研究目的
To investigate the structural transformation and catalytic mechanism of sputtered amorphous MoSx as an efficient hydrogen evolution catalyst during electrochemical activation.
研究成果
Amorphous MoSx films deposited at room temperature exhibit the highest catalytic activity for hydrogen evolution after electrochemical activation, with an overpotential of 180 mV at -10 mA/cm2. The activation involves structural transformation from amorphous Mo3S13/Mo3S12 clusters to sulfur-deficient MoS2-x nano-islands, with H2S release and formation of catalytically active edge sites. This provides insights for improving earth-abundant hydrogen evolution catalysts.
研究不足
The study is limited to MoSx films on FTO substrates; long-term stability shows degradation over time. The catalytic mechanism is not fully elucidated, and further experiments are needed to confirm the rate-limiting steps and optimize performance.
1：Experimental Design and Method Selection:
Reactive magnetron sputtering was used to deposit MoSx films on FTO substrates at varying temperatures (RT to 500°C). Electrochemical measurements, Raman spectroscopy, XPS, DEMS, and in-situ Raman were employed to study catalytic activity and structural changes.
2：Sample Selection and Data Sources:
FTO substrates were used; samples were prepared by sputtering and characterized using SEM, XRD, Raman, XPS, and TEM.
3：List of Experimental Equipment and Materials:
Molybdenum target (99.99%, Freiberger NE-Metall GmbH), FTO substrates, H2S/Ar gas mixture, potentiostat (VersaSTAT), SEM (LEO GEMINI 1530, ZEISS), TEM (Philips CM12/STEM), XPS (SPECS PHOIBOS 100), Raman spectrometers (Horiba XploRA, DILOR LabRAM), XRD (Bruker AXS D8 Advance), DEMS system (QMG 220 M1, PrismaPlus).
4：99%, Freiberger NE-Metall GmbH), FTO substrates, H2S/Ar gas mixture, potentiostat (VersaSTAT), SEM (LEO GEMINI 1530, ZEISS), TEM (Philips CM12/STEM), XPS (SPECS PHOIBOS 100), Raman spectrometers (Horiba XploRA, DILOR LabRAM), XRD (Bruker AXS D8 Advance), DEMS system (QMG 220 M1, PrismaPlus). Experimental Procedures and Operational Workflow:
4. Experimental Procedures and Operational Workflow: Substrates were cleaned, sputtered at different temperatures, and characterized. Electrochemical measurements were performed in a three-electrode setup with 0.5 M H2SO4 electrolyte. CV, Tafel analysis, capacitance measurements, and DEMS were conducted. In-situ Raman and XPS were used to monitor changes during cycling.
5：5 M H2SO4 electrolyte. CV, Tafel analysis, capacitance measurements, and DEMS were conducted. In-situ Raman and XPS were used to monitor changes during cycling. Data Analysis Methods:
5. Data Analysis Methods: Data were analyzed using Scherrer's equation for particle size, Tafel slopes for reaction mechanisms, and XPS/Raman for chemical and structural changes.
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FESEM
LEO GEMINI 1530
ZEISS
Used for morphology measurement of the films.
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molybdenum target
99.99%
Freiberger NE-Metall GmbH
Used in reactive magnetron sputtering to deposit MoSx films.
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HRTEM
Philips CM12/STEM
Philips
Used for high-resolution transmission electron microscopy of amorphous MoSx electrodes.
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XPS analyzer
PHOIBOS 100
SPECS
Used to study composition and valence state of elements in the films.
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Raman spectrometer
XploRA
Horiba
Used for Raman spectroscopy measurements.
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Raman spectrometer
DILOR LabRAM
DILOR
Used for in-situ Raman measurements.
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X-ray diffractometer
D8 Advance
Bruker AXS
Used for glancing incidence X-ray diffraction.
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Potentiostat
VersaSTAT
Used for electrochemical measurements in a three-electrode configuration.
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Mass spectrometer
QMG 220 M1
PrismaPlus
Part of the DEMS system to measure gases released during electrochemical measurements.
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