The effect of typical membrane processing conditions on the structure, interfacial morphology, and gas separation performance of MOF/polymer nanocomposite membranes is investigated. In particular, the ZIF-8/Matrimid® nanocomposite membrane system is examined, and it is shown that ultrasonication - a commonly employed particle dispersion method - induces significant changes in the shape, size distribution, and structure of ZIF-8 particles suspended in an organic solvent during membrane processing. Dynamic light scattering and electron microscopy reveal that ZIF-8 nanoparticles undergo substantial Ostwald ripening when subjected to high intensity ultrasonication as often required in the formation of MOF/polymer nanocomposite membranes. Other characterization techniques reveal that the ripened particles exhibit lower pore volumes and lower surface areas compared to the as-made material. ZIF-8/Matrimid® composite membranes fabricated using two sonication methods show significant differences in microstructure. Permeation measurements show significant enhancement in permeability of CO 2 and increased CO 2/CH 4 selectivity in membranes fabricated with high-intensity sonication. In contrast, composite membranes prepared with low-intensity sonication are found to be defective. A careful evaluation of MOF membrane processing conditions, as well as knowledge of the properties of the MOF material after these membrane processing steps, are necessary to develop reliable processing-structure-property relations for MOF-containing membranes. © 2012 Elsevier Inc. All rights reserved.