mm the radiation of high energy is necessary to minimize radiation absorption. The SR XRD patterns were registered with Toshiba FDX4343R Flat Panel detector. Time resolution was 4 sec/frame.

  1. Gubin, S.P., Buslaeva, E.Y.: Supercritical isopropanol as a reducing agent for inorganic oxides. Russ. J. Phys. Chem. B. 3, 1172–1186 (2009). doi:10.1134/S1990793109080077
  2. Nesterov, N.S., Simentsova, I.I., Yudanov, V.F., Martyanov, O.N.: A comparative FMR study of the reduction of Co-containing catalysts for the Fischer–Tropsch process in hydrogen and supercritical isopropanol. J. Struct. Chem. 57, 90–96 (2016). doi:10.1134/S0022476616010108