• Membrane Journal
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• v.25 no.2
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• pp.191-201
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• 2015

We have studied on the preparation of $TiCo_xFe_{1-x}$(x=0.50~1.00) system alloy, the characteristics of $TiCo_xFe_{1-x}$(x=0.50~1.00) system alloy by X-ray diffractometer (XRD), pressure composition temperature (PCT) curve, scanning electron microscopy (SEM) and the $H_2-N_2$ gas mixture separation of $TiCo_xFe_{1-x}$(x=0.50~1.00)- stainless steel (SS) composite membranes. The formation of $TiCo_xFe_{1-x}$(x=0.50~1.00) system alloys with cubic crystal same as TiCo was confirmed by X-ray diffractometer. $TiCo_xFe_{1-x}$(x=0.50~1.00) system alloys showed the hysteresis at $120^{\circ}C$. As the Fe content of $TiCo_xFe_{1-x}$(x=0.50~1.00) system alloys increased, the hysteresis was increased both range x=0.90~1.00 and x=0.55~0.60, and the range x=0.55~0.90 gave decreased hysteresis. $TiCo_{0.55}Fe_{0.45}$ alloy was the one showed the lowest hysteresis among them. The lowest value of hydrogen permeation pressure of $TiCo_xFe_{1-x}$(x=0.50~1.00)-SS composite membrane was $TiCo_{0.55}Fe_{0.45}$-SS composite membrane with the value of 2.5 atm at $120^{\circ}C$; otherwise, $TiCo_{0.90}Fe_{0.10}$-SS composite had the highest pressure value among the membranes with the value of 10 atm. $TiCo_{0.55}Fe_{0.45}$-SS composite membrane was the best to separate the $H_2-N_2$ gas mixture excellently among the $TiCo_xFe_{1-x}$(x=0.50~1.00)-SS composite membranes since $TiCo_{0.55}Fe_{0.45}$ had the least hysteresis, and hydrogen permeation pressure was the lowest with value of 2.5 atm.

• Membrane Journal
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• v.25 no.2
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• pp.123-131
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• 2015

The PTMSP/PDMS graft copolymer were synthesized from the PTMSP[poly(1-trimethylsilyl-1-propyne)] and the PDMS[poly(dimethylsiloxane)] and then the PTMSP/PDMS-borosilicate composite membranes were prepared by adding the porous borosilicates to the PTMSP/PDMS graft copolymer. The number-average molecular weight (${\bar{M}}_n$) and the weight-average molecular weight (${\bar{M}}_w$) of PTMSP/PDMS graft copolymer were 460,000 and 570,000 respectively, and glass transition temperature ($T_g$) of PTMSP/PDMS graft copolymer appeared at $33.53^{\circ}C$ according to DSC analysis. According to the TGA measurements, the addition of borosilicate to the PTMSP/PDMS graft copolymer leaded the decreased weight loss and the completed weight loss temperature went down. SEM observation showed that borosilicate was dispersed in the PTMSP/PDMS-borosilicate composite membranes with the size of $1{\sim}5{\mu}m$. Gas permeation experiment indicated that the addition of borosilicate to PTMSP/PDMS graft copolymer resulted in the increase in free volume, cavity and porosity resulting in the gradual shift of the mechanism of the gas permeation from solution diffusion to molecular sieving surface diffusion, and Knudsen diffusion. Consequently, the permeability of $H_2$ and $N_2$ increased and selectivity ($H_2/N_2$) decreased as the contents of borosilicate increased.

• Membrane Journal
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• v.14 no.2
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• pp.99-107
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• 2004

