CN114430040A - Preparation method of low-expansion long-cycle graphite negative electrode material for lithium ion battery - Google Patents
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Abstract
The invention discloses a preparation method of a low-expansion long-cycle graphite cathode material for a lithium ion battery, which comprises the following steps of: putting natural graphite into a high-pressure carbonization furnace, introducing carbon source gas, and performing pressure rise, temperature preservation and pressure preservation to obtain gas-phase densified natural graphite; and then putting the graphite powder and asphalt into a high-efficiency mixer in proportion to mix so that the asphalt is coated on the surface of the natural graphite, and then sintering to obtain the low-expansion long-cycle graphite cathode material. The preparation method comprises the steps of fully filling gaseous carbon source gas into internal gaps of a coiled carbon layer through high pressure, carbonizing at a certain temperature to modify the inner surface of natural graphite, coating asphalt powder on the surface of the natural graphite to modify the outer surface of the natural graphite, and preparing the low-expansion long-cycle graphite cathode material.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a preparation method of a low-expansion long-cycle graphite cathode material for a lithium ion battery.
Background
With the development of science and technology and the severe energy and environmental situation faced at present, the high-end energy storage fields of pure electric or hybrid electric vehicles and the like put an urgent need on lithium ion batteries with higher energy density and power density, and the further development of the lithium ion batteries mainly depends on whether the lithium intercalation capacity and the large current rate capability of the cathode material can be greatly improved on the existing level.
The current commercialized negative electrode materials of lithium batteries are mainly modified natural graphite and artificial graphite, and although the preparation technology is quite mature, the requirements of the lithium ion batteries are gradually increased, and especially the requirements on long-cycle low-expansion of energy storage batteries are very strict. The natural graphite has abundant reserves, does not need an expensive graphitization process, better meets the requirement of the national double-carbon strategy, but has the defects of cycle and expansion all the time. In order to further improve the cycle performance of the graphite, most of the methods adopt a vacuum and pressurization method to press a modifier into the gaps of the spherical graphite, adopt isostatic pressing treatment to press various surface modifiers into the gaps of the spherical graphite, or mix natural crystalline flake graphite with molten asphalt, and then sequentially crush and shape the natural crystalline flake graphite with the asphalt coated on the surface to reduce the gaps, and the details can be seen in Chinese patent application CN107814383B, Chinese patent CN107814382B and Chinese patent CN 111232971B. Therefore, there is a need for an improvement in the existing method for preparing low-expansion long-cycle graphite negative electrode materials for lithium ion batteries.
Disclosure of Invention
In view of the above, the present invention is directed to the defects in the prior art, and the main object of the present invention is to provide a method for preparing a low-expansion long-cycle graphite negative electrode material for a lithium ion battery, which can fully coat the interior of the voids of natural graphite and has high coating efficiency.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a low-expansion long-cycle graphite negative electrode material for a lithium ion battery comprises the following steps:
(1) gas-phase densification:
placing natural graphite into a high-pressure carbonization furnace, introducing carbon source gas, raising the pressure and raising the temperature, raising the temperature to 500-700 ℃ at the temperature rise speed of 20 ℃/min under the pressure of 1-20 MPa, and keeping the temperature and the pressure for 1-4h to obtain gas-phase densified natural graphite;
(2) coating:
putting the gas-phase densified natural graphite obtained in the step (1) and asphalt into a high-efficiency mixer according to the mass ratio of 100 (2-10) for mixing for 20-80min, so that the asphalt is coated on the surface of the natural graphite to obtain coated natural graphite;
(3) carbonizing:
and (3) placing the coated natural graphite obtained in the step (2) in a nitrogen atmosphere protective furnace for sintering, raising the temperature to 1100-1500 ℃ at the heating rate of 2-25 ℃/min, preserving the heat for 3-10 hours, and removing magnetism and screening to obtain the low-expansion long-cycle graphite cathode material.
Preferably, the natural graphite in step (1) is spherical graphite, and D50 is 5-20 μm.
Preferably, the carbon source gas in the step (1) is one or a mixture of more than one of methane, acetylene, ethane, propyne and propane.
Preferably, the asphalt in the step (2) is one or a mixture of coal-based asphalt and oil-based asphalt, the softening point of the asphalt is 50-200 ℃, and the particle size D50 is 3-10 μm.
