Synthesis of PbS nanocrystallites using a novel single molecule precursors approach: X-ray single-crystal structure of Pb(S₂CNEtPrⁱ)₂

Abstract

The synthesis and characterisation of some lead(ii) dithiocarbamato complexes Pb(S₂CNRR′)₂ is reported. These compounds were used as single molecule precursors to produce nanocrystalline PbS by their thermolysis in trioctylphosphine oxide. The optical and morphological properties of the resulting PbS nanocrystallites were investigated; the influence of experimental parameters, such as precursor, growth time and temperature, on the final nanodispersed materials is also reported.

References

1. A. Henglein, Chem. Rev., 1989, 89, 1861.
2. M. L. Steigerwald and L. E. Brus, Acc. Chem. Res., 1990, 23, 183.
3. H. Weller, Adv. Mater., 1993, 5, 88.
4. A. Hagfeldt and M. Grätzel, Chem. Rev., 1995, 95, 49.
5. J. H. Fendler and F. C. Meldrun, Adv. Mater., 1995, 7, 607.
6. A. P. Alivisatos, J. Phys. Chem., 1996, 100, 13226.
7. A. J. Nozik, F. Williams, M. T. Nenadovic, T. Rajh and O. I. Micic, J. Phys. Chem., 1985, 89, 397.
8. T. K. Leodidou, W. Caseri and U. W. Suter, J. Phys. Chem., 1994, 98, 8992.
9. S. Gallardo, M. Gutierrez, A. Henglein and E. Janata, Ber. Bunsen-Ges. Phys. Chem., 1989, 93, 1080.
10. Y. Wang and N. Herron, J. Phys. Chem., 1991, 95, 525.
11. Y. Wang, A. Suna, W. Mahler and R. Kasowski, J. Chem. Phys., 1987, 87, 7315.
12. R. Tassoni and R. R. Schrock, Chem. Mater., 1994, 6, 744.
13. M. Moffitt and A. Eisenberg, Chem. Mater., 1995, 7, 1178.
14. T. Trindade and P. O'Brien, Adv. Mater., 1996, 8, 161.
15. C. B. Murray, D. J. Norris and M. G. Bawendi, J. Am. Chem. Soc., 1993, 115, 8706.
16. G. Kräuter, P. Favreau and W. S. Rees, Jr., Chem. Mater., 1994, 6, 543.
17. T. Trindade and P. O'Brien, Adv. Mater., in press.
18. R. A. Zingaro and J. C. White, J. Inorg. Nucl. Chem., 1960, 12, 315.
19. G. M. Sheldrick, SHELX, a program for crystal structure solution, University of Göttingen, 1986.
20. G. M. Sheldrick, SHELXL-93, program for crystal structure solution, University of Göttingen, 1993.
21. M. A. Bernard and M. M. Borel, Bull. Soc. Chim. Fr., 1969, 9, 3064.
22. M. A. Bernard and M. M. Borel, Bull. Soc. Chim. Fr., 1969, 9, 1966.
23. F. Bonati and G. Minghetti, Chim. Ind. (Milan), 1970, 52, 1204.
24. L. A. Kosareva and S. V. Larionov, Izv. Sib. Otd. Akad. Nauk SSSR, Ser. Khim. Nauk, 1989, 4, 33.
25. H. Iwasaki, Acta Crystallogr., Sect. B, 1980, 36, 2138.
26. Z. V. Zvonkova, A. N. Khvatkina and N. S. Ivanova, Kristallografiya, 1967, 12, 1065.
27. H. Iwasaki and H. Hagihara, Acta Crystallogr., Sect. B, 1972, 28, 507.
28. M. Ito and H. Iwasaki, Acta Crystallogr., Sect. B, 1980, 36, 443.
29. A. J. Bondi, J. Phys. Chem., 1964, 68, 441.
30. S. L. Lawton and G. T. Kokotailo, Inorg. Chem., 1972, 11, 363.
31. H. U. Hummel, E. Fischer, T. Fischer, D. Gruβ, A. Franke and W. Dietzsch, Chem. Ber., 1992, 125, 1565.
32. F. Bonati and R. Ugo, J. Organomet. Chem., 1967, 10, 257.
33. D. M. Adams and J. B. Cornell, J. Chem. Soc. A, 1968, 1299.
34. D. M. Adams and J. B. Cornell, J. Chem. Soc. A, 1967, 884.
35. T. Y. Koh, PhD Thesis, University of London, 1994.
36. M. Motevalli, P. O'Brien, J. R. Walsh and I. M. Watson, Polyhedron, 1996, 15, 2801.
37. P. O'Brien, J. R. Walsh, I. M. Watson, M. Motevalli and L. Henriksen, J. Chem. Soc., Dalton Trans., 1996, 2491.