1.preparation method of porous Fe2O3 nanotubes
Weigh a certain mass of polyvinylpyrrolidone and dissolve it in N, N-dimethylformamide. When stirring at room temperature for 12h, prepare a viscous solution with a mass fraction of 17%. Weigh 0.2g, 0.3g, 0.4g and 0.5g acetylacetone iron (0.5g acetylacetone drill) and add 3G of the above prepared viscous solution respectively, and stir at room temperature for 12h. Put the transparent and uniform spinning solution into the syringe with polished stainless steel needle, install the syringe with spinning solution on the electrospinning device, and electrospun the fiber film of non-woven fabric after setting the electrospinning parameters. The specific spinning parameters are: the electrostatic voltage applied between the spinneret and the receiving plate is 15kV, the vertical distance between the spinneret and the receiving plate is 12cm, the propulsion speed of the syringe pump is set to 1.0ml/h, and the flat plate receiving device coated with aluminum foil is adopted.
The prepared non-woven film was placed in a tubular furnace, calcined at 500 ℃ for 3h at a heating rate of 1 ℃ / min in air atmosphere, and then naturally cooled to room temperature. The samples were taken out for characterization and performance test.
- Characterization of porous Fe2O3 nanotubes
The morphology of the samples was analyzed by Fei tacnaig2 transmission electron microscope and hitachis4800 field emission scanning electron microscope. German Bruker D8 X-ray diffractometer, Cuk α Ray（ λ= 1.5406) test material structure. Sta449f3 thermogravimetric and differential thermal (TG / DSC) synchronous analyzer produced by Netzsch company in Germany is used to test the thermal analysis curve of the sample in air atmosphere. The heating rate is 5 ℃ / min and the cooling is a natural cooling process. Escalabmk Ⅱ photoelectron spectrometer of thermo company of the United States. The ray source is ALK α X-ray, with C1s (284.6ev) as the correction standard, the test vacuum is less than 10-8pa, the working voltage is 12kV, the current is 20mA, and the step size is 0.1eV. Micromeritics asap-2000 specific surface analyzer is used to measure the specific surface area and pore size distribution of materials.
- Electrochemical properties of porous Fe2O3 nanotubes
Mix the active substance, adhesive (PVDF) and conductive agent (acetylene black) in the mass ratio of 7:2:1, add N-methylpyrrolidone (NMP) and grind for a period of time to make the mixture mix evenly in the mortar. Then it was coated on copper foil and dried at 80 ℃ for 8h. An electrode sheet with a diameter of 12cm was formed by punching mechanism and weighed. A 2025 button battery was assembled in the glove box, using lithium sheet as the counter electrode and reference electrode, celgard2400 diaphragm and LiPF6 (1mol / L) / EC: DMC (1:1, mass ratio) as the electrolyte. Conduct cyclic voltammetry and constant current charge discharge test on the battery. The cyclic voltammetry test is conducted by vmp3 electrochemical workstation of biological company, and the constant current charge discharge test is conducted by the charge discharge instrument of Wuhan blue power company.
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