Nitrogen-doped hollow-structure graphite microsphere, composite negative electrode material and preparation method thereof
A negative electrode material, nitrogen doping technology, applied in the direction of negative electrode, structural parts, nanotechnology for materials and surface science, etc., can solve the problems of SEI film rupture, low Coulombic efficiency, material pulverization, etc., and achieve low cost , The preparation process is simple, and the effect of improving the rate performance
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[0021] The invention provides a method for preparing a nitrogen-doped hollow graphite microsphere negative electrode material, which comprises:
[0022] In the first step, the surfactant and the nitrogen-containing organic matter are dissolved in the dispersion medium to obtain a solution;
[0023] In the second step, the ultrafine graphite powder is dispersed in the solution prepared in the first step, stirred evenly, and ultrasonically treated to obtain a uniform slurry;
[0024] The third step is spray drying and granulation to obtain powder materials;
[0025] The fourth step, optionally, the powder material obtained in the third step is fully mixed with the coating material;
[0026] The fifth step, carbonization treatment;
[0027] The sixth step, cooling treatment, is prepared.
[0028] The dispersion medium in the first step is water and ethanol, and the volume ratio of water and absolute ethanol is 1:(0-0.3).
[0029] The surfactant is one or more mixtures of poly...
Embodiment 1
[0060] Dissolve the surfactant PVP accounting for 0.5% of the mass of ultrafine graphite and the melamine accounting for 2% of the mass of ultrafine graphite in a mixed solution in which the ratio of water and absolute ethanol is 4:1, and disperse 2g of ultrafine graphite powder in the above solution , stirring and ultrasonic treatment for 10-120min, the obtained homogeneous slurry is atomized, dried and granulated on a spray dryer to obtain a powder material, and the powder material is placed in a tube furnace for carbonization treatment under an argon atmosphere. The treatment temperature is 100-400°C, the heat treatment is 1-3 hours, and the carbonization is 2-5 hours at a high temperature of 600-1000°C. The obtained nitrogen-doped hollow graphite ball negative electrode material ( figure 1 ), and conductive carbon black, CMC and SBR are uniformly mixed in deionized water at a mass ratio of 8:1:0.5:0.5 to make a slurry, coated with copper foil, and after drying, rolling and...
Embodiment 2
[0062] Dissolve the surfactant PVP accounting for 0.5% of the ultrafine graphite mass and the melamine accounting for 15% of the ultrafine graphite mass in a mixed solution of water and ethanol, the ratio of water and absolute ethanol is 4:1, and disperse the ultrafine graphite powder In the above solution, carry out stirring and ultrasonic treatment for 10-120 minutes, and the obtained uniform slurry is atomized, dried and granulated on a spray dryer to obtain a powder material, and the powder material and asphalt are fully mixed, and placed in a tube Carbonization treatment under argon atmosphere in a type furnace, treatment temperature 100-400 ° C, heat treatment 1-3 hours, high temperature 600-1000 ° C, carbonization 2-5 hours. The obtained nitrogen-doped hollow graphite ball negative electrode material is uniformly mixed with conductive carbon black, CMC and SBR in deionized water at a mass ratio of 8:1:0.5:0.5 to make a slurry, coated on a copper foil, and subjected to A...
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