Quantitative Deviation of Nanocrystals Using the RIR Method in X-ray Diffraction (XRD)

The reference intensity ratio (RIR) method, using X-ray diffraction (XRD), is considered one most of the rapid and convenient approaches for phase quantification in multi-phase mixture, in which nanocrystals are commonly contained in a mixture and cause a broadening of the diffraction peak, while another broadening factor, instrumental broadening, does not attract enough attention in related quantitative analysis. Despite the specimen consisting of 50 wt.% TiO₂ nanomaterials (nano-TiO₂) and 50 wt.% microscale ZnO powder, the nano-TiO₂ quantitative result changes from 56.53% to 43.33% that occur as a variation of instrumental broadening are caused by divergence slit adjustment. This deviation could be accounted through a mathematical model that involves instrumental broadening. The research in this paper might provide a useful guide for developing an approach to measure accuracy quantification in unknown multi-phase mixtures.