Electrochemistry of Conductive Polymers 46. Polymer Films as Overcharge Inhibitors for Lithium-Ion Rechargeable Batteries

Choi, Sangmin; Park, Su‐Moon

doi:10.5229/jecst.2010.1.1.001

Consecutive Ligand‐Based Electron Transfer in New Molecular Copper‐Based Water Oxidation Catalysts

Gil‐Sepulcre

¹

,

Garrido‐Barros

²

,

Oldengott

³

et al. 2021

Angewandte Chemie

2

0

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Experimental Procedures MaterialsAll general reagents and chemicals were used as purchased from Sigma-Aldrich, Fluka and Merck chemical companies without further purification unless otherwise stated. The ligand precursor ([2,2'-bipyridine]-6,6'-dicarboxylic acid) and 5-amino-m-xylol-4-sulfonic acid were prepared according to the experimental procedure reported in the literature. 1,2 Air and moisture sensitive reactions were carried out under N2 or Ar in oven-dried (120 °C) glassware. Evaporation of solvents in vacuo was done with a Büchi Rotevapor R-200 at 40 °C. Instrumentation and measurementsNMR spectra were measured on a Bruker AV-500, Bruker AV-400, and Bruker 300 MHz spectrometers. All NMR experiments were performed at room temperature in corresponding deuterated solvents and using solvent signals as reference. UV-Vis spectra were measured on a Cary 50 UV-vis spectrometer by Varian Inc. Electrospray ionization mass spectra (ESI-MS) were performed on an Agilent Technologies 6130-Quadrupole LC/MS connected to an Agilent Technologies HPLC-1200 series. Samples were dissolved in MeOH or H2O and injected directly with an auto-sampler. HRMS samples were measured on a Bruker HPLC-QqTOF Maxis impact device. Elemental Analysis of the samples was carried out in a Thermo Finnigan elemental analyzer Flash 1112 model. Electron Paramagnetic Resonance was performed in an EMX Micro X-band EPR spectrometer (Bruker) at 77 K using a liquid N2 finger dewar. Data acquisition: perpendicular mode, modulation frequency of 100 KHz, microwave frequency of 9.38 GHz, modulation amplitude of 4 G, a 0.01 ms time constant and 4.12 ms conversion time with a microwave power of 0.556 mW. Electrochemical measurementsDifferential pulse voltammetry (DPV) and cyclic voltammetry (CV) were measured on a CHI660D potentiostat using a three-electrode cell. Glassy carbon (GC), Carbon paper (C-paper, SGL Carbon, Sigracet 39 AA) or boron-doped diamond (BDD) (d = 3 mm) working electrodes were employed while a Pt rod/mesh was used as counter electrode and a Hg/HgSO4 (K2SO4 sat.) or Ag/AgCl (KCl sat.) electrode were used as a reference electrode. Working electrodes were polished with 1 and 0.05 micron alumina paste, washed with distilled water and acetone, and sonicated in acetone for 5 minutes before each measurement. DMF employed for electrochemical measurements was prepared containing the necessary amount of n-Bu4NPF6 (TBAPF6) as supporting electrolyte to yield a solution of 0.1 M ionic strength. CVs were typically recorded at different scan rates from 25 to 1000 mV/s. DPVs were recorded with the following parameters: amplitude = 50 mV, step height = 4 mV, pulse width = 0.05 s. All redox potentials in the present work are reported versus NHE by adding 0.648 V to the measured potential.

show abstract

Consecutive Ligand‐Based Electron Transfer in New Molecular Copper‐Based Water Oxidation Catalysts

Gil‐Sepulcre

¹

,

Garrido‐Barros

²

,

Oldengott

³

et al. 2021

View full text Add to dashboard Cite

Experimental Procedures MaterialsAll general reagents and chemicals were used as purchased from Sigma-Aldrich, Fluka and Merck chemical companies without further purification unless otherwise stated. The ligand precursor ([2,2'-bipyridine]-6,6'-dicarboxylic acid) and 5-amino-m-xylol-4-sulfonic acid were prepared according to the experimental procedure reported in the literature. 1,2 Air and moisture sensitive reactions were carried out under N2 or Ar in oven-dried (120 °C) glassware. Evaporation of solvents in vacuo was done with a Büchi Rotevapor R-200 at 40 °C. Instrumentation and measurementsNMR spectra were measured on a Bruker AV-500, Bruker AV-400, and Bruker 300 MHz spectrometers. All NMR experiments were performed at room temperature in corresponding deuterated solvents and using solvent signals as reference. UV-Vis spectra were measured on a Cary 50 UV-vis spectrometer by Varian Inc. Electrospray ionization mass spectra (ESI-MS) were performed on an Agilent Technologies 6130-Quadrupole LC/MS connected to an Agilent Technologies HPLC-1200 series. Samples were dissolved in MeOH or H2O and injected directly with an auto-sampler. HRMS samples were measured on a Bruker HPLC-QqTOF Maxis impact device. Elemental Analysis of the samples was carried out in a Thermo Finnigan elemental analyzer Flash 1112 model. Electron Paramagnetic Resonance was performed in an EMX Micro X-band EPR spectrometer (Bruker) at 77 K using a liquid N2 finger dewar. Data acquisition: perpendicular mode, modulation frequency of 100 KHz, microwave frequency of 9.38 GHz, modulation amplitude of 4 G, a 0.01 ms time constant and 4.12 ms conversion time with a microwave power of 0.556 mW. Electrochemical measurementsDifferential pulse voltammetry (DPV) and cyclic voltammetry (CV) were measured on a CHI660D potentiostat using a three-electrode cell. Glassy carbon (GC), Carbon paper (C-paper, SGL Carbon, Sigracet 39 AA) or boron-doped diamond (BDD) (d = 3 mm) working electrodes were employed while a Pt rod/mesh was used as counter electrode and a Hg/HgSO4 (K2SO4 sat.) or Ag/AgCl (KCl sat.) electrode were used as a reference electrode. Working electrodes were polished with 1 and 0.05 micron alumina paste, washed with distilled water and acetone, and sonicated in acetone for 5 minutes before each measurement. DMF employed for electrochemical measurements was prepared containing the necessary amount of n-Bu4NPF6 (TBAPF6) as supporting electrolyte to yield a solution of 0.1 M ionic strength. CVs were typically recorded at different scan rates from 25 to 1000 mV/s. DPVs were recorded with the following parameters: amplitude = 50 mV, step height = 4 mV, pulse width = 0.05 s. All redox potentials in the present work are reported versus NHE by adding 0.648 V to the measured potential.

show abstract

Determination of the thermoelectric properties of exfoliated graphitic carbon nitride-filled unsubstituted polythiophene composites

Uğraşkan

¹

,

Karaman

²

2022

Fullerenes, Nanotubes and Carbon Nanostructures

2

0

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Electrochemistry of Conductive Polymers 46. Polymer Films as Overcharge Inhibitors for Lithium-Ion Rechargeable Batteries

Cited by 3 publications

References 96 publications

Consecutive Ligand‐Based Electron Transfer in New Molecular Copper‐Based Water Oxidation Catalysts

Consecutive Ligand‐Based Electron Transfer in New Molecular Copper‐Based Water Oxidation Catalysts

Consecutive Ligand‐Based Electron Transfer in New Molecular Copper‐Based Water Oxidation Catalysts

Determination of the thermoelectric properties of exfoliated graphitic carbon nitride-filled unsubstituted polythiophene composites

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