DRIFTS/MS/Isotopic Labeling Study on the NO-Moderated Decomposition of a Silica-Supported Nickel Nitrate Catalyst Precursor

International audienceIn the preparation of silica-supported nickel oxide from nickel nitrate impregnation and drying, the replacementof the traditional air calcination step by a thermal treatment in 1% NO/Ar prevents agglomeration, resultingin highly dispersed NiO. The mechanism by which NO prevents agglomeration was investigated by usingcombined in situ diffuse reflectance infrared fourier transform (DRIFT) spectroscopy and mass spectrometry(MS). After impregnation and drying, a supported nickel hydroxynitrate phase with composition Ni3(NO3)2(OH)4had been formed. Comparison of the evolution of the decomposition gases during the thermal decompositionof Ni3(NO3)2(OH)4 in labeled and unlabeled NO and O2 revealed that NO scavenges oxygen radicals, formingNO2. The DRIFT spectra revealed that the surface speciation evolved differently in the presence of NO ascompared with in O2 or Ar. It is proposed that oxygen scavenging by NO depletes the Ni3(NO3)2(OH)4 phaseof nitrate groups, creating nucleation sites for the formation of NiO, which leads to very small (?4 nm) NiOparticles and prevents agglomeration