Abstract
An environmental cell high resolution electron microscope (EHREM) has been developed for in-situ studies of dynamic gas molecule-solid interactions on the atomic scale. It allows access to metastable intermediate phases of materials, to both surface and bulk structural changes which are often interrelated, to reaction mechanisms for probing materials performance in reaction environments and to sequences of reversible microstructural and chemical development associated with their operation. Materials transported through air can be restored or recreated and samples damaged, e.g. by dehydration, by the usual vacuum environment in a conventional electron microscope can be preserved. A Philips CM30 high resolution transmission EM (HRTEM)/Scanning transmission EM (STEM) system has been extensively modified in our laboratory to add an environmental cell in the EM column which provides facilities for in-situ gas-solid reaction studies in controlled atmospheres of gas or vapor at pressures of 0–50 mbar, instead of the regular TEM high vacuum environment. The integrated new environmental cell capability is combined with the original 0.23 nanometer (nm) TEM lattice resolution with access to interatomic spacings, STEM imaging (bright field/annular dark field), electron diffraction and chemical microanalyses. Regular sample holders are used and include hot stages to >1000 °C. The learnings from well designed dynamic in-situ EM studies of reaction sequences between gases or vapors and solids can be considerable. Examples of in-situ applications include direct studies of dynamic reactions with chemically stabilized silica based ceramics, the formation of active vanadyl pyrophopsphate catalysts from their hemihydrate precursors for vapor phase oxidation of hydrocarbons and carbon nanostructures.
Access this chapter
Tax calculation will be finalised at checkout
Purchases are for personal use only
Preview
Unable to display preview. Download preview PDF.
Similar content being viewed by others
References
Gai, P.L., Catal. Reviews-Sci. & Eng. 34, 1, 1992.
Sinclair, R., Yamashita, T. and Ponce, F.A. Nature 290, 386, 1981.
Pashley, D.W. et al, Phil. Mag.10, 127, 1964.
Yagi, K. et al Thin Solid Films 126, 95, 1985; and this book.
Butler, E. P. and Hale, K. F.: Dynamic Experiments in the Electron Microscope, North Holland, Amsterdam, 1981.
Agar, A. W. et al, in: Proc. 7th Int.Congr.on Electron Microscopy, Vol.1, p. 115; Grenoble, 1982.
Swann, P.R. and Tighe, N., in: Proc. 5th Eur. Congr. on Electron Microscopy, Manchester, p. 436, 1972.
Baker, R.T.K and Chuldzinki, J. Carbon, 19, 75, 1981.
Doole, R.C., Parkinson, G. and Stead, J.M., in: Inst.Phys.Conf.Ser., Vol. 119, Bristol, p.161, 1991.
Gai, P.L., Phil.Mag. 43, 841, 1981.
Gai, P.L. et al, Phil. Mag. A45 531, 1982.
Gai, P.L., Smith, B.C. and Owen, G. Nature 348, 430, 1990.
Hirsch P.B., Howie, A. et al, EM of Thin Crystals, Krieger, 1985.
Cowley, J.M. Diffraction Physics, North Holland, 1981.
Williams D.B. and Carter B.C., Transmission EM, Plenum, 1996.
Boyes, E.D. and Gai, P.L., Proc. Mat.Res.Soc. Vol 404, 53, 1996, Publ. Materials Res.Soc, Pittsburgh USA; Ultramicroscopy (1997).
Haggin, J.: Chem & Eng News. Amer.Chem.Soc. 1995.
Gai, P.L., Thomas, J.M., Wright P.et al: J.Phys.Chem. 1992.
Boyes, E.D., Hanna. L.G. and Gai. P.L., Proc. MSA (Micr.Soc.America, San Frans. Press; Ed: G.Bailey), 50, 1630 (1992).
Florke, O., Ber.Keram.Ges. 32, 369, 1955.
Fenner, C.N., Am.J.Sc. 36, 331, 1913.
Peacor, D.R., Z. Kristall. 138, 274, 1973.
O.Keefe, M. and Hyde, B.G., Acta Cryst. B32, 2923, 1976.
Leadbetter, A.J., Nature 244, 125, 1973.
Wright, A.F. and Leadbetter, A.J., Phil.Mag. 31, 1391, 1975.
Perrota, A. et al, J. Am.Ceram.Soc, 72, 441, 1979.
Wilson, M.J. et al, Cent.Min.Pet. 47, 1, 1974.
Welberry, T.R., Hua, G.L. and Withers, R., J.Appl.Cryst. 22, 87, 1989. and Withers R. and Thompson, J. 1997; this book.
Saltzberg, M. et al, J.Am.Cer.Soc. 75, 89, 1992.
Gai, P.L., Saltzberg,, M. and Vega, A., J.Solid.St.Chem. 106, 35, 1993.
Buerger, M.J., Am.Min. 39, 600, 1954.
Boyes, E.D. Proc. XIII Internat.EM Congress, Paris, France, 1994.
Hodnett, B.K., Catal.Rev-Sci.& Eng. 27, 373, 1985.
Bordes, E., Catal.Today 1 (1987) 499
Bordes, E. Catal.Rev-Sci.& Eng., 16, 1993.
Gai, P. L. and Kourtakis, K., Science 267, 647, 1995.
Gai, P.L. et al, Catalyst Materials for High Temp. Processes; Ed: K.S. Ramesh, Makoto Misono and Pratibha L. Gai, Publ: American Ceramic Society, 73, 1997.
Torardi, C.C. and Calabrese,J.C. Inorg.Chem. 23, 1308, 1984.
Gorbunova, Yu.E. and Linde, S.A, Sov.Phy-Dockl (Eng.Trans.) 24, 138, 1979.
Gai, P.L. and Torardi, C.C., in: Proc. Materials Research Society, Vol. 404, (Ed: R. Sharma, P.L. Gai, M. Gazdarziska, R. Sinclair, L. Whitman); Publ: Mat. Res. Soc Pittsburgh, 1996.
Gai, P.L., Acta Cryst. B53, 346, 1997.
Author information
Authors and Affiliations
Editor information
Editors and Affiliations
Rights and permissions
Copyright information
© 1997 Springer Science+Business Media New York
About this chapter
Cite this chapter
Gai, P.L., Boyes, E.D. (1997). Environmental High Resolution Electron Microscopy in Materials Science. In: Gai, P.L. (eds) In-Situ Microscopy in Materials Research. Springer, Boston, MA. https://doi.org/10.1007/978-1-4615-6215-3_6
Download citation
DOI: https://doi.org/10.1007/978-1-4615-6215-3_6
Publisher Name: Springer, Boston, MA
Print ISBN: 978-0-7923-9989-6
Online ISBN: 978-1-4615-6215-3
eBook Packages: Springer Book Archive