Hostname: page-component-586b7cd67f-t7czq Total loading time: 0 Render date: 2024-11-25T15:17:23.176Z Has data issue: false hasContentIssue false

The Art of the Possible: An Overview of Catalyst Specimen Preparation Techniques for TEM Studies

Published online by Cambridge University Press:  21 February 2011

Stephen B. Rice
Affiliation:
Exxon Research & Engineering Co., Clinton Township, Route 22 East, Annandale, NJ 08801
Michael M. J. Treacy
Affiliation:
Exxon Research & Engineering Co., Clinton Township, Route 22 East, Annandale, NJ 08801
Get access

Abstract

Obtaining useful microstructural information about catalysts requires appropriate procedures for preparing specimens for the transmission electron microscope. Unfortunately, most descriptions of catalyst specimen preparation are scattered throughout numerous journal articles or are unavailable. Traditional techniques for preparing heterogeneous catalyst powders include primarily dilute dispersion and ultramicrotomy. The advantages and disadvantages of these will be discussed in terms of information obtainable and possible artifacts. In addition, techniques for preparing layered materials, as well as some novel approaches and model systems, will be presented. With these, as with more traditional approaches, the best method for a specific material will be arrived at only through experimentation. Our aim is to describe a variety of possibilities for getting an already synthesized catalyst into the microscope suitably neat, thin, and artifactfree.

