In this work, a study of the secondary porosity of two zeolite‐based composites is carried out by small angle X‐ray scattering (SAXS) and N2 adsorption at 77 K. The composites were obtained by the inclusion of ZnO nanoparticles in a Cuban natural clinoptilolite by mechanosynthesis and ‘in situ’ methods. It was observed a decrease in the specific surface area as a result of ZnO nanoparticles inclusion from 149 m2 g−1 in the started material to 60 m2 g−1 in the composite prepared by in situ method, whereas the mesopore diameter remained almost constant. The results confirmed the presence of mesopores with diameter between 3 and 36 nm, with good match by both methodologies. These materials were developed in view of their future application as catalysts and adsorbents, where the presence of secondary porosity is key to favor the diffusion processes.
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