Compared with the prior art, the invention has obvious advantages and beneficial effects, and specifically, the technical scheme includes that:
firstly, fully filling gaseous carbon source gas into internal gaps of a coiled carbon layer at high pressure, carbonizing at a certain temperature to realize modification of the inner surface of natural graphite, then coating the surface of the natural graphite with asphalt powder by a common solid-phase coating method to realize modification of the outer surface of the natural graphite, and preparing the low-expansion long-cycle graphite cathode material, so that the bottleneck problems of poor cycle performance, poor safety and the like caused by that electrolyte enters internal pores after the carbon coating layer falls off when the natural graphite is used as a cathode are solved; compared with the existing isostatic pressing method, the method has the advantages that the solid asphalt is adopted to fill the gap, the carbon source of the gas can be filled into the gap more fully, the performance can be more excellent, the preparation method is simple in process, convenient to operate and few in production equipment, so that the cost is further reduced, the method is convenient to popularize and apply, and the method is beneficial to industrial production and suitable for large-scale production.
To more clearly illustrate the features and effects of the present invention, the present invention is described in detail below with reference to specific embodiments and the accompanying drawings.
Drawings
FIG. 1 is a SEM cross-sectional view of a low expansion long cycle graphite anode material prepared in example 1 of the present invention;
fig. 2 is an SEM sectional view of the graphite negative electrode material prepared in the comparative example.
Detailed Description
The invention discloses a preparation method of a low-expansion long-cycle graphite cathode material for a lithium ion battery, which comprises the following steps of:
(1) gas-phase densification:
placing natural graphite into a high-pressure carbonization furnace, introducing carbon source gas, raising the pressure and raising the temperature, raising the temperature to 500-700 ℃ at the temperature rise speed of 20 ℃/min under the pressure of 1-20 MPa, and keeping the temperature and the pressure for 1-4h to obtain gas-phase densified natural graphite; the natural graphite is spherical graphite, and the D50 is 5-20 mu m; the carbon source gas is one or more of methane, acetylene, ethane, propine and propane.
(2) Coating:
putting the gas-phase densified natural graphite obtained in the step (1) and asphalt into a high-efficiency mixer according to the mass ratio of 100 (2-10) for mixing for 20-80min, so that the asphalt is coated on the surface of the natural graphite to obtain coated natural graphite; the asphalt is coal-series asphalt or oil-series asphalt or a mixture of the coal-series asphalt and the oil-series asphalt, the softening point of the asphalt is 50-200 ℃, and the particle size D50 is 3-10 mu m.
(3) Carbonizing:
and (3) placing the coated natural graphite obtained in the step (2) in a nitrogen atmosphere protective furnace for sintering, raising the temperature to 1100-1500 ℃ at the heating rate of 2-25 ℃/min, preserving the heat for 3-10 hours, and removing magnetism and screening to obtain the low-expansion long-cycle graphite cathode material.
The invention is illustrated in more detail below in the following examples:
example 1
(1) Gas-phase densification:
putting natural graphite into a high-pressure carbonization furnace, introducing carbon source gas, raising the pressure and the temperature, raising the temperature to 500 ℃ at the temperature rise speed of 20 ℃/min under 1MPa, and keeping the temperature and the pressure for 1h to obtain gas-phase densified natural graphite; the natural graphite is spherical graphite, and the D50 is 5-20 mu m; the carbon source gas is methane.
(2) Coating:
putting the gas-phase densified natural graphite obtained in the step (1) and asphalt into a high-efficiency mixer according to the mass ratio of 100:4 for mixing for 60min, so that the asphalt is coated on the surface of the natural graphite to obtain coated natural graphite; the asphalt is a mixture of coal-series asphalt and oil-series asphalt, and has a softening point of 50-200 deg.C and a particle size D50 of 3-10 μm.
(3) Carbonizing:
and (3) placing the coated natural graphite obtained in the step (2) in a nitrogen atmosphere protective furnace for sintering, raising the temperature to 12500 ℃ at a heating rate of 10 ℃/min, preserving the temperature for 8 hours, and removing magnetism and screening to obtain the low-expansion long-cycle graphite cathode material.
