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A novel synthesis of (3,6-bis(2,3-dihydrothieno[3,4-b][1,4]dioxin-5-yl)-9-(4-vinylbenzyl)-9H-carbazole), alternating polymer formation, characterization, and capacitance measurements
(Springer, 2013) Ateş, Murat; Uludağ, Nesimi; Karazehir, Tolga; Arican, Fatih
In this work, (3,6-bis(2,3-dihydrothieno[3,4-b][1,4]dioxin-5-yl)-9-(4-vinylbenzyl)-9H-carbazole) (EDOTVBCz) comonomer was chemically synthesized and characterized by Fourier transform infrared (FTIR), proton nuclear magnetic resonance, and carbon nuclear magnetic resonance spectroscopy. EDOTVBCz was electrocoated on glassy carbon electrode (GCE) in various initial molar concentrations ([EDOTVBCz](0) = 1.0, 1.5, 2.0, and 3.0) in 0.1 M lithium perchlorate (LiClO4)/acetonitrile (CH3CN). P(EDOTVBCz)/GCE was characterized by cyclic voltammetry, FTIR reflectance-attenuated total reflection spectroscopy, scanning electron microscopy-energy dispersive X-ray analysis, atomic force microscopy, and electrochemical impedance spectroscopy (EIS). EIS was used to determine the capacitive behaviors of modified GCE via Nyquist, Bode magnitude, Bode phase, and admittance plots. The highest low-frequency capacitance value was obtained as C (LF) = similar to 2.35 mF cm(-2) for [EDOTVBCz](0) = 3.0 mM. Double-layer capacitance of the polymer/electrolyte system was calculated as C (dl) = similar to 2.78 mF cm(-2) for [EDOTVBCz](0) = 1.0 and 3.0 mM. The maximum phase angle was obtained as theta = similar to 76.7(o) for [EDOTVBCz](0) = 1.0, 1.5, 2.0, and 3.0 mM at the frequency of 20.6 Hz. AC impedance spectra of P(EDOTVBCz)/LiClO4/CH3CN was obtained by performing electrical equivalent circuit model of R(Q(R(CR))) with linear Kramers-Kronig test.
A novel synthesis of 3,6-bis(2,3-dihydrothieno[3,4-b][1,4]dioxin-5-yl)-9-tosyl-9H-carbazole
(Ovidius Univ Press, 2012) Ateş, Murat; Uludağ, Nesimi; Karazehir, Tolga; Arican, Fatih
3,6-bis(2,3-dihydrothieno [3,4-b][1,4]dioxin-5-yl)-9-tosyl-9H-carbazole (EDOTTsCz) was synthesized and electrochemically polymerized on glassy carbon electrode (GCE) in 0.1 M tetrabutyl ammonium tetrafluoroborate (NB4BF4)/acetonitrile (CH3CN). Alternating copolymer was formed by CV method. Modified polymer electrode was characterized by Fourier transform Infrared Spectroscopy-Attenuated Transmission Reflectance (FTIR-ATR), Cyclic voltammetry (CV), Scanning electron microscopy-Energy dispersive X-ray analysis (SEM-EDX), Atomic force microscope (AFM) and Electrochemical impedance spectroscopy (EIS). Capacitive behaviors of the modified GCE were defined via Nyquist, Bode-magnitude, Bode-phase and Capacitance plots. A modified copolymer electrode provides enhanced capacitance evaluation, which may results in performance in energy storage devices.
A novel synthesis of 4-toluene 9H-carbazole-9-carbodithioate, electropolymerization and impedance study
(Budapest Univ Technol & Econ, 2014) Ateş, Murat; Uludağ, Nesimi; Karazehir, Tolga; Arican, Fatih
A novel synthesis of 4-toluene 9H-carbazole-9-carbodithioate (TCzC) was chemically synthesized and characterized by Fourier Transform Infrared (FTIR), proton nuclear magnetic resonance (H-1-NMR), and carbon nuclear magnetic resonance (C-13-NMR) spectroscopies. Specific (C-sp) and double layer capacitances (C-dl) of the electro-coated poly(carbazole) and poly(TCzC) films were obtained on glassy carbon electrode (GCE) by impedimetric method with DC potential from -0.1 to + 1.0 V by increasing potential of 0.2 V. The polymers were characterized by Cyclic voltammetry (CV), Fourier transform infrared reflectance-attenuated total reflection spectroscopy (FTIR-ATR), Atomic force microscopy (AFM), and Electrochemical impedance spectroscopy (EIS). The use of additional variable (DC potential) helped to disambiguate the equivalent circuit model of R(C(R(Q(RW))))(CR). Simulation results were compared with experimental data. In this study, substituted group effects of CS2 and tosyl on carbazole polymer were investigated by EIS technique. CS2 group together with tosyl group in the structure of carbazole decreased the specific capacitance value (C-sp = 0.43 mF cm(-2)) compared to PCz (C-sp = 1.44 mF cm(-2)). Electropolymerization formation was seriously affected by substituted groups of CS2 and tosyl on conjugation system because of the electron donor and acceptor ability.
