• Journal of Hydrogen and New Energy
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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.

• Journal of Hydrogen and New Energy
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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.

• 한국전기화학회:학술대회논문집
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• 2005.07a
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• pp.83-86
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• 2005

• Journal of Hydrogen and New Energy
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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.

• 한국신재생에너지학회:학술대회논문집
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• 2010.11a
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• pp.85.2-85.2
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• 2010

There is widespread effort to develop polymer membranes in place of Nafion for high temperature polymer electrolyte membrane fuel cell(PEMFC). In our study, SiO2 membranes are arranged by electrospinning method. For impregnation solution, the modified sulfonated poly(ether ether ketone)(SPEEK) polymer is prepared from sulfonation, sulfochlorination, partial reduction and lithiation reaction. The modified polymer is cross-linked with 1,4-diiodobetane in NMP solvent and then blended with Heteropoly acid(HPA). The characterization of membranes is confimed by FT-IR, Thermogravimetry(TGA), water uptake test and single cell performance test for PEMFC, etc. The composite membrane shows satisfactory thermal and mechanical properties. Beside, The membrane exhibits good ion exchange capacity and high proton conductivity. As a result, The composite membrane is promising as an alternative membrane in high temperature PEMFC.

• Proceedings of the Membrane Society of Korea Conference
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• 2005.05a
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• pp.144-147
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• 2005

• Journal of Hydrogen and New Energy
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• v.28 no.5
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• pp.433-439
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• 2017

The high temperature performance of PEM type electrolyser at $120^{\circ}C$ based on covalently cross-linked sulfonated poly ether ether ketone (SPEEK) composie membrane was investigated. Ion conductivity and other properties of SPEEK membrane were improved by adding heteropoly acid and Ceria. The membrane electrode assemblies were prepared using commercial PtC and nano-sized $IrRuO_2$ catalyst by electro-spraying and decal process. Voltage efficiency of MEA equipped with SPEEK membrane was slightly better than that of $Nafion^{(R)}$ membrane, due to its higher proton conductivity at high temperature. The cell performance of MEA with CL-SPEEK/Cs-TSiA/Ceria is 1.71 V at $1A/cm^2$ and $120^{\circ}C$.

• Journal of Hydrogen and New Energy
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• v.29 no.5
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• pp.411-418
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• 2018

The polymer electrolyte membranes, CL-SPEEK/Cellulose composite membrane I, II, III with the improved electrochemical and mechanical properties were prepared and characterized. The engineering plastic polyether ether ketone (PEEK) and cellulose were sulfonated and cross-linked. The membranes were prepared by sol-gel casting method with different amount of cross-linking reagent. In conclusion, the composite membranes I, II, III showed improved thermostability, tensile strength and oxidative durability. Proton conductivity of the membranes was also improved and the composite membrane I showed 0.1312 S/cm at $80^{\circ}C$ which was the best of those composite membranes.

• Journal of Hydrogen and New Energy
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• v.20 no.3
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• pp.194-201
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• 2009

The e1ectrocatalytic properties of heteropolyacids(HPAs) entrapped in covalently cross-linked sulfonated polyetheretherketone(CL-SPEEK/HPA) membranes have been studied for water electrolysis. The HPAs, including tungstophosphoric acid(TPA), molybdophosphoric acid(MoPA), and tungstosilicic acid(TSiA) were used as additives in the composite membranes. The MEA was prepared by a non-equilibrium impregnation-reduction(I-R) method, using reducing agent, sodium borohydride(NaBH4) and tetraamineplatinum(II) chloride(pt(NH$_3$)$_4$Cl$_2$). The electrocatalytic properties of composite membranes such as the cell voltage were in the order of magnitude CL-SPEEKlMoPA40 (wt%) > /TPA30 > /TSiA40. In the optimum cell applications for water electrolysis, the cell voltage of PtlPEM/Pt-Ru MEA with CL-SPEEKlTPA30 membrane was 1.75 V at 80$^{\circ}$C and I A/cm$^2$ and this voltage carried lower than that of 1.81 V of Nafion 117. Consequently, in regards of electrochemical and mechanical characteristics and oxidation durability, the newly developed CL-SPEEKITPA30 composite membrane exhibited a better performance than the others, but CLSPEEKlMoPA40 showed the best electrocatalytic activity (1.71 Vat 80$^{\circ}$C and 1 A/cm$^2$) among the composite membranes.

• Journal of Hydrogen and New Energy
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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.