• Korean Chemical Engineering Research
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• v.54 no.3
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• pp.305-309
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• 2016

Recently, there are many efforts focused on development of more economical non-fluorinated membranes for PEMFCs (Proton Exchange Membrane Fuel Cells). In this study, to test the durability of sPEEK MEA (Membrane and Electrode Assembly), ADT (Accelerated Degradation Test) of MEA degradation was done at the condition that membrane and electrode were degraded simultaneously. Before and after degradation, I-V polarization curve, hydrogen crossover, electrochemical surface area, membrane resistance and charge transfer resistance were measured. Although the permeability of hydrogen through sPEEK membrane was low, sPEEK membrane was weaker to radical evolved at low humidity and OCV condition than fluorinated membrane such as Nafion. Performance after MEA degradation for 144 hours and 271 hours were reduced by 15% and 65%, respectively. It was showed that the main cause of rapid decrease of performance after 144 hours was shorting due to Pt/C particles in the pinholes.

• Korean Chemical Engineering Research
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• v.55 no.3
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• pp.296-301
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• 2017

Recently, there are many efforts focused on development of more economical non-fluorinated membranes for PEMFCs (Proton Exchange Membrane Fuel Cells). In this study, sulfonated poly (ether ether ketone) (sPEEK) membrane reinforced with poly imide was made to enhance of membrane durability. In order to test durability of single (un-reinforced) membrane and reinforced membrane MEA (Membrane and Electrode Assembly), degradation accelerated stress test was used. Before and after degradation, I-V polarization curve, hydrogen crossover current, electrochemical surface area, membrane resistance and charge transfer resistance were measured. As a result of experiments, hydrogen crossover current of reinforced MEA was lower than that of single MEA, therefor durability of reinforced MEA was higher than that of single MEA. There was not especially short phenomena in reinforced MEA after degradation accelerated stress test.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.17 no.1
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• pp.433-440
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• 2016

Composite membranes were prepared by the solution casting method from sulfonated poly(etheretherketone)(sPEEK) and imidazole and phosphotungstic acid(PWA) to enhance the electrolytic properties of the membrane. TGA measurements showed that physical crosslinking due to acid-base interactions improved the thermal resistance to the desulfonation of sulfonic acid groups of the composite membrane and the addition of PWA enhanced the resistance to thermal decomposition of the composite membrane. The acid-base interaction decreased the water uptake, proton conductivity and methanol permeability of the sPEEK/imidazole composite membranes. The addition of PWA increased the proton conductivities while it decreased the water uptake and methanol permeability of sPEEK/imidazole/PWA composite membranes. Therefore, the selectivity of the composite membranes was enhanced by the addition of PWA.

• Korean Chemical Engineering Research
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• v.45 no.4
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• pp.391-395
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• 2007

A new electrode binder mixed with sulfonated poly (ether ether ketone) (sPEEK) and Nafion is prepared and investigated as an anode binder for direct methanol fuel cell (DMFC). The mixed binder (95 wt% sPEEK/5 wt% Nafion) shows high proton conductivity and methanol transport rate as well as no dissolution and brittleness. The effect of content as an anode binder on the performance of the cell with the given cathode is investigated. The unit cell with the anode containing 10wt% mixed binder showed the highest cell performance.

• Transactions of the Korean hydrogen and new energy society
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• v.28 no.1
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• pp.17-23
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• 2017

Polyether ether ketone (PEEK) composite including tungstophosphoric acid(TPA) membranes have been intensively investigated for polymer electrolyte membrane water electrolysis (PEMWE) and thus covalently linked sulfonated polyether ether ketone (CL-SPEEK) with captured TPA composite membranes were prepared and characterized. Sulfonated polyether ether ketone (SPEEK) was prepared in sulfonation of PEEK and was cross-linked with 1,4 diiodobutane. The carbonyl group of SPEEK was reduced with $NaBH_4$ and 3-isocyanatepropyltriethoxysilane (ICPTES) was added. The TPA captured composite was prepared in reaction of TPA with 3-mercaptopropyltrime thoxysilane (MPTMS). The polymer composite membranes showed better thermostability and electrochemical properties than SPEEK. The membranes were prepared by sol-gel casting method. The polymer composite membrane featured 0.1285 S/cm of proton conductivity at $80^{\circ}C$ and outstanding durability.

• Transactions of the Korean hydrogen and new energy society
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• v.27 no.5
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• pp.478-484
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• 2016

Polyether ether ketone (PEEK) composite membranes have been intensively investigated for polymer electrolyte membrane water electrolysis (PEMWE). Covalently linked (CL) sulfonated polyether ether ketone (SPEEK) and cellulose polymer composite membranes were prepared and characterized. Polyether ether ketone (PEEK) and cellulose were sulfonated and then were covalently linked by 1,4-diiodobutane to produce covalently linked SPEEK and cellulose polymer composite membranes. The composite membranes showed better thermostability and electrochemical properties than SPEEK. The membranes were prepared by sol-gel casting method. CL-SPEEK/Cellulose composite membrane featured 0.2453 S/cm of proton conductivity at $80^{\circ}C$ which was better than that of Nafion.

