• Korean Chemical Engineering Research
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• v.62 no.1
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• pp.13-18
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• 2024

To develop flexible electrode materials for wearable devices, we investigated the electrochemical characteristics of carbon fibers tow according to pretreatment. And an electrochemical non-enzymatic sensor was fabricated using glucose as a target. The carbon fibers tow was pretreated through desizing and activation processes, and activation was performed in two ways: chemical oxidation and electrochemical oxidation. Surface morphology of carbon fibers tow samples was observed by SEM and their electrochemical characteristics and sensing performance were investigated by cyclic voltammetry, electrochemical impedance spectroscopy and chronoamperometry. Carbon fibers tow samples showed improved electrochemical properties such as reduced R_et, ΔE_p, and increased I_p through pretreatment. And similar electrochemical properties were obtained with both activation methods. We selected electrochemically activated carbon fibers tow as the final electrode material for application of electrochemical sensor. The non-enzymatic glucose sensor based on this electrode has an enhanced sensitivity of 0.744 A/mM (in a linear range of 0.09899~3.75423 mM) and 0.330 mA/mM (3.75423~50 mM), respectively. Through this study, the possibility of using carbon fibers tow was confirmed as an electrode material. It is expected to be used as basic research for development of high-performance flexible electrode materials.

• Korean Chemical Engineering Research
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• v.62 no.2
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• pp.147-152
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• 2024

Most medical sensors are disposable products. In order to reduce inspection and diagnosis costs, it is more important to develop the inexpensive electrode materials. We fabricated the CuO NPs/PANI/E-PGE as an electrode material for disposable electrochemical sensors and applied it to a non-enzymatic glucose sensor. For surface activation of PGE, pretreatment was performed using chemical and electrochemical methods, respectively. Electrochemical properties according to the pretreatment method were analyzed through chronoamperometry (CA), cyclic voltammetry (CV) and electrochemical impedance (EIS). From these analytical results, the electrochemically pretreated PGE (E-PGE) was finally adopted. The non-enzymatic glucose sensor based on CuO NPs/PANI/E-PGE shows sensitivity of 239.18 mA/mM×cm² (in a linear range of 0.282~2.112 mM) and 36.99 mA/mM×cm² (3.75423~50 mM), detection limit of 17.6 μM and good selectivity. Based on the results of this study, it was confirmed that the modified PGE is a high-performance electrode material. Therefore, these electrodes can be applied to a variety of disposable sensors.

• Analytical Science and Technology
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• v.11 no.5
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• pp.347-352
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• 1998

A study was carried out on the elelctrochemical characteristics of chemically modified electrodes (CMEs) by cyclic voltammetry. Fabrication of CMEs was made by coating with mixed valence (mv) inorganic-metal polymeric films on the glassy carbon electrode surface by potential cycling. Anodic oxidation behavior of methanol and L-ascorbic acid was studied by using CMEs working electrode. Deposition of films such as mv ruthenium oxo/ruthenium cyanide film (mv Ru-O/CN-Ru), mv ruthenium oxo/ferrocyanide film (mv Ru-O/$Fe(CN)_6$), and mv ruthenium oxo/ruthenium cyanide/Rhodium film (mv Ru-O/CN-Ru/Rh) was obtained to coat by scan rate of 50 mV/sec within the specified potential range (-0.5V ~ +1.2V). Film thickness was controlled by the repeat of the potential cycling. Anodic oxidation behavior of methanol was as follow. Calibration graph by using mv Ru-O/CN-Ru film showed linearly from 10 mM to 80 mM MeOH with slope factor of $-7.552{\mu}A/cm^2$. Although slope factor by using mv Ru-O/$Fe(CN)_6$ film was $-5.13{\mu}A/cm^2$, yet linear range of calibration graph could be extended from 10 mM to 100 mM MeOH. Anodic oxidation behavior of L-ascorbic acid was studied by mv Ru-O/CN-Ru film on the glassy carbon electrode and the glassy carbon electrode with Rh film, Glassy carbon electrode modified with Ru polymeric film was showed better sensitivity than the Rh-glassy carbon modified electrode (mv Ru-O/CN-Ru/Rh). Calibration graph was linear from 0.1 mM to 5 mM L-ascorbic acid by using glassy carbon electrode modified with Ru polymeric film. Solpe factor and relative coefficient are $-84.78{\mu}A/mM$ and 0.998, respectively.

