The article describes the features of the synthesis of a new oxide pyrochlore Bi2.7Ni0.7Mg0.46Sb2O10+? (sp. gr. Fd-3m, a = 10.4703 ?) containing antimony (V) and bismuth (III) cations from a stoichiometric mixture of oxide precursors using a modified sol-gel method (method Pecini). It is shown that the formation of antimony (III, V) and bismuth (III) compounds that are volatile upon calcination can be prevented by dissolving the precursors in sulfuric or nitric acid solutions, and excluding the use of hydrochloric acid or chloride solutions. A step-by-step synthesis of two samples obtained from sulfuric and nitric acid media was carried out, and the phase composition of the preparations calcined in the temperature range of 350…950 ?C was analyzed. When calcining the sample obtained from the sulfuric acid solution, the Bi12.67O14(SO4)5 phase was revealed, which prevents the formation of pyrochlore in the low-temperature region. In the sample synthesized from the nitric acid solution, bismuth stibates Bi3SbO7, BiNbO4 are recorded as intermediate phases Sb2O4, Bi12MgO19, Bi7.47Ni0.53O11.73, Bi3Ni2/3Sb5/3O11, NiSb2O6 were identified as other intermediate phases in the samples. The synthesis temperature of single-phase Bi2.7Ni0.7Mg0.46Sb2O10+? with the pyrochlore structure is 950 ?С. The phase purity and chemical composition of the sample were established by X-ray phase analysis and energy-dispersive X-ray analysis.
Kristina N. Parshukova – bachelor of Chemistry Department, Syktyvkar State University, Syktyvkar, Russia
Ruslana A. Simpeleva – bachelor of Chemistry Department, Syktyvkar State University, Syktyvkar, Russia
Roman I. Korolev – senior lecturer, Department of Radiophysics and Electronics, Syktyvkar State University, Syktyvkar, Russia
Boris A. Makeev – Candidate of Geological-Mineralogical Sciences, researcher at the Laboratory of Mineralogy, Institute of geology FRC Komi SC UB RAS, Syktyvkar, Russia
Nadezhda A. Zhuk – Candidate of Chemical Sciences, Associate Professor, senior researcher of Laboratory of Ceramic Materials Science, Syktyvkar State University, Syktyvkar, Russia
1. Valant M., Babu G. S., Vrcon M., et al. Pyrochlore range from Bi2O3–Fe2O3–TeO3 system for LTCC and photocatalysis and the crystal structure of new Bi3(Fe0.56Te0.44)3O11 // J. Am. Ceram. Soc. 2011. V. 95. P. 644 – 650.
2. Murugesan S., Huda M. N., Yan Y., et al. Band-engineered bismuth titanate pyrochlores for visible light photocatalysis // J. Phys. Chem. C. 2010. V. 114. P. 10598 – 10605.
3. Giampaoli G., Siritanon T., Day B., et al. Temperature in-dependent low loss dielectrics based on quaternary pyrochlore oxides // Prog. Solid State Chem. 2018. V. 50. P. 16 – 23.
4. Zhuk N. A., Sekushin N. A., Krzhizhanovskaya M. G., et al. Сr-doped bismuth tantalate pyrochlore: electrical and thermal properties, crystal structure and ESR, NEXAFS, XPS spectroscopy // Mater. Res. Bull. 2023. V. 158. P. 112067.
5. Zhuk N. A., Makeev B. A., Krzhizhanovskaya M. G., et al. Features of the phase formation of Cr/Mn/Fe/Co/Ni/Cu codoped bismuth niobate pyrochlore // Crystals. 2023. V. 13. P. 1202.
6. Miles G. C., West A. R. Pyrochlore phases in the system ZnO–Bi2O3-Sb2O5: I. stoichiometries and phase equilibria // J. Am. Ceram. Soc. 2006. V. 89. P. 1042 – 1046.