Comparison of electrolyte effects for poly(3,4-ethylenedioxythiophene) and poly(3-octylthiophene) by electrochemical impedance spectroscopy and polymerization parameters with morphological analyses on coated films
(Springer, 2013) Ateş, Murat; Karazehir, Tolga; Arican, Fatih; Eren, Nuri
3,4-Ethylenedioxythiophene and 3-octylthiophene were electropolymerized on glassy carbon electrodes (GCE) to compare with four different electrolytes [lithium perchlorate (LiClO4), sodium perchlorate, tetraethylammonium tetrafluoroborate, and tetrabutylammonium tetrafluoroborate] in a solvent of acetonitrile (CH3CN). Modified electrodes were characterized by cyclic voltammetry, attenuated total reflectance-Fourier transform IR spectroscopy, scanning electron microscopy, energy dispersive X-ray analysis, atomic force microscopy, and electrochemical impedance spectroscopy (EIS). Nyquist and Bode plots for magnitude, phase, admittance, and capacitance on both polymer-modified electrodes were comparatively investigated in detail. The highest low-frequency capacitance (C (LF)) and double-layer capacitance (C (dl)) were obtained in 0.1 M LiClO4/CH3CN for poly(3,4-ethylenedioxythiophene) and poly(octylthiophene)/GCE. EIS data were fitted to the equivalent circuit model of R(Q(R(C(R(C(RW))))))(CR), which is used to investigate circuit parameters.
Copolymer formation of 4-vinylbenzyl-9H-carbazole-9-carbodithioate and ethylenedioxythiophene and capacitive behavior
(Sage Publications Ltd, 2014) Ateş, Murat; Uludağ, Nesimi; Arican, Fatih
In this study, first, a new monomer of 4-vinylbenzyl 9H-carbazole-9-carbodithioate (VBzCzCT) was chemically synthesized and characterized using Fourier transform infrared (FTIR) reflectance, proton nuclear magnetic resonance (1 H NMR), and carbon nuclear magnetic resonance (C-13 NMR) spectroscopies. Second, VBzCzCT and 3,4-ethylenedioxythiophene (EDOT) monomers were electrocopolymerized (VBzCzCT-co-EDOT) in 0.1 M sodium perchlorate (NaClO4)/acetonitrile ((CHCN)-C-3) on glassy carbon electrode (GCE) using cyclic voltammetry (CV). Third, the best deposition conditions on the electroactivity of the modified homopolymers and copolymer were studied and characterized using different techniques such as CV, FTIR-attenuated total reflectance, scanning electron microscopyenergy dispersion x-ray analysis, and electrochemical impedance spectroscopy (EIS) analysis. The specific capacitance (C-sp) of poly(VBzCzCT) (P(VBzCzCT)) was obtained as 20.5 mF cm(-2). However, the C-sp of P(VBzCzCT-co-EDOT)/GCE was obtained as 45.5 mF cm(-2). There is an important improvement in the capacitance value of copolymer formation. The C-sp value increases more than twice from P(VBzCzCT) to copolymer. The highest double layer capacitance (C-dl approximately 27.5 mF cm(-2)) was obtained for P(VBzCzCT-co-EDOT) and P(EDOT) compared with P(VBzCzCT) (C-dl approximately 8.28 mF cm(-2). Finally, simulation graphs of Nyquist, Bode-magnitude, and Bode-phase plots were given for homopolymers and copolymer for the electrical equivalent circuit model of R-s(Q(1)(R-1(C-1(R-2(C-2(R-3.W))))))(C3R4). The EIS results of P(VBzCzCT), P(EDOT), and P(VBzCzCT-co-EDOT) might be studied as promising active electrode materials for (super) capacitor evaluations.