• Applied Chemistry for Engineering
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• v.25 no.1
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• pp.78-83
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• 2014

In this research, we evaluated the performance and characteristics of carbon supported PtM (M = Ni and Y) alloy catalysts (PtM/Cs) synthesized by a modified polyol method. With the PtM/Cs employed as a catalyst for the oxygen reduction reaction (ORR) of cathodes in proton exchange membrane fuel cells (PEMFCs), their catalytic and ORR activities and electrical performance were investigated and compared with those of commercial Pt/C. Their particle sizes, particle distributions and electrochemically active surface areas (EAS) were measured by TEM and cyclic voltammetry (CV), while their ORR activity and electrical performance were explored using linear sweeping voltammetries with rotating disk electrodes and rotating ring-disk electrodes as well as PEMFC single cell tests. TEM and CV measurements show that PtM/Cs have the compatible particle size and EAS with Pt/C. When it comes to ORR activity, PtM/C showed the equivalent or better half-wave potential, kinetic current density, transferred electron number per oxygen molecule and $H_2O_2$ production(%) to or than commerical Pt/C. Based on results gained by the three electrode tests, when the PEMFC single cell tests were carried out, the current density measured at 0.6 V and maximum power density of PEMFC single cell adopting PtM/C catalysts were better than those adopting Pt/C catalyst. It is therefore concluded that PtM/C catalysts synthesized by modified polyol can result in the equivalent or better ORR catalytic capability and PEMFC performance to or than commercial Pt/C catalyst.

• Applied Chemistry for Engineering
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• v.19 no.3
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• pp.299-303
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• 2008

A thermally cross-linkable polymer, poly[(2,5-dimethoxy-1,4-phenylenevinylene)-alt-(1,4-phenylenevinylene)] (Cross-PPV), was synthesized by the Heck coupling reaction. In order for the polymer to be cross-linkable, 20 mol% excess divinylbenzene was added. The chemical structure of Cross-PPV and thermally crosslinked Cross-PPV were confirmed by FT-IR spectroscopy. From the FT-IR, UV-Vis, and PL spectral data, thermally crosslinked Cross-PPV was insoluble in common organic solvents. The HOMO and LUMO energy level of thermally cross-linked Cross-PPV were estimated -5.11 and -2.56 eV, respectively, which were determined by the cyclic voltammetry and UV-Vis spectroscopy. From the energy level data, one can easily notice that thermally crosslinked Cross-PPV can be used for hole injection layer effectively. Bilayer structured device (ITO/crosslinked Cross-PPV/PM-PPV/Al) was fabricated using poly(1,4-phenylenevinylene-(4-dicyanomethylene-4H-pyran)-2,6-vinylene-1,4-phenylenevinylene-2,5-bis(dodecyloxy)-1,4-phenylenevinylene (PM-PPV) as the emitting layer, which have HOMO and LUMO energy levels of -5.44 eV and -3.48 eV, respectively. The bilayered device had much enhanced the maximum efficiency (0.024 cd/A) and luminescence ($45cd/m^2$) than those of a single layer device (ITO/PM-PPV/Al, 0.003 cd/A, $3cd/m^2$). The enhanced performance originated from that fact that cross-linked Cross-PPV facilitatse the hole injection to the emissive layer and the injected hole and electron from ITO and Al are recombined in emitting layer (PM-PPV) effectively.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.18 no.4
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• pp.1-7
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• 2017

Cobalt silicide was used as a counter electrode in order to confirm its reliability in dye-sensitized solar cell (DSSC) devices. 100 nm-Co/300 nm-Si/quartz was formed by an evaporator and cobalt silicide was formed by vacuum heat treatment at $700^{\circ}C$ for 60 min to form approximately 350 nm-CoSi. This process was followed by etching in $80^{\circ}C$-30% $H_2SO_4$ to remove the cobalt residue on the cobalt silicide surface. Also, for the comparison against Pt, we prepared a 100 nm-Pt/glass counter electrode. Cobalt silicide was used for the counter electrode in order to confirm its reliability in DSSC devices and maintained for 0, 168, 336, 504, 672, and 840 hours at $80^{\circ}C$. The photovoltaic properties of the DSSCs employing cobalt silicide were confirmed by using a simulator and potentiostat. Cyclic-voltammetry, field emission scanning electron microscopy, focused ion beam scanning electron microscopy, and energy dispersive spectrometry analyses were used to confirm the catalytic activity, microstructure, and composition, respectively. The energy conversion efficiency (ECE) as a function of time and ECE of the DSSC with Pt and CoSi counter electrodes were maintained for 504 hours. However, after 672 hours, the ECEs decreased to a half of their initial values. The results of the catalytic activity analysis showed that the catalytic activities of the Pt and CoSi counter electrodes decreased to 64% and 57% of their initial values, respectively(after 840 hours). The microstructure analysis showed that the CoSi layer improved the durability in the electrolyte, but because the stress concentrates on the contact surface between the lower quartz substrate and the CoSi layer, cracks are formed locally and flaking occurs. Thus, deterioration occurs due to the residual stress built up during the silicidation of the CoSi counter electrode, so it is necessary to take measures against these residual stresses, in order to ensure the reliability of the electrode.

