Comparison of the preparation of cerium oxide nanocrystallites by forward (base to acid) and reverse (acid to base) precipitation

The morphological and structural characterization of CeO2 nanocrystallites prepared by forward and reverse precipitation techniques were investigated and compared by powder x-ray diffraction (PXRD), nitrogen adsorption (BET) and high resolution transmission electron microscopy (HRTEM) analysis. The...

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Bibliographic Details
Published in:Chemical engineering science 2013-03, Vol.91, p.102-110
Main Authors: Morris, V., Fleming, P.G., Holmes, J.D., Morris, M.A.
Format: Article
Language:English
Subjects:
adsorption
Anion defects
cerium
Cerium dioxide
chemical engineering
Crystallite size
Crystallites
Density
Dispersions
Forward precipitation
Morphology
Nanocrystals
Nanoparticles
nitrogen
Particulates
Precipitation
Reverse precipitation
Surface chemistry
transmission electron microscopy
X-ray diffraction
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Summary:The morphological and structural characterization of CeO2 nanocrystallites prepared by forward and reverse precipitation techniques were investigated and compared by powder x-ray diffraction (PXRD), nitrogen adsorption (BET) and high resolution transmission electron microscopy (HRTEM) analysis. The two routes gave quite different materials although in both cases the products were essentially highly crystalline, dense particulates. It was found that the reverse precipitation technique gave the smallest crystallites with the narrowest size dispersion. This route also gave as-synthesized materials with higher surface areas. HRTEM confirmed the observations made from PXRD data and showed the two methods resulted in quite different morphologies and surface chemistries. The forward route gives products with significantly greater densities of Ce3+ species compared to the reverse route. Data are explained using known precipitation chemistry and kinetic effects. [Display omitted] ► Forward and reverse precipitation routes to CeO2 were examined. ► Reverse precipitation results in smaller particles. ► Reverse precipitation results in precipitation products containing cerium mostly in the tetravalent state. ► Particle shape varies between the two precipitation methods. ► Ce3+ defect sites are at much lower defect concentrations in reverse precipitation.
ISSN:0009-2509
1873-4405
DOI:10.1016/j.ces.2013.01.016