Electrochemical copolymerization of N-methylpyrrole and 2,2 '-bithitiophene; characterization, micro-capacitor study, and equivalent circuit model evaluation
(Indian Acad Sciences, 2013) Ateş, Murat; Arican, Fatih; Karazehir, Tolga
N-methylpyrrole (N-MPy) and 2,2'-bithiophene (BTh) were electrocopolymerized in 0 center dot 2 M acetonitrile-sodium perchlorate solvent-electrolyte couple on a glassy carbon electrode (GCE) by cyclic voltammetry (CV). The resulting homopolymers and copolymers in different initial feed ratios of [N-MPy](0)/[BTh](0) = 1/1, 1/2, 1/5 and 1/10 were characterized by CV, Fourier-transform infrared reflectance attenuated transmittance (FTIR-ATR), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX) and electrochemical impedance spectroscopy (EIS). The capacitive behaviours of the modified electrodes were defined via Nyquist, Bode-magnitude, Bode-phase and admittance plots. The equivalent circuit model of R(C(R)(QR)(CR)) was performed to fit theoretical and experimental data. The highest low-frequency capacitance (C (LF)) were obtained as C (LF) = similar to 1 center dot 23 x 10 (-4) mF cm (-2) for P(N-MPy), C (LF) = similar to 2 center dot 09 x 10 (-4) mF cm(-2) for P(BTh) and C (LF) = similar to 5 center dot 54 x 10 (-4) mF cm(-2) for copolymer in the inital feed ratio of [N-MPy](0)/[BTh] (0) = 1/2.
Electrocoated Films of Poly(N-Methylpyrrole-co-2,2 '-Bithitiophene-co-3-(Octylthiophene)), Characterizations, and Capacitor Study
(Taylor & Francis As, 2015) Ateş, Murat; Arican, Fatih
N-Methylpyrrole (N-MPy), 2,2 '-bithiophene (BTh), and 3-(Octylthiophene) (OTh) were electrocopolymerized in 0.2M NaClO4/CH3CN on glassy carbon electrode (GCE). The resulting terpolymers of N-MPy, BTh and OTh in different initial monomer feed ratios such as [N-MPy](0)/[BTh](0)/[OTh](0)=1/1/1 and 1/2/5 were characterized by cyclic voltammetry (CV), Fourier-transform infrared attenuated total reflectance spectroscopy (FTIR-ATR), scanning electron microscopy (SEM), energy-dispersive X-ray analysis (EDX), and electrochemical impedance spectroscopy (EIS). The capacitive behaviors of the modified electrodes were defined via Nyquist, Bode-magnitude, Bode-phase, and Admittance plots. The equivalent circuit model of Rs(C ( dl1 )(R ( 1 )(QR ( 2 ))))(C ( dl2 ) R ( 3 )) was performed to fit the theoretical and experimental data. The low-frequency capacitance (C-LF) were obtained from initial monomer concentrations of 50mM as C-LF=similar to 2.34x10(-4) mFcm(-2) for P(N-MPy), C-LF=5.06x10(-4) mFcm(-2) for P(BTh), C-LF=5.07 mFcm(-2) for P(OTh), and C-LF=similar to 3.78 m Fcm(-2) for terpolymer for [N-MPy](0)/[BTh](0)/[OTh](0)=1/1/1. The terpolymer may be used as energy storage devices. [GRAPHICS]
Electrolyte type and concentration effects on poly(3-(2-aminoethyl thiophene) electro-coated on glassy carbon electrode via impedimetric study
(Springer, 2013) Ateş, Murat; Karazehir, Tolga; Arican, Fatih; Eren, Nuri
In this study, 3-(2-Aminoethyl thiophene) (2AET) monomer was electropolymerized on glassy carbon electrode (GCE) using various electrolytes (lithium perchlorate (LiClO4), sodium perchlorate (NaClO4), tetrabutyl ammonium tetra fluoroborate (TBABF(4)) and tetraethyl ammonium tetra fluoroborate (TEABF(4)) in acetonitrile (CH3CN) as solvent. Poly(3-(2-aminoethyl thiophene) (P(2AET))/GCE was characterized by cyclic voltammetry (CV), Fourier transform infrared reflectance spectrophotometry (FTIR-ATR), scanning electron microscopy, energy dispersive X-ray analysis (EDX), and electrochemical impedance spectroscopy (EIS) techniques. The electrochemical impedance spectroscopic results were given by Nyquist, Bode-magnitude, Bode-phase, capacitance and admittance plots. The highest low frequency capacitance (C-LF) value obtained was 0.65 mF cm(-2) in 0.1 M LiClO4/CH3CN for the initial monomer concentration of 1.5 mM. The highest double layer capacitance (C-dl = similar to 0.63 mF cm(-2)) was obtained in 0.1 M LiClO4/ACN for [2AET](0) = 0.5, 1.0 and 1.5 mM. The maximum phase angles (theta = 76.1 degrees at 26.57 Hz) and conductivity (Y '' = 3.5 mS) were obtained in TEABF(4)/ACN for [2AET](0) = 0.5 and 1.0 mM, respectively. An equivalent circuit model of R(Q(R(Q(R(CR))))) was simulated for different electrolytes (LiClO4, NaClO4, TBABF(4) and TEABF(4))/P(2AET)/GCE system. A good fitting was obtained for the calculated experimental and theoretical EIS measurement results. The electroactivity of P(2AET)/GCE opens the possibility of using modified coated electrodes for electrochemical micro-capacitor electrodes and biosensor applications.
