In the preparation of silica-supported nickel oxide from nickel nitrate impregnation and drying, the replacement of the traditional air calcination step by a thermal treatment in 1% NO/Ar prevents agglomeration, resulting in highly dispersed NiO. The mechanism by which NO prevents agglomeration was investigated by using combined 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)4 had been formed. Comparison of the evolution of the decomposition gases during the thermal decomposition of Ni3(NO3)2(OH)4 in labeled and unlabeled NO and O2 revealed that NO scavenges oxygen radicals, forming NO2. The DRIFT spectra revealed that the surface speciation evolved differently in the presence of NO as compared with in O2 or Ar. It is proposed that oxygen scavenging by NO depletes the Ni3(NO3)2(OH)4 phase of nitrate groups, creating nucleation sites for the formation of NiO, which leads to very small (4 nm) NiO particles and prevents agglomeration
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