Direct electrochemical co-polymerization of EDOT and hydroquinone

The dataset titled "Direct Electrochemical Copolymerization of EDOT and Hydroquinone" provides supporting data for the manuscript of the same name. This includes characterization and electrochemical experimental data supporting the study of copolymer films synthesized from EDOT and hydroquinone (QH₂). This data focuses on exploration of the properties and behaviour of co-PEDOT-QH₂ films.

Methodology

The copolymerization process was conducted through direct electrochemical synthesis using cyclic voltammetry (CV), potentiostatic, and pulse potentiostatic deposition techniques. The deposition was performed in acetonitrile-based solutions containing lithium perchlorate (LiClO₄) as the supporting electrolyte. Co-PEDOT-QH₂ films contained different ratios of both components, and the impact of the ratio and the mode of copolymerisation on the electrochemical performance, structural properties, and stability. The synthesized films were subjected to multiple characterization methods, including:

• Electrochemical Analysis: Cyclic voltammetry (CV) was employed to study the redox behavior of the films under different conditions, such as varying concentrations of seed solution, deposition mode, scan rates, etc.
• Spectroscopic Techniques: Vibrational spectroscopy (Raman spectroscopy and FTIR [ATR and KBr]), X-ray photoelectron spectroscopy (XPS), and operando UV-Vis spectroelectrochemistry were used to analyze the molecular structure, chemical composition, and charge transfer behaviour.
• Operando Measurements: Electrochemical quartz crystal microbalance (EQCM) was utilized to monitor mass changes during redox cycling.
• Galvanostatic Charge-Discharge (GCD): Conducted to evaluate specific capacity, retention, and coulombic efficiency at different current densities.

Data Description

The dataset includes raw data files corresponding to experimental results for each figure in the manuscript:

1. Electrochemical Data: CV (inluding bipotentiostat data for conductance measurements on IDEs), GCD files documenting synthesis and cycling processes for co-PEDOT-QH₂ films with different molar percentages of QH₂ and, in separate cases, with p-toluenesulfonic acid (PTSA) or PEDOT without any additives.
2. Spectroscopic Data: Raman (shift-intensity) and FTIR (wave number-transmittance) files for structural analysis.
3. UV-Vis Spectroelectrochemistry: 3D absorbance data arrays showing wavelength vs potential during oxidation/reduction cycles.
4. Impedance Spectroscopy: Frequency-dependent impedance data for films synthesized at various QH2 concentrations.

Equipment

Experiments were conducted using the following instrumentation:

• Autolab PGSTAT128N for electrochemical measurements.
• DropSens μ400 bipotentiostat for conductance studies on interdigitated electrodes (IDE).
• Avantes AvaSpec spectrometer for UV-Vis spectroscopy.

Resource centres data

The data obtained from the resource centres (i.e., vibrational spectroscopy methods, X-ray photoelectron spectroscopy, ) were recorded using the equipment available at the Research Park of St Petersburg State University (https://researchpark.spbu.ru/index.php/en/). We are grateful to the operators of the following resource centres:

• Chemical Analysis and Materials Research Centre
• Centre for Optical and Laser Materials Research
• Centre for Physical Methods of Surface Investigation
• Interdisciplinary Resource Centre for Nanotechnology

Data processing

Data processing involved proprietary software associated with these instruments, supplemented by Python (>3.10) scripts and Origin (>9.0) data handling for conversion into standardized formats. Mass spectrometry data were converted to mzML format using MS Convert by ProteoWizard.

Reproducibility

Detailed descriptions of file naming conventions, experimental conditions, and equipment settings are provided within the dataset documentation (README file) to facilitate replication of results.