The work of this thesis focuses on membrane technology for gas separation due to the merit of high energy efficiency relative to conventional techniques. Advanced polymers with high fractional free volume and highly porous nanoparticles with full organic framework are selected to fabricate mixed matrix membranes (MMMs). Efforts to further improve MMMs gas separation performance include solvent choice, nanoparticle size, polymer conformation, and synergistic methodology. Results demonstrate that compatible solvent, small particle size with homogenous dispersion in the polymer matrix, enhanced polymer and additive interaction, and the corresponding gas performance. Similar effects are observed for polymer conformation and synergistic methods.