Carbon molecular sieve (CMS) membranes were prepared by pyrolysis of polyimides having carboxylic acid groups and applied to the hydrogen separation. The polymeric membranes having carboxylic acid groups showed different steric properties as compared with polymeric membranes having other side groups ($-CH_3$ and $-CF_3$) because of the hydrogen bond between the carboxylic acid groups. However, the microporous CMS membranes were significantly affected by the decomposable side groups evidenced from the wide angle X-rat diffraction, nitrogen adsorption isotherms, and single gas permeation measurement. Furthermore, the gas separation properties of the CMS membranes were essentially affected by the pyrolysis temperature. As a result, the CMS membranes Prepared by Pyrolysis of polyimide containing carboxylic acid froups at $700^{\circ}C$ showed the $H_2$ permeability of 3,809 Baller [$1{\times}10^{-10}$ H $\textrm{cm}^$(STP)cm/$\textrm{cm}^2$.s.cmHg], $H_2$/$N_2$, selectivity of 46 and $H_2$/$CH_4$ selectivity of 130 while the CMS membranes derived from polyimide showed the H$_2$ permeability of 3,272 Barrer, $H_2$/$N_2$ selectivity of 136 and $H_2$/$CH_4$ selectivity of 177.

• Membrane Journal
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• v.23 no.5
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• pp.332-342
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• 2013

In the present study, carbon molecular sieve (CMS) hollow fiber membranes were prepared by carbonizing a methyl imide hollow fiber precursor, which was spun by non-solvent induced phase separation process. And effects of carbonization parameters such as pre-oxidation, pyrolysis, and post-oxidation on the gas permeation were systematically investigated. CMS membrane having the highest gas flux was obtained by carbonizing the precursor through a combined process of air pre-oxidation at $250^{\circ}C$ for 2h, nitrogen pyrolysis at $550^{\circ}C$ for 2h, and oxygen post-oxidation at $250^{\circ}C$ for 2h. The optimized membrane showed a considerable gas permeance : the $H_2$, He, $CO_2$ permeances were 69.72, 35.61, 31.01 GPU, respectively, and the $O_2$ and $N_2$ permeances were ignorable. Therefore, it was clear that the prepared CMS hollow fiber membrane was a promising membrane for recovering small gases such as hydrogen and hellium and carbon dioxide.

• Membrane Journal
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• v.14 no.4
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• pp.304-311
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• 2004

The poly(1-trimethylsilyl-1-propyne) (PTMSP) and silica-filled PTMSP membranes were prepared by casting from a toluene solution on porous polyetherimide (PEI). FT-IR spectrum, GPC and SEM pictures have been taken to characterize the membranes. The particle size of membrane decreases as silica content of the membrane increases from 23 to 60 wt%, and a uniform distribution of the silica is observed. The separation properties of the gas mixture (32 mol% $H_2$/ 68 mol% $N_2$) through the composite membranes were studies as a function of pressure and percentage of silica. Selectivity values of $H_2$/$N_2$ increased as the pressure of permeation cell and silica content of the membrane increased. The real separation factor($\alpha$), head separation factor($\beta$), and tail separation factor((equation omitted)) of PTMSP-PEI composite membrane were 2.28, 1.58, and 1.44 respectively at $\Delta$P 30 psi and $25^{\circ}C$. $\alpha$, $\beta$, and (equation omitted) of PTMSP-Silica-PEI composite membrane for 60 wt% silica were 3.34, 1.95, 1.72 at $\Delta$P 30 psi and $25^{\circ}C$.

• Korean Chemical Engineering Research
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• v.57 no.6
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• pp.768-773
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• 2019

The Fenton reaction, which evaluates the electrochemical durability of polymer membranes of polymer electrolyte fuel cells (PEMFC), and the degradation of polymer membranes by OCV holding method are compared. The Fenton reaction is a method that can evaluate the chemical durability of the polymer membrane at outside the cell in a shorter time than the OCV Holding method. The Fenton reaction was carried out at 30% hydrogen peroxide, 10 ppm iron, and $80^{\circ}C$ for 24 hours. OCV Holding was driven at $90^{\circ}C$, 30% relative humidity and OCV for 168 hours. The Fenton reaction caused a lot of degradation inside the polymer membrane. On the other hand, in OCV Holding, the membrane thickness was thinned by the entire surface and internal degradation. The fluorine emission rate was more than 10 times higher than that of OCV Holding due to the Fenton reaction. The hydrogen permeation rate increased about 30% at 24 hours of Fenton reaction. At OCV Holding, hydrogen permeability decreased after 24 hours and then increased. As a whole, there was a difference in a membranes deteriorated by Fenton reaction and OCV Holding.

