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Formation of solid particles by hydrolysis of cerium (IV) sulphate

Part I Time evolution of the hydrolysed solutions

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Abstract

Uniform particles of controlled morphology of CeOSO4·H2O may be prepared by forced hydrolysis, at 90 °C, of solutions of cerium (IV) sulphate. A structural description is given here of the different steps of the forced hydrolysis before precipitation takes place. It uses essentially the complementary techniques of extended X-ray absorption fine structure spectroscopy and small-angle X-ray scattering to characterize, at different length scales, the structural evolution of the solution. The first step, which occurs as temperature is raised above 60 °C, is an inorganic polymerization that transforms molecular dimeric precursors Ce2(OH)2O12 into colloidal particles. In the second step, at the ageing temperature of 90 °C, no chemical and structural changes are revealed; the solution has reached an equilibrium state characterized by the presence of 3 nm large monodisperse colloids which use 85% of the initial cerium ions and smaller particles (15%). The detailed local structure around the cerium atoms in the colloids is compatible with the formation of a chain-like structure of Ce(IV) ions via hydroxo bridges (Ce(OH)2) 2 n+ n . A mechanism to explain the transformation of precursors into colloids is proposed.

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Authors and Affiliations

  1. LURE, Université Paris-Sud, 91405, Orsay Cedex, France

    V. Briois, C. E. Williams, H. Dexpert & F. Villain

  2. DSPC, CEN-Saclay, 91191, Gif-sur-Yvette Cedex, France

    B. Cabane

  3. Rhône-Poulenc, CRA, 52 rue de la Haie Coq, 93308, Aubervilliers Cedex, France

    F. Deneuve & C. Magnier

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  1. V. Briois
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  2. C. E. Williams
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  3. H. Dexpert
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  4. F. Villain
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  5. B. Cabane
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  6. F. Deneuve
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  7. C. Magnier
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Briois, V., Williams, C.E., Dexpert, H. et al. Formation of solid particles by hydrolysis of cerium (IV) sulphate. JOURNAL OF MATERIALS SCIENCE 28, 5019–5031 (1993). https://doi.org/10.1007/BF00361172

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