研究目的
Investigating the band edge properties and photoelectrochemical water splitting activity of Nb-doped WO3 nanotriangle thin films fabricated via a facile hydrothermal method.
研究成果
Nb doping in WO3 via a facile hydrothermal method successfully alters the crystal phase to hexagonal, increases band gap and oxygen vacancies, and enhances PEC water splitting activity. Band edge positions shift downward, and Fermi level shifts upward, indicating improved n-type semiconductor properties. The optimal doping level is 2.12 at% Nb, leading to higher photocurrent, IPCE, and conversion efficiency.
研究不足
The study is limited to Nb doping in WO3 and its effects on PEC water splitting; other dopants or conditions were not explored. The hydrothermal method may have scalability issues, and the stability over longer periods or under different environmental conditions was not extensively tested.
1:Experimental Design and Method Selection:
A facile hydrothermal method was used to synthesize Nb-doped WO3 nanotriangle thin films on FTO substrates. The process involved condensation of peroxopolytungstic acid solution containing Nb precursor at 150°C, followed by annealing at 500°C. This method allowed simultaneous doping and thin film formation in a single step.
2:Sample Selection and Data Sources:
Undoped and Nb-doped WO3 thin films were synthesized. The amount of niobium(V) ethoxide was varied to achieve different doping levels, with 2.12 at% Nb identified as optimal based on EDS analysis.
3:12 at% Nb identified as optimal based on EDS analysis. List of Experimental Equipment and Materials:
3. List of Experimental Equipment and Materials: Materials included sodium tungstate dihydrate (Na2WO4·H2O, Junsei ≥99.0%), hydrochloric acid (HCl, Sigma Aldrich), hydrogen peroxide (H2O2, Sigma Aldrich), niobium(V) ethoxide (Nb[OCH2CH3]5, Sigma Aldrich 99.95%), and FTO substrates. Equipment included SEM (Hitachi S4800), XRD (MiniFlex), TEM (JEOL JEM-2100F), UV-Vis spectrophotometer (Varian Cary 5000), XPS (Thermo Fisher Scientific), electrochemical analyzer (Iviumstat), solar simulator (ABET Technologies Sun 2000), and monochromator (Thermo Oriel Cornerstone 7400 1/8).
4:0%), hydrochloric acid (HCl, Sigma Aldrich), hydrogen peroxide (H2O2, Sigma Aldrich), niobium(V) ethoxide (Nb[OCH2CH3]5, Sigma Aldrich 95%), and FTO substrates. Equipment included SEM (Hitachi S4800), XRD (MiniFlex), TEM (JEOL JEM-2100F), UV-Vis spectrophotometer (Varian Cary 5000), XPS (Thermo Fisher Scientific), electrochemical analyzer (Iviumstat), solar simulator (ABET Technologies Sun 2000), and monochromator (Thermo Oriel Cornerstone 7400 1/8). Experimental Procedures and Operational Workflow:
4. Experimental Procedures and Operational Workflow: PTA solution was prepared by adding HCl and H2O2 to sodium tungstate solution. Nb precursor was added, and the mixture was hydrothermally condensed at 150°C for 2.5 hours. After synthesis, films were rinsed and annealed at 500°C for 2 hours. PEC measurements were conducted in a three-electrode setup with 0.5 M Na2SO4 electrolyte under AM 1.5G illumination.
5:5 hours. After synthesis, films were rinsed and annealed at 500°C for 2 hours. PEC measurements were conducted in a three-electrode setup with 5 M Na2SO4 electrolyte under AM 5G illumination. Data Analysis Methods:
5. Data Analysis Methods: Data were analyzed using techniques such as XRD for crystallography, SEM/TEM for morphology, UV-Vis for optical properties, XPS for surface composition, LSV for photocurrent, IPCE for efficiency, EIS for impedance, and Mott-Schottky analysis for carrier density and flat band potential.
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Scanning Electron Microscope
S4800
Hitachi
Analyzing surface morphology and thickness of WO3 thin films
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Transmission Electron Microscope
JEM-2100F
JEOL
Measuring interplanar d-spacing, selected area electron diffraction, elemental mapping, and EDS
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Monochromator
Cornerstone 7400 1/8
Thermo Oriel
Used with xenon arc lamp for IPCE measurements
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Xenon Arc Lamp
1000 W
Thermo Oriel
Light source for IPCE measurements
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X-ray Diffractometer
MiniFlex
Characterizing crystalline phase
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Spectrophotometer
Cary 5000
Varian
Measuring ultraviolet-visible absorption
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X-ray Photoelectron Spectrometer
Thermo Fisher Scientific
XPS analysis
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Electrochemical Analyzer
Iviumstat
Performing PEC measurements
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Solar Simulator
Sun 2000
ABET Technologies
Providing AM 1.5G illumination
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