Intercalation of metallic oxalato complexes CoOx 2 2-, CuOx 2 2-, MnOx 3 3-, and GaOx 3 3in [Zn 2 Al] and [Mg 2 Al] LDHs was successfully carried out leading to well characterized products in which metallic complexes lying between layers were subjected to minor modifications following intercalation as confirmed by XRD, FTIR, and particularly XAFS studies. The obtained data permitted modeling the layout of metallic oxalato complexes between the layers for each compound. Thermal treatments undertaken on exchanged compounds led to a mixing of oxides with increase in surface areas particularly for the Ga-containing product. Dispersed oxide and metallic particules were obtained by a soft chemistry treatment in refluxing ethylene glycol.
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