Supercapacitor Behavior of Poly(Carbazole-EDOT) Derivatives/Multi-Walled Carbon Nanotubes, Characterizations and Equivalent Circuit Model Evaluations
(Taylor & Francis Inc, 2014) Ateş, Murat; Uludağ, Nesimi; Karazehir, Tolga; Arican, Fatih
Three new different comonomers of carbazole-EDOT derivatives had been previously synthesized and characterized in detail. In this study, electroactive materials were electropolymerized onto multi-walled carbon nanotube (MWCNT) modified glassy carbon (GC) electrode in 0.1M sodium dodecyl sulphate (SDS) solution. The electrochemical impedance spectroscopic results of Nyquist, and Bode-magnitude and Bode-phase plots show that polymers/MWCNT composites possess good capacitive characteristics. P(Com2)/MWCNT/GCE system's specific capacitance was up to Sc=132.6Fg(-1) at the scan rate of 70mVs(-1) from the area formula, Eq. (1). Furthermore, P(Com2)/MWCNT composite had very rapid charge/discharge ability with specific capacitance of Sc=75.23Fg(-1) at DC potential of 0.3V from Nyquist plot, and Sc=90.53Fg(-1) at the scan rate of 60mVs(-1) from charge formula, Eq. (2), which is important practical advantage. In addition, such composite had a good cycling performance and a wide potential window. Long-term stability of the capacitor was also tested by CV, and the results indicated that, after 500cycles, the specific capacitance was still at approximate to 100.0%, approximate to 89%, and approximate to 97.0% of the initial capacitance for P(Com1)/MWCNT, P(Com2)/MWCNT, and P(Com3)/MWCNT, respectively. An equivalent circuit model of R-s(C-1(R-1(Q(R2W))))(CGCRGC) was obtained to fit the experimental and theoretical data. Solution resistance (Rs) and resistance from GCE decrease gradually. However, capacitance of film (C-1), constant phase element (Q), and n values increase for P(Com1), P(Com2), and P(Com3)/MWCNT, respectively. Therefore, more homogeneous and less rough surface composite film was obtained by addition of MWCNT in the composite material.
Synthesis of 2-(3,6-bis(2,3-dihydrothieno[3,4-b][1,4]dioxin-5-yl)-9H-carbazole-9-yl)ethyl Methacrylate, Electropolymerization, Characterization and Impedimetric Study
(Electrochemical Soc Inc, 2013) Ateş, Murat; Uludağ, Nesimi; Karazehir, Tolga; Arican, Fatih
In this work, 2-(3,6-bis(2,3-dihydrothieno[3,4-b][1,4]dioxin-5-yl)-9H-carbazole-9-yl)ethyl methacrylate (EDOTCzMetac) was chemically synthesized and characterized by FTIR, H-1-NMR, and C-13-NMR. A novel synthesized comonomer was firstly electropolymerized on glassy carbon electrode (GCE) in various initial molar concentrations [EDOTCzMetac] 0 = 1.0, 3.0, 5.0 and 10.0 mM) in 0.1 M tetraethyl ammonium tetrafluoroborate (TEABF(4))/acetonitrile (CH3CN). Poly(EDOTCzMetac)/GCE was characterized by the technique of Cyclic Voltammetry (CV), Fourier Transform Infrared Reflectance-Attenuated Total Reflection Spectroscopy (FTIR-ATR), Scanning Electron Microscopy-Energy Dispersive X-ray analysis (SEM-EDX), Atomic Force Microscope (AFM) and Electrochemical impedance spectroscopy (EIS). The capacitive behavior of modified electrode was obtained via EIS method by the help of Nyquist, Bode-magnitude, Bode-phase, and Admittance plots. The highest low frequency capacitance (C-LF) value was obtained as 4.99 mF cm(-2) for [EDOTCzMetac](0) = 10.0 mM. Therefore, the synthesized copolymer for [EDOTCzMetac](0) = 10 mM has more capacitive behavior than the initial monomer concentration for [EDOTCzMetac](0) = 1.0 mM as C-LF = 3.63 mF cm(-2), for [EDOTCzMetac](0) = 3.0 mM as C-LF = 4.10 mF cm(-2) and for [EDOTCzMetac](0) = 5.0 mM as C-LF = 4.67 mF cm(-2). To interpret the AC impedance spectra, R(C(R(Q(RW))))(CR) electrical equivalent circuit was employed with linear Kramers-Kronig test. (C) 2012 The Electrochemical Society. [DOI: 10.1149/2.011302jes] All rights reserved.
