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In this article, effects of synthesis parameters (synthesis temperature, synthesis time, and number of layers) on W‐type zeolite membranes synthesized over flat SUS supports for O2/SF6 gas separation were experimentally investigated. Experiments were carried out at these levels of synthesis temperature: 165°C, 185°C, and 200°C; synthesis time: 6, 12, and 18 h and number of layers: 1 and 2. Permeation measurements, XRD and SEM analysis were used for characterization of the synthesized membranes. The results showed that increasing synthesis temperature from 165°C up to 185°C increases separation factor of O2/SF6, however, further increasing decreases the separation performance. The same trend was observed for synthesis time for the single layer synthesized zeolite W membrane, although for the double layer synthesized zeolite W membrane, separation factor increased with increasing synthesis time. Repetition of layering has a net positive effect on separation factor of O2/SF6, and negative effect on permeation flux through the membranes. This behavior was attributed to the dual effect of synthesis temperature and synthesis time on selectivity. More zeolite crystals are deposited and larger crystals are formed at higher synthesis temperatures and longer synthesis times. Well W‐type zeolite membrane was synthesized at 185°C for 18 h with two repeating layers with a high separation factor of 20.1.

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