Abstract: | Mg/Cr and Ni/Cr hydrotalcites (HTs) were synthesised by the sol-gel method. This route was for the first time explored for Cr(III)-containing HTs. The hydrotalcite were synthesised starting with magnesium ethoxyde and nickel acetylacetonate, respectively, as divalent cation precursors and chromium acetylacetonate as trivalent cation precursor using basic catalysis (sodium hydroxide). Pure hydrotalcites containing materials with M(II)/Cr(III) = 3 were obtained. The presence of Ni(II) favoured the increasing of hydrotalcite crystallinity. The samples were investigated using X-ray diffraction and spectroscopic techniques, DTA/TGA measurements and transmission electron microscopy (TEM). The obtained compounds were pure hydrotalcite phases with very similar structural features, but exhibited particularities depending on the M(II) cation. The compounds were nanosized in both cases. The IR spectroscopy evidenced that the Ni(II) samples retained some organic groups on the surface, thus the decomposition processes of the Ni(II) containing sample being different from that of Mg(II) containing one. The decomposition process ended at lower temperature in the case of Ni/Cr hydrotalcite. |