• Clean Technology
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• v.13 no.1 s.36
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• pp.79-84
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• 2007

Separation of ethylene from ethane and propylene from propane have been conducted using facilitated olefin transport membrane with SPEEK-Ag (Ag substituted sulfonated poly(ether ether ketone)). SPEEK was prepared by the sulfonation of PEEK using cone. $H_2SO_4$ and the reaction time affected the degree of sulfonation (DS) of the resulting SPEEK. SPEEK-Ag composite membrane was formed by soaking SPEEK in the polyester support into the Ag salt solution. With increasing the concentration of SPEEK in MeOH, the thickness of SPEEK on the polyester increased. The selectivity and the flux of SPEEK-Ag membrane for the separation of ethylene/ethane and propylene/propane were changed by the thickness of SPEEK layer on the top of polyester support. The anion of silver salt also affects the membrane performance.

• Transactions of the Korean hydrogen and new energy society
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• v.28 no.4
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• pp.338-344
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• 2017

Polyoxometal molybdophosphoric acid (MoPA) bonded polyether ether ketone (PEEK) composite membrane for water electrolysis has been investigated. The composited membrane, covalently cross linked (CL) sulfonated polyether ether ketone (SPEEK) with a bonded MoPA, was prepared in sulfonation of PEEK, cross linkage reaction with 1,4-diiodobutane, and addition with MoPA. PEEK was covalently cross-linked with 1,4-diiodobutane to improve mechanical strength and was added with MoPA to increase proton conductivity. MoPA should be fixed to back bone of SPEEK to prevent bleeding out. Therefore, the carbonyl group of SPEEK was reduced with NaBH4 and 3-isocyanatepropyltriethoxysilane (ICPTES) was added. The MoPA bonded composite was produced in the reaction of MoPA with 3-mercaptopropyltrimethoxvsilane (MPTMS). In conclusion, MoPA bonded CL-SPEEK composite membrane featured 0.129 S/cm of proton conductivity at $80^{\circ}C$, and 2,156 hours of chemical stability in Fenton test. These properties are better than those of membranes of other SPEEK system.

• Transactions of the Korean hydrogen and new energy society
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• v.17 no.2
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• pp.149-157
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• 2006

Hydrogen as new energy sources is highly efficient and have very low environmental emissions. The proton exchange membrane fuel cell (PEMFC) is an emerging technology that can meet these demands. Therefore, the preparation of stable polymeric membranes with good proton conductivity and durability are very important for hydrogen production via water electrolysis with PEM at medium temperature above $80^{\circ}C$. Currently Nafion of Dupont and Aciflex of Asahi, etc., solid polymer electrolytes of perfluorosulfonic acid membrane, are the best performing commercially available polymer electrolytes. However, these membrane have several flaws including its high cost, and its limited operational temperature above $80^{\circ}C$. Because of this, significant research efforts have been devoted to the development of newer and cheaper membranes. In order to make up for the weak points and to improve the mechanical characteristics with cross -linking, acid-base complexes were prepared by the combination PSf-co-PPSS-$NH_2$ with PEEK-$SO_3H$. The results showed that the proton conductivity decreased in 17.6% and 40% but tensile strength increased in 78% and 98%, about $20.65\;{\times}\;10^6N/m^2$, in comparison with SBPSf/HPA and SPEEK/HPA complex membrane.

• Polymer(Korea)
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• v.36 no.2
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• pp.155-162
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• 2012

Sulfonated poly(ether ether ketone) (SPEEK) nanofibers were prepared by electrospinning. The nanofibrous membrane for polymer electrolyte membrane fuel cell (PEMFC) was fabricated by compression molding. The maximum degree of sulfonation was 95% and the initial thermal degradation temperature was $280^{\circ}C$ and it's value was lower than that of PEEK. The contact angle of SPEEK increased with decreasing the degree of sulfonation. The optimum voltage, flow rate, tip to collector distance (TCD) and concentration of electrospinning conditions were 22 kV, 0.3 mL/hr, 15 cm, and 23 wt%, respectively. The average nanofibrous diameter was 47.6 nm. The water uptake and ion exchange capacity of SPEEK nanofibrous membrane increased with increasing the sulfonation time and the amount of sulfonating agent. The electrical resistance and proton ionic conductivity of SPEEK membrane increased with decreasing and increasing the sulfonation time, respectively. Their values were 0.58~0.06 ${\Omega}{\cdot}cm^2$and 0.099 S/cm.