Hard carbon negative electrode material for lithium ion secondary battery and preparation method of hard carbon negative electrode material
A negative electrode material, secondary battery technology, applied in secondary batteries, battery electrodes, chemical instruments and methods, etc., can solve the problems of high-rate continuous charge-discharge capacity and low-temperature performance, which are difficult to effectively improve, and the theoretical specific capacity of graphite negative electrodes is low. , to reduce irreversible lithium ion loss, mature the preparation process and equipment, and improve the specific capacity
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[0046] In the embodiment of the present application, the present invention also provides a preparation method of a hard carbon negative electrode material for a lithium ion secondary battery, the hard carbon negative electrode material includes the hard carbon negative electrode material for a lithium ion secondary battery as described above. A carbon negative electrode material, the method comprising the steps of:
[0047] Preparation of hard carbon raw materials, phosphorus-containing dopants and polymers;
[0048] Coarsely crushing the hard carbon raw material and obtaining coarse crushed material;
[0049] Calcining the coarse crushed material at 200°C-500°C for 1h-10h in an inert gas environment to obtain a first calcined material;
[0050] Pickling the first calcined material with dilute hydrochloric acid with a mass fraction lower than 15%;
[0051] Drying, pulverizing and sieving the first calcined material after pickling in sequence to obtain a hard carbon precursor...
Embodiment 1
[0063] In the embodiment of the present application, a method for preparing a hard carbon negative electrode material for a lithium-ion secondary battery provided by the present application specifically includes the following steps:
[0064] (1) Take 10kg of coconut shell (hard carbon raw material) and carry out coarse crushing. The average size of the particles after coarse crushing is about 2mm, and then put it in a box-type furnace, and feed nitrogen for protection until the oxygen content in the box-type furnace is low. At 100ppm, heat up to 450°C and calcined for 2 hours to obtain 3.5kg of burnt material, then place the burnt material in dilute hydrochloric acid with a mass fraction of 10%, soak it, stir slowly for 2 hours, and then perform centrifugation. The obtained powder was dried and then pulverized to obtain a particle size D50 of 7.2 μm after pulverization. Then sieve to remove large particles, and the mesh size of the sieve is 325 mesh to obtain a hard carbon pre...
Embodiment 2
[0068] The difference from Example 1 is that the hard carbon raw material is phenolic resin, the particle size after coarse crushing is 3mm, the pre-carbonization temperature is 500°C, the pre-carbonization time is 4h, the pre-carbonization atmosphere is a nitrogen atmosphere, and the pickling process uses What is more important is that the mass fraction of dilute hydrochloric acid is lower than 12%, and after centrifugation, drying, and crushing, the particle size D50 of the hard carbon precursor obtained is 9.1 μm.
[0069] The phosphorus-containing dopant is ammonium phosphate, the mass ratio of hard carbon precursor to ammonium phosphate is 100:18, the mixing method is liquid phase mixing, and then drying, the dried material is calcined in nitrogen gas, and the calcining temperature is 400 ℃, the calcination time is 3h.
[0070] After burning, the material is broken up and sieved to obtain a particle size D50 of 9.5 μm. Polyaniline is used for compounding to cover the surf...
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