A kind of fibrous hollow hard carbon material that can be used for sodium ion battery negative electrode and preparation method thereof
A sodium-ion battery, fibrous technology, applied in nanotechnology for materials and surface science, battery electrodes, carbon preparation/purification, etc., can solve the problems of not achieving optimal kinetic performance and increasing preparation costs, etc. Achieve the effect of improving resource utilization, good structural stability, and wide sources
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Embodiment 1
[0047] A kind of preparation method of fibrous hollow hard carbon material, the process flow of its preparation method is as follows figure 1 It includes the following steps:
[0048] Step 1) Pretreatment of raw materials, the fibrous part of the biomass is taken out, washed, dried and placed in a graphite crucible, and pre-carbonized at a heating rate of 5°C / min under a protective atmosphere of 600°C for 2 hours Post-grinding to prevent the hard carbon material from being hardened after direct pyrolysis, which makes it difficult to refine, to obtain a precursor, and the biomass is kapok fiber, poplar fiber, catkin fiber, sycamore fiber, ramie or jute;
[0049] Step 2) High temperature cracking, placing the precursor obtained in step 1 in a graphite crucible, at a heating rate of 5°C / min, pyrolyzing at a high temperature for 2 hours in a protective atmosphere, cooling naturally, taking out and grinding to obtain fibrous hollow hard carbon Material.
Embodiment 2
[0051] This embodiment provides a method for electrochemically testing the prepared fibrous hollow hard carbon material. The electrochemical test process is to make a pole piece for the anode material of the sodium ion battery and assemble it into a button-type battery to test its electrochemical performance. The hard carbon material and the sodium carboxymethyl cellulose binder solution are mixed uniformly in a ratio of 95:5 to obtain a slurry, which is coated on aluminum foil, placed in a vacuum oven at 100 °C for 2 hours, and dried and cut into a size of Φ10mm , get the required negative electrode sheet, the active material loading is 2mg / cm 2 about. The electrolyte system uses 1mol / L sodium perchlorate electrolyte, the solvent is ethylene carbonate and divinyl carbonate mixed in a volume ratio of 1:1 and 1mol / L sodium perchlorate electrolyte, and the solvent is ethylene carbonate, carbonic acid Divinyl ester and fluoroethylene carbonate (FEC) were mixed in a volume ratio...
Embodiment 3
[0053] A preparation method of a fibrous hollow hard carbon material, the steps not specifically described in the specific steps are the same as the method preparation material in Example 1, the difference is: the raw material of the step 1 is jute fiber; the step 2 The temperature of the pyrolysis is 1200°C; the atmosphere of the steps 1 and 2 is argon.
[0054] The fibrous hollow hard carbon material prepared in Example 3 was tested by X-ray diffraction (XRD), and the results were as follows figure 2 As shown in the figure, two severely broadened diffraction peaks of the amorphous carbon curve can be obtained, and the graphite interlayer spacing is 0.3697 nm, which is favorable for the storage of sodium ions.
[0055] The fibrous hollow hard carbon material prepared in Example 3 was tested by Raman spectroscopy, and the results were as follows image 3 As shown, the integrated intensity ratio of the two peaks is I D / I G It is 1.6337, indicating that the material still m...
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Abstract
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