研究目的
Investigating the importance of synthesis conditions on the structural and photocatalytic properties of tantalum oxide nitride by comparing two variants of phase-pure β-TaON obtained from different synthesis routes.
研究成果
The synthesis conditions significantly affect the microstructure of β-TaON, with strained samples showing reduced photocatalytic and photoelectrochemical activity due to lattice defects acting as charge carrier traps. High crystallinity and defect minimization are crucial for optimal performance in water splitting applications.
研究不足
The study is limited to β-TaON and may not generalize to other materials. The synthesis conditions are specific, and defects introduced might vary with scale or other parameters. Photocatalytic performance could be influenced by factors not fully controlled, such as impurity levels or electrode fabrication consistency.
1：Experimental Design and Method Selection:
The study compares two synthesis routes for β-TaON, involving ammonolysis of Ta2O5 under controlled conditions, followed by structural characterization using XRD, neutron diffraction, HRTEM, and catalytic testing via photochemical and photoelectrochemical methods.
2：Sample Selection and Data Sources:
Samples were synthesized from Ta2O5 precursor, with two variants (unstrained and strained β-TaON) produced under different temperature and gas flow conditions.
3：List of Experimental Equipment and Materials:
Equipment includes tube furnace, mass flow controllers, X-ray diffractometer (Panalytical X'Pert PRO), neutron diffractometer (SPODI), SEM (Hitachi SU8030), TEM (FEI Titan 80-300), UV/Vis spectrometer (JASCO V670), mass spectrometer (Pfeiffer QMS200 OmniStar), potentiostat (Biologic SP-150), and Xe lamp (SCHOTT KL 1500). Materials include Ta2O5, ammonia, oxygen, AgNO3, La2O3, TaCl5, FTO glass, and CoPi catalyst.
4：0). Materials include Ta2O5, ammonia, oxygen, AgNO3, La2O3, TaCl5, FTO glass, and CoPi catalyst. Experimental Procedures and Operational Workflow:
4. Experimental Procedures and Operational Workflow: Synthesis involved heating Ta2O5 in ammonia and oxygen flows, followed by cooling. Characterization included XRD Rietveld refinement, neutron diffraction, TEM imaging, UV/Vis spectroscopy, and catalytic tests in batch reactors and electrochemical cells with light irradiation.
5：Data Analysis Methods:
Data were analyzed using FullProf suite for structural refinement, Kubelka-Munk function for optical properties, and transient analysis for photoelectrochemical kinetics.
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X-ray diffractometer
X'Pert PRO
Panalytical
Used for X-ray powder diffraction measurements to characterize the crystal structure of β-TaON samples.
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SEM
SU8030
Hitachi
Used for scanning electron microscopy to characterize the morphology of TaON powders and electrodes.
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TEM
Titan 80-300
FEI
Used for high-resolution transmission electron microscopy to image lattice defects in β-TaON samples.
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UV/Vis spectrometer
V670
JASCO
Used for diffuse reflectance spectroscopy to measure optical band gaps of powder samples.
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Xe lamp
KL 1500 electronics
SCHOTT
Used as a light source for photocatalytic and photoelectrochemical experiments.
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Hot gas extraction analyzer
TC-300/EF-300
LECO
Used for determining nitrogen and oxygen contents in samples.
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Neutron diffractometer
SPODI
Forschungs-Neutronenquelle Heinz-Maier-Leibnitz
Used for neutron powder diffraction to investigate anion ordering in β-TaON samples.
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Mass spectrometer
QMS200 OmniStar
Pfeiffer
Used for gas analysis in photocatalytic water oxidation tests to measure oxygen evolution.
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Potentiostat
SP-150
Biologic
Used for controlling electrode potential in photoelectrochemical measurements.
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Mass flow controller
Brooks Instruments
Used to adjust flow rates of reaction gases during synthesis.
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