研究目的
To investigate the effects of aging duration of a vanadium precursor solution (vanadyl acetylacetonate in methanol) on the reproducibility, material properties, and photoelectrochemical performance of BiVO4 photoanodes fabricated via metal–organic decomposition.
研究成果
Aging the vanadium precursor solution for an optimal duration (3 days) enhances the photoelectrochemical performance of BiVO4 photoanodes by inducing oxygen deficiency, increasing carrier concentration, and reducing charge transfer resistance. This approach improves reproducibility and efficiency, highlighting the importance of controlling solution chemistry in metal–organic decomposition processes.
研究不足
The study is limited to undoped BiVO4 and specific aging times; reproducibility might vary with other precursors or conditions. XPS analysis is surface-sensitive and may not fully represent bulk properties. The use of methanol solvent introduces oxidation issues over time.
1：Experimental Design and Method Selection:
A modified metal–organic decomposition (MOD) protocol was used, replacing acetylacetone with methanol as the solvent for vanadyl acetylacetonate to increase solubility. The aging time of the precursor solution was varied (0 to 5 days) to study its effects.
2：Sample Selection and Data Sources:
BiVO4 films were prepared on FTO substrates with a SnO2 hole-blocking layer. Precursor solutions were mixed with a Bi/V molar ratio of
3：List of Experimental Equipment and Materials:
Instruments included UV–vis spectrometer (SolidSpec-3700, Shimadzu), SEM (Philips XL30SFG), AFM (XE-100 Park Systems), XRD (D/Max-2500, Rigaku), ICP-MS (Agilent 7700S), XPS (Sigma Probe, Thermo VG Scientific), potentiostat (Bistat, Biologic Science Instruments), Xe arc lamp (Oriel 66902, 300W), Si photodiode (Oriel 91150 V). Materials included VO(acac)2 (99%, Aldrich), methanol (99%, Aldrich), Bi(NO3)3·5H2O (98%, Aldrich), acetic acid (99%, Aldrich), FTO substrates, KPi buffer, Na2SO3, Co-Pi catalyst.
4：Experimental Procedures and Operational Workflow:
VO(acac)2 was dissolved in methanol and aged for specified times. Bi and V precursors were mixed, spin-coated on substrates, and annealed at 480°C. PEC measurements were conducted in a three-electrode system with Pt counter electrode and Ag/AgCl reference electrode under AM
5：5 G illumination. Linear sweep voltammetry, electrochemical impedance spectroscopy, and Mott–Schottky analysis were performed. Data Analysis Methods:
Data were analyzed using EC-lab software for impedance fitting and Mott–Schottky plots. Charge separation and injection efficiencies were calculated from photocurrent densities. Composition was analyzed via ICP-MS and XPS.
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UV–vis spectrometer
SolidSpec-3700
Shimadzu
Measure optical transmittance, reflectance, and absorbance of samples.
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XRD
D/Max-2500
Rigaku
Perform X-ray diffraction measurements to confirm phase formation.
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ICP-MS
7700S
Agilent
Quantify chemical composition (e.g., Bi/V ratio) of films.
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SEM
XL30SFG
Philips
Conduct structural characterizations including surface morphology and grain size analyses.
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AFM
XE-100
Park Systems
Measure surface roughness and morphology in contact mode.
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XPS
Sigma Probe
Thermo VG Scientific
Analyze chemical composition including oxygen content via X-ray photoelectron spectroscopy.
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Potentiostat
Bistat
Biologic Science Instruments
Perform electrochemical measurements including linear sweep voltammetry, electrochemical impedance spectroscopy, and Mott–Schottky analysis.
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Xe arc lamp
66902
Oriel
Provide AM 1.5 G illumination for photoelectrochemical measurements.
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Si photodiode
91150 V
Oriel
Calibrate 1 sun illumination before measurements.
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