研究目的
To develop an original, halide-free non-hydrolytic sol-gel route for synthesizing mesoporous anatase TiO2 with high specific surface area and evaluate its electrochemical lithium storage performances.
研究成果
The reaction provides an efficient, non-hydrolytic route to highly condensed nanocrystalline TiO2 with high surface area and excellent lithium storage performance. Residual acetate groups do not hinder cycling, and solvent addition allows morphology tuning but reduces surface area and performance. The route is promising for extension to other metal oxide systems.
研究不足
The role of organic species during nanoparticle growth is not well understood, limiting predictability of morphology when solvents are used. The method may have constraints in scalability or application to other metal oxides without further optimization.
1：Experimental Design and Method Selection:
The study revisits the use of acetic anhydride as an oxygen donor in a non-hydrolytic sol-gel synthesis. Reactions were conducted at 200°C without catalyst or solvent, based on ester elimination mechanisms.
2：Sample Selection and Data Sources:
Titanium (IV) isopropoxide and acetic anhydride were used as precursors. Samples were prepared with and without solvents (toluene or squalane) and before/after calcination.
3：List of Experimental Equipment and Materials:
Materials included Ti(OiPr)4, Ac2O, squalane, toluene, acetone, and commercial TiO
4：Equipment included autoclaves, ovens, spectrometers (NMR, FTIR, XRD), microscopes (SEM, TEM), physisorption apparatus, thermogravimetric analyzer, and electrochemical testers. Experimental Procedures and Operational Workflow:
Precursors were mixed in an autoclave, heated at 200°C for 12h, washed with acetone, dried, and optionally calcined. Characterization involved NMR, FTIR, XRD, SEM, TEM, nitrogen physisorption, and electrochemical testing.
5：Data Analysis Methods:
Data were analyzed using Scherrer equation for crystallite size, BET method for surface area, BJH/DFT for pore size, equivalent circuit modeling for EIS, and b-value analysis for cyclic voltammetry.
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Spectrum II spectrometer
Spectrum II
Perkin-Elmer
FTIR spectroscopy
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X'Pert Pro MPD diffractometer
X'Pert Pro MPD
PANalytical
XRD analysis
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S-4800 electron microscope
S-4800
Hitachi
SEM imaging
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JEM-ARM 200F transmission electron microscope
JEM-ARM 200F
JEOL
TEM imaging
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AVANCE spectrometer
AVANCE
Bruker
NMR spectroscopy
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Titanium (IV) isopropoxide
Sigma-Aldrich
Precursor for TiO2 synthesis
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Acetic anhydride
Sigma-Aldrich
Oxygen donor in sol-gel synthesis
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Squalane
Alfa Aesar
Solvent in synthesis
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Toluene
Sigma-Aldrich
Solvent in synthesis
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PureSolve MD5 solvent purification system
MD5
PureSolve
Drying solvent to remove water
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Karl Fischer coulometer
Measuring water content
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Stainless steel digestion vessel
Reaction container
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Triflex apparatus
Triflex
Micromeritics
Nitrogen physisorption
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VNMRS spectrometer
VNMRS
VARIAN
Solid state NMR
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BTS3000 instrument
BTS3000
Neware Battery
Galvanostatic electrochemical testing
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Pulverisette 7 Planetary Micro Mill
Pulverisette 7
Fritsch
Ball-milling slurry
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3540 bird film applicator
3540
Elcometer
Tape casting electrodes
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VSP-300 instrument
VSP-300
Cyclic voltammetry and EIS measurements
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