• Membrane Journal
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• v.24 no.3
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• pp.177-184
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• 2014

Silica membranes with high permeability were prepared using colloidal and polymeric silica sols on a porous stainless steel-tube support by a DRFF and SRFF method. Silica sols were derived with tetraethylorthosilicate (TEOS) by sol-gel method and analyzed with DLS, FE-SEM, and $N_2$ adsorption. The coating of the intermediate layer with colloidal silica sol on the stainless steel-tube support led to a denser surface morphology of the membrane along with a considerable reduction in the number of surface defect. As the polymeric silica sol enclosed the colloidal silica sol with spherical particles during the SRFF method, the separation-layer-coated silica membrane showed a denser surface than the intermediate layer. Moreover, the silica membranes showed high hydrogen gas permeability of $(6.63-9.21){\times}10^{-5}mol{\cdot}m^{-2}{\cdot}s^{-1}{\cdot}Pa^{-1}$ with low $H_2/N_2$ perm-selectivity (2.9-3.1) at room temperatures.

• Transactions of the Korean hydrogen and new energy society
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• v.27 no.6
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• pp.660-669
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• 2016

A fluorinated-sulfonated, hydrophobic-hydrophilic copolymer was planed subsequently synthesized using typical nucleophilic substitution polycondensation reaction. A novel AB and ABA (or BAB) block copolymers were synthesized using sBCPSBP (sulfonated 4,4'-bis[4-chlorophenyl)sulfonyl]-1,1'-biphenyl), DHN (1,5-dihydroxynaphthalene), DFBP (decafluorobiphenyl) and HFIP (4,4'-hexafluoroisopropylidenediphenol). All block copolymers were easily cast and made into clear films. The structure and synthesized copolymers and corresponding membranes were analyzed using GPC (gel permeation chromatography), $^1H$-NMR ($^1H$ nuclear magnetic resonance) and FT-IR (Fourier transform infrared). TGA (Thermogravimetric analysis) and DSC (differential scanning calorimetry) analysis showed that the prepared membranes were thermally stable, so that elevated temperature fuel cell operation would be possible. Hydrophobic/hydrophilic phase separation and clear ionic aggregate block morpology was confirmed in both triblock and diblock copolymer in AFM (atomic force microscopy), which may be highly related to their proton transport ability. A sulfonated BAB triblock copolymer membrane with an ion-exchange capacity (IEC) of 0.6 meq/g has a maximum ion conductivity of 40.3 mS/cm at $90^{\circ}C$ and 100% relative humidity.

• Membrane Journal
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• v.23 no.4
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• pp.278-282
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• 2013

Zeolitic imidazolate frameworks (ZIFs) have been the focus of interest for their physical and chemical properties, especially, for their extraordinary gas separation properties. In this study, a novel and efficient method for the fabrication of continuous ZIF-7 film on ${\alpha}$-alumina substrate has been investigated. The electrospray deposition method was tried for the first time to prepare ZIF films directly without the necessity of prior substrate seeding. It has the advantage of depositing thin ZIF-7 films directly on the ${\alpha}$-alumina substrate by electrospraying the precursor solution. The ZIF-7 films have been characterized through XRD, FE-SEM, and single gas permeation tests.

• Membrane Journal
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• v.12 no.1
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• pp.51-53
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• 2002

The hydrogen ions in poly (vinyl alcohol) (PVA)/sulfosuccinic acid (SSA) membranes substiuted with $Li^+, Na^+, and K^+/ $of monvoalent metal ions, $Mg^{2+}, Ca^{2+} and Ba^{2+}$ of divalent metal ions, and $Al^{3+}$ of trivalent metal ion. In addition, $Li^+ ions were exchanged with varing reaction time. The effects of metal ions exchanged were investigated in terms of methanol permeability -uling diffusion cell. The methanol permeabilies decreased in the sequence of $Na^+, Li^+ and K^+$ and this might be due to the 'Salting-out' effect while the methanol permeabilities for divalent and trivalent ion-substituted membranes were affected by the combined effects of salting-out, eletrostatic crosslinking and extent of metal ion substiution. As for $Li^+$ ions, methanol permeabilities of PVA/SSA membranes decreased in proportion to the degrees of subsituted $Li^+$ ions.