研究目的
To synthesize a new photocatalyst with dehydronitrization of GaOOH under NH3 flow for hydrogen evolution from water under visible light irradiation, as a preliminary step for CO2 reduction.
研究成果
A new photocatalyst with GaNyO3-x-like phase was successfully produced by dehydronitrization of GaOOH at 1173 K, showing stable photocatalytic H2 evolution under visible light. Only this sample maintained its structure after reaction, while others oxidized. Thermodynamically, nitrogen in such a phase is more stable than in GaN, suggesting the existence of a stable gallium oxynitride phase resistant to oxidation in water.
研究不足
The reason for photocatalytic activity only at 1173 K is not fully understood. Samples at other temperatures are unstable and oxidize to GaOOH during reaction. The exact chemical state and microstructure of the active phase (GaNyO3-x) are not clear, requiring further study on optimal nitriding conditions and starting materials.
1：Experimental Design and Method Selection:
Dehydronitrization of GaOOH under NH3 flow at various temperatures to produce nitrogen-doped Ga2O3 or GaN-like phases. Photocatalytic activity tested for H2 evolution from aqueous methanol solution under visible light irradiation.
2：Sample Selection and Data Sources:
GaOOH synthesized hydrothermally from Ga(NO3)3·8H2O and aqueous ammonia. Dehydronitrization temperatures from 773 K to 1273 K.
3：List of Experimental Equipment and Materials:
Autoclave for hydrothermal synthesis, NH3 gas flow system, Xe lamp with cut filter for visible light irradiation, UV-visible spectrophotometer (JASCO V-670), XRD (Rigaku MiniFlex600), SEM (JSM-6500F FE-SEM), XAFS at synchrotron facilities, gas chromatograph (Shimadzu GC-8APT). Materials include Ga(NO3)3·8H2O (Kishida Chemical), aqueous ammonia (Kishida Chemical), H2PtCl6 (Wako Pure Chemical), BaSO4 (Kishida Chemical).
4：Experimental Procedures and Operational Workflow:
Synthesis of GaOOH via hydrothermal treatment at 393 K for 6 h. Dehydronitrization under NH3 flow (60 mL/min) at specified temperatures for 15 h. Pt loading by photodeposition. Photocatalytic H2 evolution test in reactor cell with He flow and visible light irradiation (λ > 420 nm, 127 mW/cm2). Characterization using XRD, UV-vis, SEM, XAFS before and after reactions.
5：2). Characterization using XRD, UV-vis, SEM, XAFS before and after reactions. Data Analysis Methods:
5. Data Analysis Methods: XRD for crystalline structure, UV-vis spectra converted to Kubelka-Munk function, XAFS for local structure analysis, GC-TCD for H2 quantification.
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UV-visible spectrophotometer
V-670
JASCO
Measurement of diffuse reflectance UV-visible spectra for optical property analysis.
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X-ray diffractometer
MiniFlex600
Rigaku
XRD analysis for crystalline structure determination.
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FE-SEM
JSM-6500F
JEOL
Scanning electron microscopy for morphology observation.
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Gas chromatograph
GC-8APT
Shimadzu
Detection of H2 gas with thermal conductivity detector.
GC-8A Series Gas Chromatograph
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Xe lamp
300 W
Light source for visible light irradiation in photocatalytic tests.
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Autoclave
Teflon-lined
Hydrothermal synthesis of GaOOH.
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