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We developed a series of molecule-scale hybrid amine-silica membranes synthesized from organoalkoxysilane precursors of 3-(triethoxysilyl)propan-1-amine (PA-Si) and 3-(triethoxysilyl)-N-methylpropan-1-amine (SA-Si), and made these functional using either unhindered amines or a 3-(triethoxysilyl)-N,N-dimethylpropan-1-amine (TA-Si) that is sterically hindered. CO 2 adsorption-desorption measurements of amine-silica powdered xerogels were conducted to observe the effect of amine type on CO 2 adsorption and desorption/diffusion properties. The results revealed that TA-Si xerogel powders demonstrated faster kinetics for both adsorption and desorption processes compared with those of the PA-Si and SA-Si samples due to the steric hindrance effect of the amine, which reduced the CO 2 binding energy and thereby boosted both the forward and reverse reaction rates of CO 2 -amine. In single-gas permeation performances, all the membranes exhibited excellent molecular sieving at higher temperatures and all the gases considered, except CO 2 , tended to permeate the membranes via activated diffusion. The effect of amine type on CO 2 separation performance was compared using CO 2 permeance, CO 2 /N 2 selectivity, activation energy for permeation ( E p ) of CO 2 [ E p (CO 2 ) ], and differences in E p between CO 2 and N 2 [ E p (CO 2 )-E p (N 2 ) ]. The TA-Si membrane demonstrated superior CO 2 separation performance, and achieved the highest values for both CO 2 permeance and selectivity. A relatively smaller difference in CO 2 separation performance was observed between PA-Si and SA-Si membranes despite some differences in basicity. This suggests that, rather than the basicity, it was the steric hindrance effect that played the greatest role in CO 2 transport performance across amine-silica membranes. [ABSTRACT FROM AUTHOR]