研究目的
To prepare CdO-TiO2 nanotubes using a direct impregnation-calcination method to improve photocatalytic hydrogen evolution efficiency and investigate the influence of CdO doping amount.
研究成果
The direct impregnation method successfully prepared CdO-TiO2 nanotubes with enhanced photoelectrochemical performance. Optimal CdO doping at 50 mM concentration achieved the highest IPCE of 10.16%, attributed to improved light absorption and electron accumulation, though hole accumulation caused photocurrent decay. Cd2+ incorporation into the TiO2 lattice altered electronic properties, but excessive doping formed CdTiO3 and reduced efficiency.
研究不足
The study is limited to specific Cd(NO3)2 concentrations and annealing conditions; higher concentrations led to CdTiO3 formation and reduced performance. The method may not be scalable, and the photocurrent decay indicates issues with charge carrier recombination and transport.
1:Experimental Design and Method Selection:
The study used a direct impregnation-calcination method to deposit CdO nanoparticles into TiO2 nanotube structures. TiO2 nanotubes were prepared via an optimized two-step anodization process. Characterization methods included SEM, TEM, UV-Vis DRS, XPS, XRD, and PEC measurements to analyze morphology, crystallinity, composition, and photoelectrochemical properties.
2:Sample Selection and Data Sources:
Titanium foil samples (0.1×30×40 mm, 99.6+% purity) were used. CdO-TiO2 nanotubes were prepared with varying concentrations of cadmium nitrate tetrahydrate (10, 30, 50, 70, 200, and 800 mM).
3:1×30×40 mm, 6+% purity) were used. CdO-TiO2 nanotubes were prepared with varying concentrations of cadmium nitrate tetrahydrate (10, 30, 50, 70, 200, and 800 mM). List of Experimental Equipment and Materials:
3. List of Experimental Equipment and Materials: Equipment included a ZEISS-IGMA HD/VP SEM, D/max-2200PC XRD, AXIS Ultra XPS, JEM-2100 TEM, UV-2550 UV-Vis spectrophotometer, AUTOLAB PGSTAT 30 for impedance-potential measurements, and Optimax 365 UV light source. Materials included titanium foil, ethylene glycol, deionized water, citric acid, ammonium fluoride, cadmium nitrate tetrahydrate, and sodium sulfate electrolyte.
4:Experimental Procedures and Operational Workflow:
TiO2 nanotubes were prepared by degreasing Ti foil, anodizing in a two-electrode system with specific electrolyte and conditions, followed by UV irradiation and immersion in Cd(NO3)2 solutions at different concentrations, rinsing, drying, and annealing at 450°C. PEC measurements used a three-electrode setup with CdO/TiO2 as working electrode, platinum net as counter electrode, and Ag/AgCl as reference electrode in 1 M Na2SO4 electrolyte under nitrogen purging.
5:Data Analysis Methods:
Data were analyzed using techniques such as XRD for phase identification, XPS for chemical composition, Mott-Schottky plots for flatband potential and charge carrier density calculation, and IPCE calculation from photocurrent measurements.
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Scanning Electron Microscope
ZEISS-IGMA HD/VP
ZEISS
Used for structural and morphological characterization of samples, including top view and cross-sectional observations.
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X-ray Diffractometer
D/max-2200PC
Rigaku
Used for crystalline phase characterization of the CdO-TiO2 nanotubes.
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X-ray Photoelectron Spectrometer
AXIS Ultra
Kratos
Employed to investigate the chemical composition of the CdO-TiO2 nanotubes.
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Transmission Electron Microscope
JEM-2100
JEOL
Used to obtain TEM images of the samples.
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UV-Vis Spectrophotometer
UV-2550
Shimadzu
Used to obtain UV-Vis diffuse reflection spectra of the samples.
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Potentiostat
AUTOLAB PGSTAT 30
Metrohm
Used for impedance-potential measurements, including Mott-Schottky plots.
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UV Light Source
Optimax 365
Optimax
Used for UV irradiation during sample preparation and as a light source in photoelectrochemical measurements.
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Titanium Foil
Advent
Used as the substrate for preparing TiO2 nanotubes via anodization.
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Cadmium Nitrate Tetrahydrate
Macklin
Used as the precursor for CdO doping in the impregnation process.
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