研究目的
To develop a novel two-dimensional black TiO2 ? x nanosheet with enhanced lithium-storage capacity and visible light photocatalytic hydrogen production for applications in energy storage and environmental management.
研究成果
The novel black TiO2 ? x nanosheets exhibit superior lithium-storage capacity with a reversible specific capacity of 160 mA h g?1 after 300 cycles at 0.5 C and enhanced visible-light photocatalytic hydrogen production. This material has potential applications in energy storage and environmental management, and the synthesis method can be extended to other TiO2-based nanomaterials.
研究不足
The coulombic efficiency of the black TiO2 ? x NS electrode decreased due to side reactions from increased -OH groups. The photocatalytic H2 production amount is low compared to other high-efficiency photocatalysts, and aggregation during reduction reduced surface area slightly.
1:Experimental Design and Method Selection:
A facile solvothermal method was used to synthesize white TiO2 nanosheets, followed by a solid-phase NaBH4 reduction method to produce black TiO2 ? x nanosheets under moderate temperature.
2:Sample Selection and Data Sources:
Samples were prepared using hydrofluoric acid and titanium butoxide for solvothermal synthesis, and sodium borohydride for reduction.
3:List of Experimental Equipment and Materials:
Equipment includes Teflon-lined stainless steel autoclave, horizontal tube furnace, Bruker D8 Advance XRD, JEM1400plus TEM, SPI3800/SPA400 AFM, PHI 5000 VersaProbe XPS, Lambda 750 UV/Vis/NIR spectrometer, FTIR spectrometer, Bruker EMX-10/12 EPR, Micrometrics ASAP 2020 analyzer, Neware BTS-5 V 50 mA battery tester, CEL-SPH2N photocatalytic system, CEL-PF300-T8 xenon arc lamp, GC7920-TF2Z gas chromatograph. Materials include HF, TBOT, NaBH4, N2 gas, HCl, ethanol, water, graphite, PVDF binder, NMP solvent, Cu foil, LiPF6 electrolyte, EC/DMC mixture.
4:Experimental Procedures and Operational Workflow:
For TiO2 NS synthesis, HF was added to TBOT, stirred, autoclaved at 190°C for 24h, centrifuged, washed with ethanol, dried. For TiO2 ? x NS, NaBH4 and TiO2 NS were ground, heated at 300°C under N2 for 1h, stirred in HCl, washed, dried. Characterizations included XRD, TEM, HR-TEM, AFM, XPS, UV-Vis-NIR DRS, FTIR, EPR, N2 sorption. Electrochemical tests used CR2025 cells with active material, graphite, PVDF on Cu foil, tested with Neware device. Photocatalytic tests used
5:5 mg sample in water under visible light from xenon lamp with UV-cutoff filter, H2 analyzed by GC. Data Analysis Methods:
Data were analyzed using instrument-specific software for XRD, TEM, XPS, etc.; electrochemical data analyzed for capacity and cycling performance; photocatalytic data analyzed for H2 production rates.
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X-ray diffraction instrument
D8 Advance
Bruker
Used for XRD measurements to analyze crystal structure of samples.
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EPR apparatus
EMX-10/12
Bruker
Used for EPR analysis to detect oxygen deficiencies and Ti3+ species.
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Transmission electron microscope
JEM1400plus
Japan (likely JEOL, but not specified)
Used for TEM and HR-TEM imaging to characterize morphology and structure of nanosheets.
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Atomic force microscope
SPI3800/SPA400
Seiko Inc.
Used for AFM in contact mode to measure thickness and surface topography of nanosheets.
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X-ray photoelectron spectrometer
PHI 5000 VersaProbe
PHI (Physical Electronics)
Used for XPS measurements to analyze element composition and valence states.
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UV/Vis/NIR spectrometer
Lambda 750
PerkinElmer (inferred, not specified)
Used for UV-Vis-NIR diffuse reflectance spectra measurements to analyze light absorption.
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FTIR spectrometer
Vector 22
Bruker (inferred, not specified)
Used for FTIR spectra measurements with KBr pellet method to analyze chemical bonds.
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Nitrogen sorption analyzer
ASAP 2020
Micromeritics
Used for N2 sorption isotherms at 77 K to measure specific surface area.
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Battery testing device
BTS-5 V 50 mA
Neware
Used for electrochemical measurements of lithium ion batteries at constant current mode.
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Photocatalytic water splitting testing system
CEL-SPH2N
AULTT
Used for photocatalytic H2 production experiments under visible light irradiation.
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Xenon arc lamp
CEL-PF300-T8
AULTT
Used as a visible light source for photocatalytic reactions, with UV-cutoff filter.
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Gas chromatograph
GC7920-TF2Z
AULTT
Used to analyze H2 content in photocatalytic experiments.
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Autoclave
Teflon-lined stainless steel
Used for solvothermal synthesis of TiO2 nanosheets at high temperature and pressure.
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Tube furnace
Horizontal
Used for heat treatment under N2 atmosphere for reduction reactions.
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