A sol-gel method was applied for the development of highly permeable hydrogen separation membranes using bis(triethoxysilyl)ethane (BTESE) as a silica precursor. Hybrid silica membranes showed quite high hydrogen permeance (1 x 10(-5) mol m(-2) s(-1) Pa(-1)) with a high H(2)-to-SF(6) selectivity of 1000 because of loose organic-inorganic silica networks. Hybrid silica membranes were found to show high hydrothermal stability due to the presence of Si-C-C-Si bonds in silica networks.

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Exceptionally homogeneous and ultrathin COF membranes were successfully fabricated using exfoliated COF nanosheets with uniform perforations as membrane building blocks. The COF membranes showed highly permeable performance due to the ultrafast molecular diffusion through the perforations of the COF nanosheets and the excellent thermal stability due to the robust covalent bonds in the framework.

Co‐doped silica sol solutions with varying Co composition (Co/(Si+Co)=10–50 mol%) were prepared from tetraethoxysilane and Co(NO3)2·6H2O. Subsequently, these solutions were used in the preparation of hydrogen separation microporous membranes with enhanced hydrothermal stability at 500°C under a steam pressure of 300 kPa. At Co concentrations >33%, the XRD pattern and peak intensity of the Co‐doped silica preparations were similar and were not dependent on Co composition, suggesting that Co was incorporated into the silica network. The best H2 permeation performance in a steam atmosphere (500°C; steam pressure, 300 kPa) was obtained using silica doped with approximately 30 mol% Co. Co‐doped silica membranes (Co 33 mol%) fired at 600°C under a steam partial pressure of 90 kPa showed stable gaseous permeances and a H2 permeance of approximately 2.00–4.00 × 10−6 m3(STP)·(m·s·kPa)−1 with a selectivity of 250–730 (H2/N2), even after 60 h of exposure to steam (steam pressure, 300 kPa) at 500°C.

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Organic/inorganic hybrid silica membranes were prepared from 1,1,3,3‐tetraethoxy‐1,3‐dimethyl disiloxane (TEDMDS) by the sol‐gel technique with firing at 300–550°C in N2. TEDMDS‐derived silica membranes showed high H2 permeance (0.3–1.1 × 10−6 mol m−2 s−1 Pa−1) with low H2/N2 (∼10) and high H2/SF6 (∼1200) perm‐selectivity, confirming successful tuning of micropore sizes larger than TEOS‐derived silica membranes. TEDMDS‐derived silica membranes prepared at 550°C in N2 increased gas permeances as well as pore sizes after air exposure at 450°C. TEDMDS had an advantage in tuning pore size by the “template” and “spacer” techniques, due to the pyrolysis of methyl groups in air and SiOSi bonding, respectively. For pore size evaluation of microporous membranes, normalized Knudsen‐based permeance, which was proposed based on the gas translation model and verified with permeance of zeolite membranes, reveals that pore sizes of TEDMDS membranes were successfully tuned in the range of 0.6–1.0 nm. © 2011 American Institute of Chemical Engineers AIChE J, 2011

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