US 12,275,649 B1
Lithium manganese iron phosphate substrate, cathode material, preparation method, and lithium battery
Tao Chen, Xiangtan (CN); Fenglei Yu, Xiangtan (CN); Tao Lin, Xiangtan (CN); and Jiangtao Cheng, Xiangtan (CN)
Assigned to Hunan Yuneng new energy battery materials Co., LTD., Hunan (CN)
Filed by Hunan Yuneng new energy battery materials Co., LTD., Xiangtan (CN)
Filed on Dec. 3, 2024, as Appl. No. 18/967,354.
Claims priority of application No. 202410174804.7 (CN), filed on Feb. 7, 2024.
Int. Cl. C01B 25/45 (2006.01); B82Y 30/00 (2011.01); B82Y 40/00 (2011.01); C01G 49/00 (2006.01); H01M 4/36 (2006.01); H01M 4/48 (2010.01); H01M 4/58 (2010.01); H01M 4/583 (2010.01); H01M 4/62 (2006.01); H01M 10/0525 (2010.01)
CPC C01G 49/009 (2013.01) [H01M 10/0525 (2013.01); C01P 2004/03 (2013.01); C01P 2006/40 (2013.01)] 8 Claims
OG exemplary drawing
 
1. A preparation method of a cathode material, characterized in that the preparation of the cathode material comprises the following steps:
B1. placing lithium manganese iron phosphate substrate in a dry coating machine, adding coating agent and mixing, then adding carbon source and mixing to obtain mixture C;
B2. calcining the mixture C in a protective atmosphere, crushing it to obtain the cathode material;
the coating agent comprises at least one of metal oxide and metal salt,
the carbon source comprises a composite carbon source;
the preparation of the composite carbon source comprises the following steps:
(1) mixing sulfuric acid aqueous solution and nitric acid aqueous solution, adding carbon nanotubes, performing ultrasonic dispersion, adding deionized water, conducting temperature-controlled stirring, performing suction filtration, taking solid phase and dry it to obtain acidified carbon nanotubes;
wherein the dosage ratio of the sulfuric acid aqueous solution, the nitric acid aqueous solution, the carbon nanotube, and the deionized water is 300-450 mL: 100-150 mL: 0.8-1.2 g: 500 mL;
(2) adding reed pulp and potassium permanganate to the sulfuric acid aqueous solution, stirring, performing a temperature-controlled reaction, centrifugal washing, ultrasonically crushing, separating, taking solid phase to add into deionized water, stirring for 15-30 minutes, and performing homogenization treatment 3-4 times under 300 bar pressure to obtain nanocellulose gel, which is sealed and stored at 4° C. for later use;
wherein the dosage ratio of the sulfuric acid aqueous solution, the reed pulp, the potassium permanganate, and the deionized water is 50-80 mL: 1-2 g: 8-12.8 g: 200 mL; the temperature-controlled reaction refers to a reaction at 50° C. for 2-3 hours;
(3) mixing the acidified carbon nanotubes, the nanocellulose gel, and the deionized water, and performing ultrasonic dispersion in an ice-water bath to obtain a carbon-containing mixture solution;
wherein the dosage ratio of the acidified carbon nanotubes, the nanocellulose gel, and the deionized water is 4-7 mg: 2-6 mL: 20-40 mL; the ultrasonic dispersion refers to sonication at an amplitude of 650-700 W for 20-30 minutes;
(4) mixing dimethylformamide, graphene oxide, and diethylenetriamine, performing ultrasonic oscillation for 15-20 minutes, conducting a temperature-controlled reaction, filtering, and drying the solid phase to obtain modified graphene oxide;
wherein the mass ratio of the dimethylformamide, the graphene oxide, and the diethylenetriamine is 40-60:1.5-3:50-60;
the temperature-controlled reaction refers to stirring at 60° C. for 12-16 hours;
(5) taking the modified graphene oxide and deionized water, mixing and ultrasonically dispersing for 1-1.5 hours, adding the carbon-containing mixture solution, and ultrasonically dispersing for 1-2 hours to obtain a dispersion, adjusting the pH of the dispersion to 1.0-1.5, adding aniline, stirring in a 0-5° C. water bath for 1-2 hours, adding ammonium persulfate aqueous solution, reacting at 0-5° C. for 6-8 hours, performing suction filtration, taking the solid phase and drying it to obtain the composite carbon source;
wherein the mass ratio of the modified graphene oxide, the deionized water, the carbon-containing mixture solution, the aniline, and the ammonium persulfate aqueous solution is 1-2:10-20:4-6:1-1.5:2.4-3.8.