研究目的
To design and fabricate a CuOx/WO3 p-n heterojunction thin-film photocathode using magnetron reactive sputtering and annealing to enhance photoelectrochemical performance and stability for water splitting.
研究成果
The CuOx/WO3 p-n heterojunction thin-film photocathode fabricated by magnetron reactive sputtering and slow rate annealing at 500°C significantly enhances photoelectrochemical performance, with a photoinduced current density of -3.8 mA cm-2, 1.5 times higher than bare CuOx, due to improved charge separation and stability. This approach offers a promising method for efficient water splitting.
研究不足
The study is limited to specific annealing conditions and materials; scalability and long-term stability in real-world applications may require further investigation. The use of a laboratory setup may not fully represent industrial conditions.
1:Experimental Design and Method Selection:
The study employed magnetron reactive sputtering for thin-film deposition due to its ability to produce high-quality, uniform films at high growth rates. Annealing in O2 ambient was used to stabilize the structure and improve crystallinity.
2:Sample Selection and Data Sources:
F-doped SnO2 transparent conducting glass (FTO) was used as the substrate. Samples were prepared with different annealing conditions (no annealing, rapid thermal annealing at 500°C, slow rate annealing at 300°C and 500°C).
3:List of Experimental Equipment and Materials:
Equipment includes magnetron sputtering system, annealing furnace, ultrasonic cleaner, X-ray diffractometer (XRD, D/max-500, Rigaku Co.), Raman spectrometer (InVia Confocal Raman Microscope, Renishaw), scanning electron microscope (SEM, Ultra 55, Zeiss), atomic force microscope (AFM), X-ray photoelectron spectrometer (XPS, PHI 5000 Versa Probe, ULVAC-PHI, INC.), UV-Vis spectrophotometer (TU-1901, PERSEE), electrochemical workstation (CHI660D, Shanghai Chenhua Instrument Co., Ltd.), Xe lamp (PLS-SXE300, Beijing Changtuo Co., Ltd.). Materials include acetone, ethanol, deionized water, Ar and O2 gases, Cu and W targets (
4:99% purity), Na2SO4 electrolyte. Experimental Procedures and Operational Workflow:
The FTO substrate was cleaned ultrasonically. CuOx was deposited first by sputtering Cu target in Ar/O2 atmosphere, followed by WO3 deposition using W target. Annealing was performed under specified conditions. Photoelectrodes were fabricated by connecting copper wire to FTO. Characterization involved XRD, Raman, SEM, AFM, XPS, UV-Vis, and photoelectrochemical tests using a three-electrode system with Pt counter electrode and Ag/AgCl reference electrode in Na2SO4 electrolyte under light illumination.
5:Data Analysis Methods:
Data were analyzed using techniques such as Kubelka-Munk function for bandgap calculation, Mott-Schottky plots for carrier concentration and flat band potential, and equivalent circuit fitting for electrochemical impedance spectroscopy (EIS).
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X-ray diffractometer
D/max-500
Rigaku Co.
Analyze the crystalline structures of the sputtered CuOx/WO3 thin-films.
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Scanning electron microscope
Ultra 55
Zeiss
Characterize the morphology and element mapping of the CuOx/WO3 thin-film.
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Raman spectrometer
InVia Confocal Raman Microscope
Renishaw
Record Raman spectra in the spectral range of 20-1400 cm-1 with 633 nm excitation wavelength.
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X-ray photoelectron spectrometer
PHI 5000 Versa Probe
ULVAC-PHI, INC.
Analyze the element composition, chemical and electronic state of the CuOx/WO3 thin-film.
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UV-Vis spectrophotometer
TU-1901
PERSEE
Investigate the optical properties of the CuOx/WO3 photocathodes.
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Electrochemical workstation
CHI660D
Shanghai Chenhua Instrument Co., Ltd.
Perform photoelectrochemical tests, including volt-ampere curves, Mott-Schottky plots, and electrochemical impedance spectroscopy.
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Xe lamp
PLS-SXE300
Beijing Changtuo Co., Ltd.
Serve as the incident light source for photoelectrochemical tests with an intensity of 100 mW cm-2.
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