• Journal of the Korean Chemical Society
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• v.36 no.2
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• pp.261-272
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• 1992

Tetradentate Schiff base Cobalt(II)(3MeOSED)$(H_2O)_2$ complexe was synthesized and allowed to react with dry oxygen to form oxygen adducts of Cobalt(III) complexes such as ${\mu}$-peroxo type [Co(III)(3MeOSED)(DMF)]$_2O_2$ and [Co(III)(3MeOSED)(DMSO)]$_2O_2$in DMF and DMSO or superoxo type [Co(III)(3MeOSED)(Py)]$O_2$ in pyridine. The oxygen adducted complex was investigated by cyclic voltammetry and DPP method with glassy carbon electrode in 0.1M TEAP-DMF (-DMSO,-Py) as supporting electrolyte solution. As a result the reduction reaction process occurred to four steps including prewave Of $O_2^-$in 1 : 1 oxygen adducted superoxo type [Co(III)(3MeOSED)(Py)]$O_2$complex and three steps not including prewave of $O_2^-$ in 1 : 2 oxygen adducted ${\mu}$-peroxo type [Co(III)-(3MeOSED)(DMF)]$_2O_2$ and [Co(III)(3MeOSED)(DMSO)]$_2O_2$. A superoxo type [Co(III)(3MeOSED)(L)]$O_2\;(L: CH_3OH)$ was generated with oxygen in methanol. Selectively oxidized hydrazobenzene $(H_2AB)$ to trans-azobenzene(t-AB) and the rate constant k for oxidation reaction of the following equation is $(2.96 {\pm} 0.2)$${\times}$ $10^{-1}$M/sec. $H_2AB$ + Co (II)(3MeOSED)$(L_2)+O_2\;{\rightleftarrow^K}$ [Co(III)(3MeOSED)(L)]$O_2{\cdot}H_2AB{\longrightarrow^K}$ Co(II(3MeOSED)$(L)_2$+t-AB+$H_2O_2 $.

• Korean Chemical Engineering Research
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• v.57 no.6
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• pp.868-873
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• 2019

In this study, the evaluation of performance of AORFB using methyl viologen and TEMPOL as organic active materials in neutral supporting electrolyte (NaCl) with various membrane types was performed. Using methyl viologen and TEMPOL as active materials in neutral electrolyte solution, the cell voltage is 1.37V which is relatively high value for AORFB. Two types of membranes were examined for performance comparison. First, when using Nafion 117 membrane which is commercial cation exchange membrane, only the charge process occurred in the first cycle and the single cell couldn't work because of its high resistance. However, when using Fumasep anion exchange membrane (FAA-3-50) instead of Nafion 117 membrane, the result was obtained as the totally different charge-discharge graphs. When current density was $40mA{\cdot}cm^{-2}$ and cut off voltage range was from 0.55 V to 1.7 V, the charge efficiency (CE) was 97% and voltage efficiency (VE) was 78%. In addition, the discharge capacity was $1.44Ah{\cdot}L^{-1}$ which was 54% of theoretical capacity ($2.68Ah{\cdot}L^{-1}$) at $10^{th}$ cycle and the capacity loss rate was $0.0015Ah{\cdot}L^{-1}$ per cycle during 50 cycles. Through cyclic voltammetry test, it seems that this difference in the performance between the full cell using Nafion 117 membrane and Fumasep anion exchange membrane came from increasing resistance due to chemical reaction between membrane and active material, not the capacity loss due to cross-over of active material through membrane.

• Korean Chemical Engineering Research
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• v.60 no.4
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• pp.588-593
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• 2022

Terephthalaldehyde (TPA) is introduced as a cross liker to enhance electron transfer of hemin-based cathodic catalyst consisting of polyethyleneimine (PEI), carbon nanotube (CNT) for hydrogen peroxide reduction reaction (HPRR). In the cyclic voltammetry (CV) test with 10 mM H₂O₂ in phosphate buffer solution (pH 7.4), the current density for HPRR of the suggested catalyst (CNT/PEI/hemin/PEI/TPA) shows 0.2813 mA cm^-2 (at 0.2 V vs. Ag/AgCl), which is 2.43 and 1.87 times of non-cross-linked (CNT/PEI/hemin/PEI) and conventional cross liker (glutaraldehyde, GA) used catalyst (CNT/PEI/hemin/PEI/GA), respectively. In the case of onset potential for HPRR, that of CNT/PEI/hemin/PEI/TPA is observed at 0.544 V, while those of CNT/PEI/hemin/PEI and CNT/PEI/hemin/PEI/GA are 0.511 and 0.471 V, respectively. These results indicate that TPA plays a role in facilitating electron transfer between the electrodes and substrates due to the π-conjugated cross-linking bonds, whereas conventional GA cross-linker increases the overpotential by interrupting electron and mass transfer. Electrochemical impedance spectroscopy (EIS) results also display the same tendency. The charge transfer resistance (R_ct) of CNT/PEI/hemin/PEI/TPA decreases about 6.2% from that of CNT/PEI/hemin/PEI, while CNT/PEI/hemin/PEI/GA shows the highest R_ct. The polarization curve using each catalyst also supports the superiority of TPA cross liker. The maximum power density of CNT/PEI/hemin/PEI/TPA (36.34±1.41 μWcm^-2) is significantly higher than those of CNT/PEI/hemin/PEI (27.87±0.95 μWcm^-2) and CNT/PEI/hemin/PEI/GA (25.57±1.32 μWcm^-2), demonstrating again that the cathode using TPA has the best performance in HPRR.