Type
Research Article
Copyright
Copyright © Materials Research Society 1988

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

REFERENCES

1. Goodhew, P., Specimen Preparation in Materials Science, Vol. I, Part I, Practical Methods in Electron Microscopy, edited by Glauert, Audrey M. (North-Holland, 1973), 184 pp.Google Scholar
2. Sprys, J. W., Bartosiewicz, L., McCune, R., and Plummer, H. K., J. Catal. 39, 91103 (1975).CrossRefGoogle Scholar
3. Sanders, J. V., J. Elec. Micr. Tech. 3, 6793 (1986).Google Scholar
4. Onuferko, J. H., DeCanio, S. J., Dybowski, C., Hall, I. W., and Gates, B. C., J. Catal. 89, 550552 (1984).CrossRefGoogle Scholar
5. Via, G. H., Meitzner, G., Lytle, F. W., and Sinfelt, J. H., J. Chem. Phys. 79, 11527–1529 (1983).Google Scholar
6. Adams, C. R., Benesi, H. A., Curtis, R. M., and Meisenheimer, R. G., J. Catal. 1, 336344 (1962).CrossRefGoogle Scholar
7. Carr, M. J., J. Elec. Micr. Tech. 2, 439443 (1985).Google Scholar
8. Backus, R. C. and Williams, R. C., J. Appl. Phys. 21, 1115 (1950).CrossRefGoogle Scholar
9. Wilson, G. R. and Hall, W. K., J. Catal. 17, 190206 (1970).Google Scholar
10. Timsit, R. S., Hutchison, J. L., and Thornton, M. C., Ultramicr. 15, 371374 (1984).Google Scholar
11. Glauert, A. M. and Phillips, R., in Techniques for Electron Microscopy, edited by Kay, D. H. (Blackwell, Oxford, 1965), p. 213.Google Scholar
12. Chan, I. Y., Cain, J. H., and Rea, T. M., 43rd Proc. Elec. Micr. Soc. Amer., edited by Bailey, G. W. (San Francisco Press, 1985), pp. 174–5.Google Scholar
13. Csencsits, R., Schooley, C., and Gronsky, R., J. Elec. Micr. Tech. 2, 643644 (1985).CrossRefGoogle Scholar
14. Sawruk, S., Rohrman, A. C. Jr., and Kokotailo, G. T., J. Catal. 40, 379382 (1975).CrossRefGoogle Scholar
15. Hall, J. B., 42nd Proc. Elec. Micr. Soc. Amer., edited by Bailey, G.W. (Claitor's Publishing, Baton Rouge, 1984), p. 650; J. B. Hall and P. P. Hruskoci, 41st Proc. Elec. Micr. Soc. Amer., edited by G. W. Bailey (Claitor's Publishing, Baton Rouge, 1983), pp. 342–3.Google Scholar
16. Lyman, C. E., in Materials Problem Solving With the Transmission Electron Microscope, edited by Hobbs, L. W., Westmacott, K. H., and Williams, D. B. (Mater. Res. Soc. Proc. 62, Pittsburgh, PA 1986) pp. 403413.Google Scholar
17. Koo, J. and Smith, P., personal communication.Google Scholar
18. Fernández-Morán, H., Exptl. Cell Res. 5, 255 (1953).CrossRefGoogle Scholar
19. Reid, N., Ultramicrotomy, Vol.3, Part H of Practical Methods in Electron Microscopy, edited by Glauert, Audrey (Elsevier/North-Holland Biomedical Press, 1975), 353 p.Google Scholar
20. Blake, D. F., Bunch, T. E., Philpott, D. E., and Zeiger, R., J. Elec. Micr. Tech. 6, 305306 (1987).Google Scholar
21. Sclar, C. B. and Dillinger, L., Am. Mineral. 45, 862870 (1960).Google Scholar
22. Deckman, H. W. and Dunsmuir, J. H., Appl. Phys. Lett. 41(4), 377–9 (1982); C. B. Roxlo, H. W. Deckman, J. Gland, S. D. Cameron, and R. R. Chianelli, Science 235, 1629–31 (1987).Google Scholar
23. Murphy, D. W. and Hull, G. W., J. Chem. Phys. 62,973 (1975); A. Lerf and R. Schöllhorn, Inorg. Chem. 16, 2950 (1975); L. F. Nazar and A. J. Jacobson, J. Chem. Soc., Chem. Commun. 1986, 570–571.Google Scholar
24. Rice, S. B., Treacy, M. M. J., Jacobson, A. J., and Lewandowski, J. T., in preparation.Google Scholar
25. Baker, R. T. K., Prestridge, E. B., and Garten, R. L., J. Catal. 56, 390406 (1979).CrossRefGoogle Scholar
26. Ruckenstein, E. and Malhotra, M. L., J. Catal. 41, 303311 (1976); Y. F. Chu and E. Ruckenstein, J. Catal. 55, 281 (1978).Google Scholar
27. Harris, P. J. F., Boyes, E. D., and Cairns, J. A., J. Catal. 82, 127 (1983); P. J. F. Harris, J. Catal. 7, 527–542 (1986).CrossRefGoogle Scholar
28. Chen, M. and Schmidt, L. D., J. Catal. 55, 348360 (1978).Google Scholar
29. Datye, A. K. and Logan, A. D., in 44th Proc. Elec. Micr. Soc. Amer., edited by Bailey, G. W. (San Francisco Press, 1986), pp. 772–3.Google Scholar
30. Smith, D. M., Wright, T., and Stermer, D., Amer. Assoc. Aerosol Res., 1985 Ann. Meeting, paper 1F3 (1985).Google Scholar
31. Jacobs, J. W. M. and Verhoeven, J. F. C. M., J. Micr. 143, 103116 (1986).CrossRefGoogle Scholar
32. Renou, A., J. Catal. 78, 7787 (1982).Google Scholar
33. Disko, M. M., Treacy, M. M. J., Rice, S. B., Chianelli, R. R., Gland, J. A., Halbert, T. R., and Ruppert, A. F., Ultramicr., in press.Google Scholar
34. Hoelke, C. W., Micron 5, 307311 (1975); R. Reichelt, T. König, and G. Wangermann, Micron 8, 29–31 (1977).Google Scholar
35. Poppa, H., Papageorgopoulos, C. A., Marks, F., and Bauer, E., Atoms, Molecules and Clusters 3, 279289 (1986).Google Scholar
36. Kesson, S. E. and White, T. J., Proc. Roy. Soc. Lond. A 408, 295319 (1986).Google Scholar
37. Headley, T. J., in 39th Proc. Electron Microscopy Society of America, edited by Bailey, G. W. (Claitor's Publishing, Baton Rouge, 1981), pp. 114–5.Google Scholar