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Ni/ZrO 2 catalysts, active and selective for the catalytic partial oxidation of methane to syngas (CH 4 -CPO), were prepared by the dry impregnation of zirconium oxyhydroxide (Z hy ) or monoclinic ZrO 2 (Z m ), calcination at 1173 K and activation by different procedures: oxidation-reduction ( ox-red ) or direct reduction ( red ). The characterization included XRD, FESEM, in situ FTIR and Raman spectroscopies, TPR, and specific surface area measurements. Catalytic activity experiments were carried out in a flow apparatus with a mixture of CH 4 :O 2 = 2:1 in a short contact time. Compared to Z m , Z hy favoured the formation of smaller NiO particles, implying a higher number of Ni sites strongly interacting with the support. In all the activated Ni/ZrO 2 catalysts, the Ni-ZrO 2 interaction was strong enough to limit Ni aggregation during the catalytic runs. The catalytic activity depended on the activation procedures; the ox-red treatment yielded very active and stable catalysts, whereas the red treatment yielded catalysts with oscillating activity, ascribed to the formation of Ni δ+ carbide-like species. The results suggested that Ni dispersion was not the main factor affecting the activity, and that active sites for CH 4 -CPO could be Ni species at the boundary of the metal particles in a specific configuration and nuclearity.

Oscillatory Behaviour of Ni Supported on ZrO2 in the Catalytic Partial Oxidation of Methane as Determined by Activation Procedure