This README.txt file was generated on 2024-11-27 by José García Antón (Principal Investigator) ------------------- GENERAL INFORMATION ------------------- Title of Dataset: Synthesis of TiO2/ZnO2 hybrid nanosponges by electrodeposition with different times, temperatures and Zn(NO3)2 concentrations used as photoanodes for 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: 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: 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: Rita Sánchez-Tovar, Avinguda de la Universitat s/n, 46100 Burjassot, Valencia (Spain), rita.sanchez@uv.es, ORCID: 0000-0002-6811-5854 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 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”. General description: The dataset contains the data that have been obtained during the synthesis and the characterization (chemical and photoelectrochemical) of TiO2/ZnO2 hybrid nanosponges obtained by electrodeposition of ZnO on TiO2 nanosponges with different times (15 min, 30 min, and 60 min), temperatures (25ºC, 65 ºC, and 75 ºC) and Zn(NO3)2 concentrations (0.5-10 mM) and used as photoanodes for photoelectrochemical applications. Keywords: Hybrid Nanostructures; Nanosponge; Photoelectrochemical water splitting; Titanium dioxide; Zinc dioxide. -------------------------- 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/10.3390/ma14216441 Links/relationships to previous or related data sets: Links to other publicly accessible locations of the data: -------------------- DATA & FILE OVERVIEW -------------------- File list: 01.-PWS tests_Time: Photoelectrochemical water splitting (PWS) tests were performed for nanosponges with electrodeposition times of 15 min, 30 min, and 60 min to study the photoelectrochemical properties of the nanosponges. 02.-Electrodeposition_Temperature: ZnO electrodeposition was performed with temperatures of 25 ºC, 65 ºC, and 75 ºC. 03.-PWS tests_Temperature: Photoelectrochemical water splitting (PWS) tests were performed for nanosponges with electrodeposition temperatures of 25 ºC, 65 ºC, and 75 ºC to study the photoelectrochemical properties of the nanosponges. 04.-Electrodeposition_Concentration: ZnO electrodeposition was performed with Zn(NO3)2 concentrations between 0.5 mM and 10 mM. 05.-PWS tests_Concentration: Photoelectrochemical water splitting (PWS) tests were performed for nanosponges with Zn(NO3)2 concentrations between 0.5 mM and 10 mM to study the photoelectrochemical properties of the nanosponges. 06.-XPS tests: Nanosponges were characterised by X-Ray Photoelectron Spectroscopy (XPS) to verify the ZnO electrodeposition. 07.-GIXRD tests: Nanosponges were characterised by Grazing Incidence X-Ray Diffraction (GIXRD) to verify the ZnO electrodeposition. Relationship between files: Type of version of the dataset: Processed data. Total size: 6.92 MB -------------------------- METHODOLOGICAL INFORMATION -------------------------- Description of methods used for collection/generation of data: - Synthesis of TiO2/ZnO hybrid nanosponges: The formation of TiO2/ZnO hybrid nanosponges was carried out by ZnO electrodeposition on crystalline TiO2 nanosponges. Titanium rods (8 mm in diameter and 99.3% purity) were polished with 240–4000 silicon carbide (SiC) papers until a mirror surface was reached. After that, samples were immersed in ethanol for 2 min in an ultrasonic bath, rinsed with distilled water, and dried with air. The synthesis of the nanosponges was carried out by electrochemical anodization of titanium rods under hydrodynamic conditions (3000 rpm) in a glycerol/water (60:40 vol %) electrolyte with a concentration of 0.27 M NH4F. A two-electrode electrochemical cell with a rotating electrode configuration was used during anodization. The polished Ti sample (0.5 cm^2) was used as working electrode and a platinum foil as counter electrode. The samples were anodized at room temperature by increasing the potential from 0 to 30 V at a rate of 100 mV·s^-1, and applying subsequently 30 V for 3 h. During the anodization process, the current density was monitored. Next, samples were rinsed with distilled water and dried with air. Finally, photoelectrodes were annealed at 450 ºC for 1 h in air atmosphere with a heating rate of 15 C·min^-1 to transform TiO2 nanosponges to the anatase phase. Annealing improves conductivity and lifetime of charge carriers. Once the TiO2 nanosponges were formed, the ZnO electrodeposition process from a Zn(NO3)2 solution was carried out. ZnO electrodeposition was carried out in a three-electrode electrochemical cell and the temperature was controlled with a thermostatic bath. TiO2 nanosponges were used as working electrode, an Ag/AgCl (3 M KCl) electrode was used as reference electrode, and a platinum tip was used as counter electrode. ZnO electrodeposition was carried out at a potential of - 0.86 VAg/AgCl using an Autolab PGSTAT302N potentiostat. The influence of electrodeposition time (15, 30, and 60 min), electrodeposition temperature (25 ºC, 65 ºC, and 75 ºC), and Zn(NO3)2 concentration (0.5–10 mM) were studied to analyse how these parameters affect the photoelectrochemical activity of the photoelectrodes. - Chemical characterization of the nanosponges: X-Ray Photoelectron Spectroscopy (XPS) and Grazing Incidence X-Ray Diffraction (GIXRD) were used to verify the ZnO electrodeposition. On the one hand, all XPS spectra (K-ALPHA Thermo Scientific) were collected using Al-K monochromatized radiation (1486.6 eV) at 3 mA x 12 kV. Scanning step energies of 200 eV were used to measure the whole energy band and 50 eV to selectively measure elements. On the other hand, the apparatus used to obtain GIXRD spectra is a Bruker D8AVANCE diffractometer with Cu radiation operating at 30 mA and 40 kV from 20 degree to 60 degree and a grazing incidence of 2 degree. - Photoelectrochemical characterization of the nanosponges: Photoelectrochemical experiments were performed in a cell with a three-electrode configuration using 0.1 M NaOH as electrolyte and a solar simulator (AM 1.5, 100 mW·cm^-2) connected to a potentiostat (Autolab PGSTAT302N). The TiO2/ZnO hybrid nanosponges, with an area of 0.13 cm^2 exposed to the test solution were the working electrodes. A platinum tip was used as counter electrode, and an Ag/AgCl(3 M KCl) electrode as reference electrode. For the experiments, a potential sweep was performed from -1 VAg/AgCl to 0.84 VAg/AgCl with a scan rate of 2 mV·s^-1 by chopped light irradiation (60 mV (30 s) in the dark and 20 mV (10 s) with light). Current intensity obtained was normalized with the electrode area. 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. Missing data codes: Specialized formats or other abbreviations used: A: Amps. a.u.: Arbitrary units. eV: electron volt. VAg-AgCl: Volts respect to silver/silver chloride reference electrode.