Control of Dispersion of Ni2+ Ions via Chelate Ligands in the Preparation of Ni/SiO2 Materials. A XAFS Study

The influence of the Ni deposition mode on the dispersion of Ni2+ precursors was investigated in the preparation of Ni/SiO2 catalysts. The coordination sphere of Ni complexes was mainly studied by XAFS spectroscopy in the initial step (dried samples) and after a vacuum activating treatment at 700 °C. Four modes of deposition were compared, two leading to supported silicate phases (exchange with ammine ligands and deposition−precipitation) and the other ones using the ethanediamine ligand (exchange and impregnation modes) which produced isolated Ni2+ precursors in electrostatic interaction with the silica support. In this work, EXAFS spectroscopy has been found to be a suitable technique to probe metal−support interactions in the first step of the preparation (dried samples). For samples activated at 700 °C, this spectroscopy showed the presence of several categories of atoms in the first (oxygen backscatterers) and second (Ni and Si backscatterers) shells. A distribution of long (d ≈ 2.04 A) and short (d ...