研究目的
To prepare self-hybridized graphitic carbon nitride (g-C3N4) using a room temperature deep eutectic solvent (DES) as a precursor for enhanced visible light photocatalytic activity.
研究成果
The self-hybridized g-C3N4 from DES precursors exhibits enhanced photocatalytic activity due to improved charge separation and increased active sites, providing a novel strategy for metal-free photocatalyst design with applications in environmental remediation and energy production.
研究不足
The study is limited to specific DES compositions (urea and AT mixtures) and thermal conditions; scalability and cost of DES precursors may be constraints. Potential optimizations include exploring other DES components and varying thermal parameters.
1:Experimental Design and Method Selection:
The study involves synthesizing g-C3N4 from DES precursors (urea and ammonium thiocyanate mixtures) via thermal polymerization at 550°C for 2 hours, comparing with conventional precursors (melamine, urea, AT). Methods include XRD, FTIR, XPS, UV-Vis DRS, PL spectroscopy, TEM, SEM, BET surface area analysis, TGA, and photocatalytic activity tests for RhB degradation and hydrogen evolution.
2:Sample Selection and Data Sources:
Samples include CNU (from urea), CNAT (from AT), CN2U1AT (from DES with urea:AT mass ratio 2:1), CN1U2AT (from DES with urea:AT mass ratio 1:2), and pristine g-C3N4 (from melamine). Data are obtained from laboratory experiments and characterization techniques.
3:List of Experimental Equipment and Materials:
Equipment includes X'Pert Pro powder diffractometer (XRD), Micromeritics ASAP 3020 (BET), Zeiss SIGMA (SEM), JEM-1400 and FEI Tecnai 30 (TEM/HRTEM), TG 209F1 (TGA), Thermo Nicolet Nexus spectrometer (FTIR), Qtac100 spectrometer (XPS), Varian-Cary 5000 (UV-Vis DRS), Hitachi F-7000 (PL), FLS980 fluorescence lifetime spectrophotometer (time-resolved PL), JEM-F200 with Gatan Enfina Spectrometer (EELS), CHI-660E electrochemical system (photocurrent), Shimadzu UV-2550 (UV-vis spectrophotometer), gas chromatography with TCD (hydrogen evolution). Materials include urea, ammonium thiocyanate, melamine, ethanol, triethanolamine, methanol, benzoquinone, P25 TiO2, chloroplatinic acid, Nafion solution, DI water.
4:Experimental Procedures and Operational Workflow:
Precursors are calcined at 550°C for 2 hours. DESs are prepared by grinding urea and AT mixtures. Characterization involves standard procedures for each technique. Photocatalytic tests involve RhB degradation under visible light with scavengers and hydrogen evolution with Pt cocatalyst and TEOA scavenger.
5:Data Analysis Methods:
Data are analyzed using Kubelka-Munk function for bandgaps, Langmuir-Hinshelwood model for kinetics, and fitting equations for PL lifetimes. Statistical analysis includes comparison of rates and constants.
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X'Pert Pro automatic powder diffractometer
X'Pert Pro
PANalytical
Performing powder X-ray diffraction (XRD) analysis to characterize crystal structures.
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SEM
SIGMA
Zeiss
Obtaining scanning electron microscopy images to examine morphology.
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TEM
JEM-1400
JEOL
Performing transmission electron microscopy for detailed structural analysis.
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HRTEM
Tecnai 30
FEI
High-resolution transmission electron microscopy for atomic-level imaging.
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FTIR spectrometer
Nicolet Nexus
Thermo
Recording Fourier transform infrared spectra for chemical bonding analysis.
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Fluorescence spectrophotometer
F-7000
Hitachi
Performing steady-state photoluminescence spectroscopy.
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Fluorescence lifetime spectrophotometer
FLS980
Edinburgh Instruments
Recording time-resolved PL decay curves.
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Electrochemical system
CHI-660E
CH Instruments
Performing photoelectrochemical measurements, including photocurrent.
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UV-vis spectrophotometer
UV-2550
Shimadzu
Analyzing concentration of RhB solution during photocatalytic degradation.
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ASAP 3020 apparatus
ASAP 3020
Micromeritics
Measuring nitrogen physisorption for surface area and pore size analysis.
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TGA
TG 209F1
Netzsch
Thermogravimetric analysis to study thermal decomposition.
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XPS spectrometer
Qtac100
Physical Electronics
X-ray photoelectron spectroscopy for surface composition analysis.
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UV-Vis diffuse reflectance spectrometer
Cary 5000
Varian
Recording UV-Vis diffuse reflectance spectra for optical properties.
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EELS spectrometer
Enfina Spectrometer
Gatan
Electron energy loss spectroscopy for elemental analysis.
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Xe lamp
300 W
Light source for photocatalytic reactions and photocurrent measurements.
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Gas chromatography
Analyzing evolved gases during hydrogen evolution experiments.
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