Synthesis of 9H-carbazole-9-carbothioic methacrylic thioanhydride, electropolymerization, characterization and supercapacitor applications
(Springer, 2014) Ateş, Murat; Uludağ, Nesimi; Arican, Fatih
A novel organic molecule of 9H-carbazole-9-carbothioic methacrylic thioanhydride (CzCS(2)metac) was synthesized by incorporating CS2 and methacrylate groups into the carbazole monomer structure. CzCS(2)metac was characterized by FTIR, H-1-NMR and C-13-NMR spectroscopy. CzCS(2)metac was electropolymerized in 0.1 M tetraethylammonium tetrafluoroborate (TEABF(4))/acetonitrile (CH3CN) on glassy carbon electrode (GCE). The characterization of the electrocoated P(CzCS(2)metac)/CFME thin film was studied by various techniques, such as cyclic voltammetry, scanning electron microscopy-energy-dispersive X-ray analysis and electrochemical impedance spectroscopy. The specific capacitance (C (sp)) of P(CzCS(2)metac)/MWCNT/GCE in the scan rate of 20 mV s(-1) (C (sp) = 38.48 F g(-1) from area formula, C (sp) = 38.52 F g(-1) from charge formula) was increased similar to 15.66 and similar to 15.64 times in area and charge formulas compared to P(CzCS(2)metac)/GCE (C (sp) = 2.46 F g(-1) from area and charge formulas). The same results were also obtained from Nyquist graphs. The specific capacitance value of composite film (C (sp) = 1.09 x 10(-3) F) is similar to 15.66 times higher than the polymer film (C (sp) = 6.92 x 10(-5) F). The composite film may be used as supercapacitor electrode material in energy storage devices.
Synthesis of methyl 4-(9H-carbazole-9-carbanothioylthio) benzoate: electropolymerization and impedimetric study
(Scientific Technical Research Council Turkey-Tubitak, 2015) Ateş, Murat; Uludağ, Nesimi; Arican, Fatih; Karazehir, Tolga
Methyl 4((9H-(carbazole-97carbanothioylthio) benzoate (MCzCTB) was chemically synthesized and characterized by FTIR, H-1 NMR, and C-13 NMR. A novel synthesized monomer was electropolymerized on a glassy carbon electrode (GCE) in various initial molar concentrations of [MCzCTB](0) = 1, 3, 5, and 10 mM in 0.1 M NaClO4/CH3CN and 1 M H2SO4 center dot P(MCzCTB)/GCE was characterized by cyclic voltammetry, Fourier transform infrared-attenuated transmittance reflectance, scanning electron microscopy-energy dispersive X-ray, and electrochemical impedance spectroscopy. The capacitive behavior of the modified electrode was obtained by Nyquist, Bode-magnitude, and Bode-phase plots. The highest capacitance at low frequency was obtained as similar to 53.1 mF cm(-2) from Nyquist plot and 19.454 Fg(-1) at a scan rate of 10 mV s(-1) for [MCzCTB](0) = 1.0 mM. CS2 and OCH3 groups are electron-withdrawing and electron-donating groups in the monomer structure. These groups affect the polymerization and capacitive behavior of the polymer. The polymer may be used for supercapacitor and biosensor applications in the future.

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