Identification of Outer and Inner Nickel Particles in a Mesoporous Support: How the Channels Modify the Reducibility of Ni/SBA‐15 Catalysts

Abstract Two different nickel supported on SBA‐15 catalytic systems have been prepared by means of impregnation (Ni/SBA‐15‐ImU) and deposition‐precipitation (Ni/SBA‐15‐DP) methodologies. Upon calcination, Ni/SBA‐15DP presents a well‐developed nickel phyllosilicate phase, which after reduction gives rise to a dispersed and homogeneous metallic phase, mainly located inside the 5 nm in diameter mesoporous structure of the support. On the contrary, as evidenced by XRD and a double temperature programmed reduction (TPR) peak, the Ni/SBA‐15‐ImU catalyst presents two different NiO phases, which after reduction in hydrogen generate nickel particles in a wide range of sizes. In situ XAS and XPS have unambiguously showed that the distinct TPR profiles obtained for each system are related with particles located in and out the mesoporous structure of the SBA‐15 channels. The particles inside the porous are more difficult to reduce, clearly showing a kind of confinement effect of the SBA‐15 mesostructure, modifying the reducibility of the NiO phase.