Hostname: page-component-8448b6f56d-sxzjt Total loading time: 0 Render date: 2024-04-19T01:05:48.579Z Has data issue: false hasContentIssue false

The early stages of crystallite growth of CeO2 obtained from a cerium oxide nitrate

Published online by Cambridge University Press:  10 January 2013

N. Guillou
Affiliation:
Laboratoire de Cristallochimie (CSIM, URA CNRS 1495), Université de Rennes, Avenue du Général Leclerc, 35042 Rennes cedex, France
J. P. Auffrédic
Affiliation:
Laboratoire de Cristallochimie (CSIM, URA CNRS 1495), Université de Rennes, Avenue du Général Leclerc, 35042 Rennes cedex, France
D. Louër
Affiliation:
Laboratoire de Cristallochimie (CSIM, URA CNRS 1495), Université de Rennes, Avenue du Général Leclerc, 35042 Rennes cedex, France

Abstract

An analysis of the microstructure of nanocrystalline cerium oxide produced by thermal decomposition of cerium (IV) oxide nitrate at temperatures in the range 230° to 960 °C is described. Parameters describing the breadths and shape of X-ray diffraction line profiles were obtained by means of pattern decomposition and a method based on the Voigt function was used to obtain information on the temperature dependence of the microstructure. No marked anisotropy in size and strain broadening was observed. It was found that the crystallites are on average spherical, the dimensions increasing significantly with formation temperature, while microstrains decrease with annealing temperature. The results of size determinations were compared with SEM measurements. They suggest a competition between the crystallite growth and “particle” growth processes in the initial sintering of the loosely packed cerium oxide powder.

Type
Research Article
Copyright
Copyright © Cambridge University Press 1995

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

Auffrédic, J. P., Boultif, A., Langford, J. I., and Louër, D. (1995). “The early stages of crystallite growth of ZnO obtained from an oxalate precursor,” J. Am. Ceram. Soc. 78, 323328.CrossRefGoogle Scholar
de Keijser, Th. H., Langford, J. I., Mittemeijer, E. J., and Vogels, A. B. P. (1982). “Use of the Voigt function in single-line method for the analysis of X-ray diffraction line broadening,” J. Appl. Cryst. 15, 308314.CrossRefGoogle Scholar
Delhez, R., de Keijser, Th. H., and Mittemeijer, E. J. (1982). “Determination of crystallite size and lattice distortions through X-ray diffraction line profile analysis,” Fres. Z. Anal. Chem. 312, 116.Google Scholar
Fievet, F., Germi, P., de Bergevin, F., and Figlarz, M. (1979). “Lattice parameter, microstrains and non-stoichiometry in NiO. Comparison between mosaic microcrystals and quasi-perfect single microcrystals,” J. Appl. Cryst. 12, 387394.CrossRefGoogle Scholar
Guillou, N., Auffrédic, J. P., and Louér, D. (1994). “Synthesis, crystal structure, and thermal behavior of cerium (IV) oxide nitrate Ce2O(NO3)6(H2O)6.2H2O,” J. Solid State Chem. 112, 4552.CrossRefGoogle Scholar
Halder, N. C., and Wagner, C. N. J. (1966). “Separation of particle size and lattice strain in integral breadth measurements,” Acta Cryst. 20, 312313.CrossRefGoogle Scholar
Langford, J. I. (1992). “The use of the Voigt function in determining microstructural properties from diffraction data by means of pattern decomposition,” in Accuracy in Powder Diffraction II, edited by Prince, E. and Stalick, J. K. (NIST Spec. Public. 846, Gaithersburg), pp. 110126.Google Scholar
Langford, J. I., Boultif, A., Auffrédic, J. P., and Louér, D. (1993). “The use of pattern decomposition to study the combined X-ray diffraction effects of crystallite size and stacking faults in ex-oxalate zinc oxide,” J. Appl. Cryst. 26, 2223.CrossRefGoogle Scholar
Langford, J. I., Louër, D., Sonneveld, E. J., and Visser, J. W. (1986). “Applications of total pattern fitting to a study of crystallite size and strain in zinc oxide powder,” Powder Diffr. 1, 211221.CrossRefGoogle Scholar
Louër, D. (1994). “Applications of profile analysis for micro-crystalline properties from total pattern fitting,” Adv. X-ray Anal. 37, 2735.Google Scholar
Louër, D., and Langford, J. I. (1988). “Peak shape and resolution in conventional diffractometry with monochromatic X-rays,” J. Appl. Cryst. 21, 430437.CrossRefGoogle Scholar
Morosin, B., and Graham, R. A. (1984). “X-ray diffraction line-broadening studies on shock-modified rutile and alumina,” Mater. Sci. Eng. 66, 7387.CrossRefGoogle Scholar
Toraya, H. (1989). “The determination of direction-dependent crystallite size and strain by X-ray whole-powder-pattern fitting,” Powder Diffr. 4, 130136.CrossRefGoogle Scholar