Journal of Materials Science

, Volume 27, Issue 6, pp 1617–1625 | Cite as

On the formation of M2+ -Sb3+ -alkoxide precursors and sol-gel processing of M-Sb oxides with M = Cr, Mn, Fe, Co, Ni, Cu and Zn

  • G. Westin
  • M. Nygren


Binary alkoxide complexes of compositions close to MSb(OEt)5, with M = Mn, Fe, Co and Ni, have been prepared and characterized by their i.r. and u.v.-VIS spectra, while Cr, Cu and Zn do not form similar ethoxide complexes with Sb(OEt)3. The Mn and Fe complexes must be prepared in inert atmosphere as they are very easily oxidized. The Fe complex is metastable and decomposes within a few hours. The Co complex can only be prepared in the presence of acetonitrile. X-ray amorphous gels were formed upon hydrolysis of solutions containing M to Sb species in the ratio 1∶2 for M = Mn, Fe, Co and Ni. The gels consisted of agglomerated particles of sizes from 75 to 300 nm. The decomposition of the gels in air and in nitrogen has been monitored by means of thermogravimetric measurements. Samples of heated gels were quenched from various temperatures in the region 50–950°C, and the formed oxides were characterized by their X-ray powder patterns and by their infrared spectra. At 950 °C MSb2O6 was formed in air, while in nitrogen MSb2O4 (M = Mn, Co and Ni) was formed at intermediate temperatures. At higher temperatures the latter compound decomposed and Sb2O3 sublimated.


Acetonitrile Infrared Spectrum Alkoxide Inert Atmosphere Formed Oxide 
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  1. 1.
    US Patent 2 839 554, (1958).Google Scholar
  2. 2.
    M. H. Abraham, J. Chem. Soc. (1960) 4130.Google Scholar
  3. 3.
    C. H. Brubaker Jr. and M. Wicholas, J. Inorg. Nucl. Chem.27 (1965) 59.CrossRefGoogle Scholar
  4. 4.
    G. E. Binder, U. Ensinger, W. Dorsch and A. Schmidt, Z. Anorg. Chem.507 (1983) 163.CrossRefGoogle Scholar
  5. 5.
    B. Horvath, R. Mösler and E. G. Horvath, Z. Anorg. Allg. Chem.449 (1979) 41.CrossRefGoogle Scholar
  6. 6.
    J. R. Gavarri, G. Calvarin and B. Chadron, J. Solid State Chem.47 (1983) 132.CrossRefGoogle Scholar
  7. 7.
    X. M. Turrilas, H. Vincent and I. Rasines, Rev. Chem. Min.22 (1985) 625.Google Scholar
  8. 8.
    D. Smith, JCPDS Grant in Aid Report JCPDS-PDS-2, 25-1181 (1973).Google Scholar
  9. 9.
    Mason and Vialiano, Min. Mag.30 (1953) 108.Google Scholar
  10. 10.
    S. Stål, Arkiv Kemimin. Geol.17B (1943) 1.Google Scholar
  11. 11.
    National Bureau of Standards Monograph No. 25 (NBS, 1967) p. 26.Google Scholar
  12. 12.
    B. P. Baranwal and R. C. Mehrotra, Aust. J. Chem.33 (1980) 37.CrossRefGoogle Scholar
  13. 13.
    R. C. Mehrotra and J. Singh, Can. J. Chem.62 (1984) 1003.CrossRefGoogle Scholar
  14. 14.
    R. Jain, A. K. Rai and R. C. Mehrotra, Z. Naturforsch.40B (1985) 1371.CrossRefGoogle Scholar
  15. 15.
    J. R. Gavarri and A. W. Hewat, J. Solid State Chem.49 (1983) 14.CrossRefGoogle Scholar
  16. 16.
    R. Chater, J. R. Gavarri and F. Genet, ibid.63 (1986) 295.CrossRefGoogle Scholar
  17. 17.
    F. Larson and G. McCarthy, JCPDS Grant in Aid Report JCPDS-PDS-2, 38-1083 (1986).Google Scholar
  18. 18.
    E. Husson, Y. Repelin, H. Brusset and A. Cerez, Spectrochem. Acta35A (1979) 1177.CrossRefGoogle Scholar

Copyright information

© Chapman & Hall 1992

Authors and Affiliations

  • G. Westin
    • 1
  • M. Nygren
    • 1
  1. 1.Department of Inorganic Chemistry, Arrhenius LaboratoryUniversity of StockholmStockholmSweden

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