Mesoscale Characterization of Nanoparticles Distribution Using X‐ray Scattering

The properties of many functional materials depend critically on the spatial distribution of an active phase within a support. In the case of solid catalysts, controlling the spatial distribution of metal (oxide) nanoparticles at the mesoscopic scale offers new strategies to tune their performance and enhance their lifetimes. However, such advanced control requires suitable characterization methods, which are currently scarce. Here, we show how the background in small‐angle X‐ray scattering patterns can be analyzed to quantitatively access the mesoscale distribution of nanoparticles within supports displaying hierarchical porosity. This is illustrated for copper catalysts supported on meso‐ and microporous silica displaying distinctly different metal distributions. Results derived from X‐ray scattering are in excellent agreement with electron tomography. Our strategy opens unprecedented prospects for understanding the properties and to guide the synthesis of a wide array of functional nanomaterials.