This README.txt file was generated on 2024-07-25 by José García Antón (Principal Investigator) ------------------- GENERAL INFORMATION ------------------- Title of Dataset: Synthesis and Characterisation of TiO2/ZnO2 hybrid nanostructures formed by electrodeposition with different Zn(NO3)2 concentrations and used in photoelectrochemical applications [Dataset] Author Information: Principal Investigator: José García-Antón, Universitat Politècnica de València, Camino de Vera s/n, 46022 Valencia (Spain), jgarciaa@iqn.upv.es, ORCID: 0000-0002-0289-1324 Associate or Co-investigator: Pedro José Navarro-Gázquez, Universitat Politècnica de València, Camino de Vera s/n, 46022 Valencia (Spain), pednagz@etsii.upv.es Associate or Co-investigator: Encarna Blasco-Tamarit, Universitat Politècnica de València, Camino de Vera s/n, 46022 Valencia (Spain), meblasco@iqn.upv.es, ORCID: 0000-0001-7314-082X Associate or Co-investigator: María José Muñoz-Portero, Universitat Politècnica de València, Camino de Vera s/n, 46022 Valencia (Spain), mjmunoz@iqn.upv.es, ORCID: 0000-0002-7407-2598 Associate or Co-investigator: Benjamín Solsona-Espriu, Avinguda de la Universitat s/n, 46100 Burjassot, Valencia (Spain), benjamin.solsona@uv.es, ORCID: 0000-0001-7235-2038 Associate or Co-investigator: Ramón Manuel Fernández-Domene, Avinguda de la Universitat s/n, 46100 Burjassot, Valencia (Spain), ramon.fernandez@uv.es, ORCID: 0000-0003-4839-8225 Associate or Co-investigator: Rita Sánchez-Tovar, Avinguda de la Universitat s/n, 46100 Burjassot, Valencia (Spain), rita.sanchez@uv.es, ORCID: 0000-0002-6811-5854 Date of data collection: 2021 Geographic location of data collection: Valencia, Spain (39.482369, -0.343578). Information about funding sources or sponsorship that supported the collection of the data: Ministerio de Ciencia e Innovación, Project code: PID2019-105844RB-I00/AEI/10.13039/501100011033. Project co-funded by FEDER operational programme 2014-2020 of Comunitat Valenciana (IDIFEDER/2018/044) for the financial funding. Grant PEJ2018-003596-A-AR funded by MCIN/AEI/10.13039/501100011033 and by “ESF Investing in your future”. MINECO, Project code: MAT2017-84118-C2-1-R. General description: The dataset contains the data that have been obtained during the synthesis and the characterization (structural, compositional, and electrochemical) of TiO2/ZnO2 hybrid nanostructures formed by electrodeposition with different Zn(NO3)2 concentrations (10-60 mM) and used in photoelectrochemical applications. Keywords: TiO2/ZnO hybrid Nanostructures; Zn(NO3)2 concentration; Photoelectrochemical applications. -------------------------- SHARING/ACCESS INFORMATION -------------------------- Open Access to data: Open Date end Embargo: Licenses/restrictions placed on the data, or limitations of reuse: All rights reserved Citation for and links to publications that cite or use the data: https://doi.org/10.1016/j.ceramint.2022.01.339 Links/relationships to previous or related data sets: Links to other publicly accessible locations of the data: -------------------- DATA & FILE OVERVIEW -------------------- File list: 01.-Anodization_Ti_TiO2: Synthesis of TiO2 nanosponges with crystalline structure was carried out by electrochemical anodization on titanium metallic substrate. 02.-Electrodeposition_ZnO: ZnO electrodeposition was performed with Zn(NO3)2 concentrations between 10 mM and 60 mM. 03.-XRD tests: Nanostructures were characterised by X-Ray Diffraction (XRD) to obtain more detail about the their crystalline structure. 04.-PWS tests: Photoelectrochemical water splitting (PWS) tests were performed to study the photoelectrochemical properties of the nanostructures. 05.-Stability tests: Stability tests at 0.84 VAg/AgCl for 1 h were carried out to check the photostability to photocorrosion of the nanostructures. 06.-EIS tests_Nyquist: Nyquist diagrams obtained from electrochemical Impedance Spectroscopy (EIS) tests at different conditions were performed to analyse the electrochemical behaviour of the nanostructures. 07.-EIS tests_Bode: Bode diagrams obtained from electrochemical Impedance Spectroscopy (EIS) tests at different conditions were performed to analyse the electrochemical behaviour of the nanostructures. 08.