Synthesis OF Bi1.5CoSb1.5O7 pyrochlore under hydrothermal conditions and its catalytic properties in the CO oxidation

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Abstract

The pyrochlore solid solution region in the Bi2O3–CoO–Sb2O5 system is determined. A previously unknown ternary oxide Bi3Co2/3Sb7/3O11 with cubic KSbO3 structure (sp. gr. Pn-3, a = 9.5801(1) Å, wR =0.0132) is found. An isothermal section of the system is constructed in the region of CoO-Bi3SbO7-CoSb2O6-BiSbO4 at 650°C. It is shown that cobalt state in pyrochlore crystal lattice is Co2+. For pyrochlore composition Bi1.5CoSb1.5O7, the synthetic methods under hydrothermal conditions of both without microwave-assisted treatment and with it have been developed. Based on the data of X-ray diffraction analysis, local energy-dispersive X-ray analysis, scanning microscopy and IR spectroscopy, a mechanism for the pyrochlore phase formation under hydrothermal condition is proposed. The dispersed Bi1.5CoSb1.5O7 samples (SCD = 30 nm) are synthesized and the prospects of their use as catalysts for CO oxidation are shown.

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About the authors

A. V. Egorysheva

Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences

Author for correspondence.
Email: anna_egorysheva@rambler.ru
Russian Federation, Moscow, 119991

S. V. Golodukhina

Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences

Email: anna_egorysheva@rambler.ru
Russian Federation, Moscow, 119991

E. Yu. Liberman

D.Mendeleev University of Chemical Technology of Russia

Email: anna_egorysheva@rambler.ru
Russian Federation, Moscow, 125047

L. S. Razvorotneva

Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences; National Research University Higher School of Economics

Email: anna_egorysheva@rambler.ru
Russian Federation, Moscow, 119991; Moscow, 101000

D. I. Kirdyankin

Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences

Email: anna_egorysheva@rambler.ru
Russian Federation, Moscow, 119991

E. F. Popova

Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences

Email: anna_egorysheva@rambler.ru
Russian Federation, Moscow, 119991

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Supplementary files

Supplementary Files
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2. Fig. 1. Isothermal cross section of Bi2O3-CoO-Sb2O5 system at temperature 650С. P-region of the solid solution with pyrochlore structure.

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3. Fig. 2. Dependence of the lattice parameter a of pyrochlore (Bi1.5-HCo0.5+x)Co0.5Sb1.5O7-δ on x.

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4. Fig. 3. Absorption spectrum of Bi1.5CoSb1.5O7.

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5. Fig. 4. Diffractograms of samples obtained under hydrothermal conditions at different synthesis times (a). Fragments of diffractograms at large angles 2θ (b).

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6. Fig. 5. Diffractograms of samples obtained at different NaOH concentrations (a). Fragments of diffractograms at large angles 2θ (b).

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7. Fig. 6. Microphotographs of samples obtained after co-precipitation (a) and hydrothermal treatment at 200С for 1 (b), 2 (c), 4 (d), 16 (e) and 24 h (f).

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8. Fig. 7. IR spectra of samples obtained at different synthesis times under hydrothermal conditions.

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9. Fig. 8. Diffractograms of Bi1.5CoSb1.5O7 samples synthesized in hydrothermal conditions under microwave exposure for different times (a). Microphotograph of the sample synthesized under hydrothermal-microwave conditions at 220С for 3 h (b).

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10. Fig. 9. Temperature dependence of CO conversion (α, %) in the presence of Bi1.5CoSb1.5O7 obtained by the hydrothermal method. Roman numerals indicate the cycle number.

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