View PDF Version
 
DOI: 10.1039/A605665B (Paper) Reference Section for: J. Chem. Soc., Dalton Trans., 1997, 231-236

Convenient, room-temperature liquid ammonia routes to metal chalcogenides[hair space]

(Note: The full text of this document is currently only available in the PDF Version )

Geoff Henshaw, Ivan P. Parkin and Graham A. Shaw

Abstract

Reaction of sulfur, selenium or tellurium with elemental metals in liquid ammonia at room temperature in a pressure vessel produced metal chalcogenides ME (M = Ca, Sr, Ba, Eu, Yb, Ni, Zn, Cd, Hg, Sn or Pb; E = S, Se or Te), Ag2E, solid solutions of mixed-metal chalcogenides MxM′yEz (x + y = 1, z = 1 or 2), and metal-mixed chalcogenides MSxSey. Products showed a range of crystallite sizes from 700 Å for PbSe and Ag2S to essentially amorphous (ZnS). Heating at 250–300 °C under vacuum for 2 h induced crystallinity in the amorphous powders. The pre- and post-heated metal chalcogenides were analysed by X-ray powder diffraction, Fourier-transform IR, Raman microscopy, scanning electron microscopy-energy dispersive analysis of X-rays, electron microprobe, X-ray photoelectron spectroscopy, elemental analysis and magnetic susceptibility studies.

References

  1. W. L. Jolly and C. J. Mallada, in Non Aqueous Solvent Systems, Academic Press, London, ch. 1, p. 1 Search PubMed.
  2. W. L. Jolly, Prog. Inorg. Chem., 1959, 1, 235 CAS.
  3. Metal Ammonia Solutions, Proceedings of the International Conference on the Nature of Metal Ammonia Solutions, Colloque Wey III, Ithaca, New York (1969), Butterworths, London, 1970 Search PubMed.
  4. M. R. C. Symons, Chem. Soc. Rev., 1976, 5, 337 RSC.
  5. P. Dubois, J. P. Lelieur and G. Lepourte, Inorg. Chem., 1988, 27, 73 CrossRef CAS; Inorg. Chem., 1989, 28, 195 Search PubMed.
  6. P. Belton, I. P. Parkin and J. D. Woollins, J. Chem. Soc., Dalton Trans., 1989, 511 RSC.
  7. D. G. Oei, Inorg. Chem., 1973, 12, 438 CrossRef CAS.
  8. A. Cisar and J. D. Corbett, Inorg. Chem., 1977, 16, 632 CrossRef CAS.
  9. H. Schafer, B. Eisenmann and W. Muller, Angew. Chem., Int. Ed. Engl., 1973, 12, 694 CrossRef.
  10. R. Coustal, J. Chim. Phys., 1958, 38, 277 Search PubMed.
  11. Y. M. Gao, P. Wu, J. Baglio, K. M. Dwight and A. Wold, Mater. Res. Bull., 1989, 24, 1215 CrossRef CAS.
  12. D. M. P. Mingos and D. R. Baghurst, Chem. Soc. Rev., 1991, 20, 1 RSC.
  13. H. C. Metcalf, J. E. Williams and J. F. Caskta, Modern Chemistry, Holt, Reinhart, Winston, New York, 1982, p. 54 Search PubMed.
  14. D. M. Wilhelmy and E. Matijevic, J. Chem. Soc., Faraday Trans., 1984, 563 RSC.
  15. C. E. Johnson, D. K. Hickey and D. C. Harris, Mater. Res. Soc. Symp. Proc., 1986, 73, 685; D. M. Frigo, O. F. Z. Khan and P. O'Brien, J. Cryst. Growth, 1989, 96, 989 CrossRef CAS; T. Trindade, J. D. De Jesus and P. O'Brien, J. Mater. Chem., 1994, 4, 1611 RSC; J. G. Brennan, T. Seigrist, P. J. Carroll, S. M. Stuczynski, P. Reynders, L. E. Brus and M. L. Steigerwald, Chem. Mater., 1990, 2, 403 CrossRef CAS; G. Krauter and W. S. Rees, J. Mater. Chem., 1995, 5, 1265 RSC.
  16. N. L. Pickett, D. F. Foster and D. J. Cole Hamilton, J. Mater. Chem., 1996, 6, 507 RSC.
  17. H. C. Yi and J. J. Moore, J. Mater. Sci., 1990, 25, 1159 CAS.
  18. I. P. Parkin, Chem. Soc. Rev., 1996, 25, 199 RSC.
  19. S. Dev, E. Ramli, T. B. Rauchfuss and S. R. Wilson, Inorg. Chem., 1991, 30, 2514 CrossRef CAS; P. P. Paul, T. B. Rauchfuss and S. R. Wilson, J. Am. Chem. Soc., 1993, 115, 3316 CrossRef CAS; E. Ramli, T. B. Rauchfuss and C. L. Stern, J. Am. Chem. Soc., 1990, 112, 4043 CrossRef CAS.
  20. H. Grijavala, M. Inoue, S. Buggavarapu and P. Calvert, J. Mater. Chem., 1996, 7, 1157 RSC.
  21. G. Henshaw, I. P. Parkin and G. Shaw, Chem. Commun., 1996, 1095 RSC.
  22. PDF-2 database on CD-ROM, International Centre for Diffraction Data, Swarthmore, PA, 1990.
  23. H. P. Klug and L. E. Alexander, X-Ray Diffraction Procedure for Polycrystalline and Amorphous Materials, 2nd edn., Wiley, New York, 1974 Search PubMed.
  24. K. Nakamoto, Infrared and Raman Spectra of Inorganic and Coordination Compounds, 3rd edn., Wiley, Chichester, 1978 Search PubMed.
  25. C. D. Wagner, in Practical Surface Analysis, 2nd edn., eds. D. Briggs and M. Peah, Wiley, Chichester, 1990, vol. 1 Search PubMed.
  26. I. P. Parkin and G. Shaw, Main Group Metal Chem., 1996, 19, 499 Search PubMed.
  27. CRC Rubber Handbook of Chemistry and Physics, 40th edn., eds. C. D. Hodgman, R. C. West and S. M. Selby, CRC Press, Boca Raton, FL, 1959, p. 647 Search PubMed.
  28. J. C. Fitzmaurice and I. P. Parkin, Polyhedron, 1993, 12, 1569 CrossRef CAS.
  29. N. N. Greenwood and E. A. Earnshaw, Chemistry of the Elements, Pergamon, Oxford, 1990, p. 1400 Search PubMed.
  30. O. Kubaschewski, C. B. Alcock and P. J. Spencer, Materials Thermochemistry, Pergamon, Oxford, 1993, p. 257 Search PubMed.
  31. P. F. Warner, L. Eriksson and M. Westdahl, J. Appl. Crystallogr., 1985, 18, 360.
  32. M. Polak, J. Electron Spectrosc. Relat. Phenom., 1982, 28, 171 CrossRef CAS.
Click here to see how this site uses Cookies. View our privacy policy here.