-Mott-Schottky tests: Mott–Schottky (M-S) tests at different conditions were performed to analyse the electrochemical behaviour of the nanostructures. Relationship between files: Type of version of the dataset: Processed data. Total size: 5.15 MB -------------------------- METHODOLOGICAL INFORMATION -------------------------- Description of methods used for collection/generation of data: - Synthesis of TiO2/ZnO hybrid nanostructures: The formation of TiO2/ZnO hybrid nanostructures was carried out by ZnO electrodeposition on crystalline TiO2 nanosponges. First, TiO2 nanosponges were synthesised by electrochemical anodization of titanium (Ti) under hydrodynamic conditions at room temperature. For this purpose, metallic titanium rod (99.3% purity and 8 mm in diameter) was polished with 240–4000 silicon carbide (SiC) papers to obtain a mirror surface. After that, the sample was sonicated in ethanol for 2 min, rinsed with distilled water, and dried with air. Finally, the sample was covered with a polytetrafluoroethylene (PTFE) coating (0.5 cm2 area exposed to the electrolyte). Polished Ti was used as working electrode, and a platinum foil as counter electrode. A solution composed of glycerol/water (60/40 vol%) with 0.27 M ammonium fluoride (NH4F) at room temperature was used as electrolyte. The potential was increased from 0 to 30 V at a constant rate of 0.1 V·s-1 applying subsequently 30 V for 3 h. TiO2 nanosponges were then annealed at 450 ◦C for 1 h to obtain the anatase crystalline structure of TiO2. Finally, the ZnO electrodeposition was carried out at a potential of -0.86 VAg/AgCl for 15 min at 75 ◦C with zinc nitrate hexahydrate (Zn(NO3)2⋅6H2O) concentrations between 10 and 60 mM. TiO2 nanosponges were used as working electrodes, a platinum tip was used as counter electrode, and an Ag/AgCl (3 M KCl) electrode was used as reference electrode. - Structural and compositional characterisation of the nanostructures: X-Ray Diffraction (XRD) was used to verify the ZnO formation, to identify the composition of the phases of the crystals, and to obtain the crystallite size of the nanostructures. In order to carry out this process, a Bruker D8AVANCE diffractometer with Cu radiation operating at 30 mA and 40 Kv was used. - Electrochemical characterisation of the nanostructures: The electrochemical characterisation was carried out in both dark and illuminated (AM 1.5, 100 mW·cm-2) conditions in a cell composed of three electrodes connected to a potentiostat (Autolab PGSTAT302 N) where the nanostructures were the working electrodes, a platinum tip was the counter electrode, and an Ag/AgCl (3 M KCl) electrode was the reference electrode. A 0.1 M NaOH aqueous solution was used as electrolyte. The photoelectrochemical response of nanostructures was measured by photoelectrochemical water splitting (PWS) tests performed between -1.0 and 0.84 VAg/AgCl with a scan rate of 2 mV·s-1 by chopped light irradiation. In addition, stability tests to photocorrosion were also carried out applying a potential of 0.84 VAg/AgCl for 1 h. Electrochemical Impedance Spectroscopy (EIS) and Mott-Schottky (M-S) tests were performed to analyse the electrochemical behaviour of the nanostructures that presented the best photoelectrocatalytic performance. On the one hand, EIS was carried out at 0.6 VAg/AgCl in a frequency range from 100 kHz to 10 mHz with a 10 mV signal amplitude. On the other hand, Mott-Schottky (M-S) tests were performed from 0.8 to -0.9 VAg/AgCl at a frequency of 10 kHz with an amplitude signal of 10 mV. Methods for processing the data: Processed data are registered in files with extension xlsx. Software- or Instrument-specific information needed to interpret the data, including software and hardware version numbers: Microsoft Excel 2019. Standards and calibration information, if appropriate: Environmental/experimental conditions: Describe any quality-assurance procedures performed on the data: -------------------------- DATA-SPECIFIC INFORMATION -------------------------- Number of variables: Number of cases/rows: Variable list, defining any abbreviations, units of measure, codes or symbols used: "I" represents current intensity, "i" represents current density, "Z" represents impedance, "C" represents capacitance. Missing data codes: Specialized formats or other abbreviations used: A: Amps. a.u.: Arbitrary units. VAg-AgCl: Volts respect to silver/silver chloride reference electrode. Hz: Hertz. rad: Radians. F: Farad.