7. Valant M., Suvorov D. The Bi2O3–Nb2O5–NiO phase diagram // J. Am. Ceram. Soc. 2005. V. 88. P. 2540 – 2543.
8. Subramanian M. A., Aravamudan G., Subba Rao G. V. Oxide pyrochlores – a review // Prog. Solid State Chem. 1983. V. 15. P. 55 – 143.
9. Jusoh F. A., Tan K. B., Zainal Z., et al. Novel pyrochlore-structured bismuth iron antimonates: Structural, impedance and electrochemical studies // Results in Physics. 2021. V. 27, No. 104542.
10. Egorysheva A. V., Ellert O. G., Gajtko O. M., et al.Complex dependence of magnetic properties on Mn concentration in Bi–Mn–Sb–O pyrochlores // J. Alloys Compd. 2017. V. 718. P. 311 – 318.
11. Egorysheva A. V., Gajtko O. M., Rudnev P. O., et al. Synthesis of Bi–Fe–Sb–O pyrochlore nanoparticles with visible-light photocatalytic activity // Eur. J. Inorg. Chem. 2016. V. 2016, No. 13–14. P. 2193 – 2199.
12. Egorysheva A. V., Ellert O. G., Zubavichus Y. V., et al. New complex bismuth oxides in the Bi2O3–NiO–Sb2O5 system and their properties // J. Sol. St. Chem. 2015. V. 225. P. 97 – 104.
13. Баданина К. А., Королев Р. И., Макеев Б. А., Жук Н. А. Синтез нанокристаллической керамики Bi2Cr0.5Co0.5Nb2O9+?. // Стекло и керамика. 2024. T. 97, № 8. С. 20 – 27.[Badanina K. A., Korolev R. I., Makeev B. A., Zhuk N. A. Synthesis of Bi2Cr0.5Co0.5Nb2O9+? nano-crystalline ceramics // Glass Ceram. 2024. V. 81. P. 315 – 320.]
14. Чиркова Д. С., Королев Р. И., Макеев Б. А., Жук Н. А. Синтез цинк- и марганецсодержащей пирохлороподобной керамики // Стекло и керамика. 2024. Т. 97, № 9. С. 20 – 27.[Chirkova D. S., Korolev R. I., Makeev B. A., Zhuk N. A. Synthesis of Zn and Mn Co-doped bismuth tantalate pyrochlore type ceramics // Glass Ceram. 2025. V. 81. P. 356 – 362.]
15. Муравьев В. A., Макеев Б. A., Кржижановская M. Г. и др. Cинтез Bi2NiTa2O9 со структурой типа пирохлора // Стекло и керамика. 2022. Т. 95, № 2. С. 40 – 46.[Murav’ev V. A., Makeev B. A., Krzhizhanovskaya M. G., et al. Synthesis of Bi2NiTa2O9 with pyrochlore structure // Glass Ceram. 2022. V. 79. P. 70 – 74.]
16. Akselrud L. G., Grin Yu. N., Zavalij P. Yu., et al. CSD-universal program package for single crystal or powder structure data treatment // Thes. Rep. XII Eur. Crystallogr. Meet. 1989. V.155.
17. Zhuk N. A., Badanina K. A., Korolev R. I., et al. Sol-gel derived Bi2NiNb2O9 pyrochlore: Synthesis, characterization and dielectric properties // Ceramics International. 2024. V. 50. No. 23. P. 50397 – 50409.
18. Zhuk N. A., Krzhizhanovskaya M. G., Sekushin N. A., et al. Novel Ni-doped bismuth–magnesium tantalate pyrochlores: structural and electrical properties, thermal expansion, X-ray photoelectron spectroscopy, and near-edge X-ray absorption fine structure spectra // ACS Omega. 2021. V. 6. P. 23262 – 23273.
The article can be purchased
electronic!
PDF format
700 руб
DOI: 10.14489/glc.2025.06.pp.032-040
Article type:
Research Article
Make a request
