We studied the possibility of producing powder catalysts Al–Fe/SiO2 and Al–Co/SiO2 by mixing precursor powders of Al, Fe, Co, and SiO2 in a planetary mill in gross weight ratios corresponding to the domain of existence of intermetallic compounds Al3Fe and Al3Co and annealing in vacuum at 900°C for 30 min. Annealing in air at lower temperatures (580–600°С) leads to the formation of corundum Al2O3, mullite Al6Si2O13, and silicides CoSi2, CoSi, Co2Si, FeSi2, and Fe3Si in the composite structure. The synthesized composite powders 13Al/4Co/6.5SiO2 and 13Al/4Fe/6.5SiO2 contain nonequilibrium phases. Powders without sintered masses with good flow and a fractional composition of less than 100 μm are obtained after synthesis in vacuum at 900°C for 30 min. The fractional composition of powder Fe–Al/SiO2 is characterized by a distribution of less than 50 μm (27.1%), 50–63 μm (15.3%), and 63–100 μm (57.4%); the fractional composition of powder Co-Al/SiO2 is 37.5%, 16.2%, and 46.3%, respectively. According to X-ray phase analysis, the powders synthesized at 900°С contain the phases of Fe3Al, Fe0.5Al0.5, Fe14Al86, Co2Al5, and Co27Al73; they do not contain silicides and mullites of the type Al6Si2O13. It is experimentally established that the mass fractions of the precursors Al, Fe, and Co are (Al + Fe) : SiO2 = 31 : 69 and (Al + Co) : SiO2 = 58 : 42 as a result of cladding of powder SiO2. It is concluded that the vacuum annealing mode of 900°C for 30 min does not provide the formation of intermetallic structures of the type Al13Fe4/Al3Fe and Al13Co4/Al3Co during the synthesis. We suggest optimizing the synthesis mode by using precursors of finer fractions and increasing the time of their grinding, mixing, and annealing.
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We thank Dr. G.D. Nipan (Kurnakov Institute of General and Inorganic Chemistry of the Russian Academy of Sciences) for assistance in conducting a preliminary analysis of phase transformations in the systems Fe–Al/SiO2 and Co–Al/SiO2 at a temperature of 580–600°С in air. We also thank the employees of ISMAN for their active participation in the work.
This work was supported by the Presidium of the Russian Academy of Sciences (basic research program no. 33 “Carbon Energy: Chemical Aspects”) and by the Russian Academy of Sciences in the development of research topics of the state assignment (project no. 007-00129-18-00, 2018).
Translated by I. Obrezanova
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Artyukh, V.A., Borsch, V.N., Yusupov, V.S. et al. Peculiarities of a Solid-Phase Method for the Production of Al–Fe/SiO2 and Al–Co/SiO2 Powder Catalysts. Inorg. Mater. Appl. Res. 11, 709–712 (2020). https://doi.org/10.1134/S2075113320030041
- solid-phase synthesis
- mechanical alloying
- intermetallic compounds
- powder catalysts