研究目的
To study the effect of voltage on the formation and crystalline phase of TiO2 nanotubes in ethylene glycol solution without heat treatment.
研究成果
Higher anodization voltages (40 V and 60 V) promote the formation of crystalline anatase TiO2 nanotubes without heat treatment, attributed to oxygen vacancies and ionic mobilities. This provides a simple method for producing various TiO2 nanostructures with potential for high-performance applications.
研究不足
The study is limited to specific electrolyte composition and voltage ranges; the amorphous nature at lower voltages and potential for tube rupture at higher voltages may affect application performance. Further optimization of parameters and scalability for industrial use are not addressed.
1：Experimental Design and Method Selection:
The experiment involved anodizing Ti foils in an ethylene glycol-based electrolyte with NH4F and H2O2 at different voltages to form TiO2 nanotubes, followed by characterization using FESEM, XRD, and Raman spectroscopy to analyze morphology and crystallinity.
2：Sample Selection and Data Sources:
Ti foils (99.5% purity, 0.25 mm thickness) were cut into 1 cm x 3 cm pieces, degreased by sonication in ethanol and distilled water, and dried before anodization.
3：5% purity, 25 mm thickness) were cut into 1 cm x 3 cm pieces, degreased by sonication in ethanol and distilled water, and dried before anodization.
List of Experimental Equipment and Materials:
3. List of Experimental Equipment and Materials: Ti foils, ethylene glycol, ammonium fluoride (NH4F), hydrogen peroxide (H2O2), ethanol, distilled water, deionized water, high-voltage potentiostat (Instek GPC 6030D), graphite cathode, field emission scanning electron microscope (FESEM, Hitachi, Japan), x-ray diffractometer (Analytical X’Pert Pro with Cu Kα radiation), Raman spectrometer (LabRAM HR800 with 532 nm laser excitation).
4：Experimental Procedures and Operational Workflow:
Ti foils were anodized for 60 minutes in ethylene glycol with 5% H2O2 and 0.3 wt% NH4F at voltages of 10 V, 40 V, and 60 V using a two-electrode configuration with graphite cathode. After anodization, some samples were annealed at 450 °C for 2 hours in air with a heating rate of 10 °C/min. Morphology was analyzed by FESEM, crystalline phase by XRD, and structure by Raman spectroscopy.
5：3 wt% NH4F at voltages of 10 V, 40 V, and 60 V using a two-electrode configuration with graphite cathode. After anodization, some samples were annealed at 450 °C for 2 hours in air with a heating rate of 10 °C/min. Morphology was analyzed by FESEM, crystalline phase by XRD, and structure by Raman spectroscopy.
Data Analysis Methods:
5. Data Analysis Methods: XRD patterns and Raman spectra were analyzed to identify crystalline phases and structural changes; FESEM images were used to observe nanotube morphology and dimensions.
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