Investigation of the Structure of Highly Dispersed NiO–SiO2 Catalyst Features Using X-Ray Analysis of the Atomic Pair Distribution Function

In this work, NiO and NiO–SiO₂ are studied using X-ray diffraction and the method of atomic-pair radial distribution. Using X-ray phase analysis, it is determined that the sizes of NiO particles have a coherent-scattering region of more than 100 nm, while the NiO–SiO₂ sample has particle sizes of about 2–3 nm. However, full-profile simulation using the Rietveld method does not allow one to describe the effects observed during diffraction: asymmetry of the peaks, the appearance of an additional shoulder of peak 111 in the region of small angles; therefore, the method of atomic-pair radial distribution is used to analyze the structure. When simulating the experimental curve of the atomic-pair radial distribution, 3 different models are used: pure NiO, a mixture of NiO and Ni₂SiO₄, as well as a modified NiO model with Si embedded into the crystal lattice. The latter model is created based on the assumption of the incorporation of silicon into the NiO structure, as can be evidenced by the X-ray diffraction data. According to the results of simulation of the curve of the atomic-pair radial distribution, it is the latter model that provides the best description of the observed effects: a significantly increased unit-cell parameter in comparison with the sample without the addition of SiO₂, as well as decreased cation–oxygen distances in the structure while the distances between cations are increased.