Example 2
(1) Gas-phase densification:
putting natural graphite into a high-pressure carbonization furnace, introducing carbon source gas, raising the pressure and the temperature, raising the temperature to 700 ℃ at the temperature raising speed of 20 ℃/min under 20MPa, and keeping the temperature and the pressure for 4 hours to obtain gas-phase densified natural graphite; the natural graphite is spherical graphite, and the D50 is 5-20 mu m; the carbon source gas is acetylene.
(2) Coating:
putting the gas-phase densified natural graphite obtained in the step (1) and asphalt into a high-efficiency mixer according to the mass ratio of 100:3 for mixing for 30min, so that the asphalt is coated on the surface of the natural graphite to obtain coated natural graphite; the asphalt is coal-series asphalt, the softening point of the asphalt is 50-200 ℃, and the particle size D50 is 3-10 μm.
(3) Carbonizing:
and (3) placing the coated natural graphite obtained in the step (2) in a nitrogen atmosphere protective furnace for sintering, raising the temperature to 1300 ℃ at the heating rate of 8 ℃/min, preserving the heat for 5 hours, and removing magnetism and screening to obtain the low-expansion long-cycle graphite cathode material.
Example 3
(1) Gas-phase densification:
putting natural graphite into a high-pressure carbonization furnace, introducing carbon source gas, raising the pressure and the temperature, raising the temperature to 600 ℃ at the temperature rise speed of 20 ℃/min under 10MPa, and keeping the temperature and the pressure for 2 hours to obtain gas-phase densified natural graphite; the natural graphite is spherical graphite, and the D50 is 5-20 mu m; the carbon source gas is ethane.
(2) Coating:
putting the gas-phase densified natural graphite obtained in the step (1) and asphalt into a high-efficiency mixer according to the mass ratio of 100:2 for mixing for 20min, so that the asphalt is coated on the surface of the natural graphite to obtain coated natural graphite; the asphalt is oil asphalt with softening point of 50-200 deg.C and particle size D50 of 3-10 μm.
(3) Carbonizing:
and (3) placing the coated natural graphite obtained in the step (2) in a nitrogen atmosphere protective furnace for sintering, raising the temperature to 1350 ℃ at the heating rate of 15 ℃/min, preserving the heat for 4 hours, and removing magnetism and screening to obtain the low-expansion long-cycle graphite cathode material.
Example 4
(1) Gas-phase densification:
putting natural graphite into a high-pressure carbonization furnace, introducing carbon source gas, raising the pressure and the temperature, raising the temperature to 650 ℃ at the temperature raising speed of 20 ℃/min under 11MPa, and keeping the temperature and the pressure for 3 hours to obtain gas-phase densified natural graphite; the natural graphite is spherical graphite, and the D50 is 5-20 mu m; the carbon source gas is propyne.
(2) Coating:
putting the gas-phase densified natural graphite obtained in the step (1) and asphalt into a high-efficiency mixer according to the mass ratio of 100:10 for mixing for 80min, so that the asphalt is coated on the surface of the natural graphite to obtain coated natural graphite; the asphalt is coal-series asphalt with softening point of 50-200 deg.C and particle size D50 of 3-10 μm.
(3) Carbonizing:
and (3) placing the coated natural graphite obtained in the step (2) in a nitrogen atmosphere protective furnace for sintering, raising the temperature to 1400 ℃ at the heating rate of 18 ℃/min, preserving the heat for 6 hours, and removing magnetism and screening to obtain the low-expansion long-cycle graphite cathode material.
Example 5
(1) Gas-phase densification:
putting natural graphite into a high-pressure carbonization furnace, introducing carbon source gas, raising the pressure and the temperature, raising the temperature to 620 ℃ at the temperature raising speed of 20 ℃/min under 11MPa, and keeping the temperature and the pressure for 2.5h to obtain gas-phase densified natural graphite; the natural graphite is spherical graphite, and the D50 is 5-20 mu m; the carbon source gas is propane.
(2) Coating:
putting the gas-phase densified natural graphite obtained in the step (1) and asphalt into a high-efficiency mixer according to the mass ratio of 100:5 for mixing for 50min, so that the asphalt is coated on the surface of the natural graphite to obtain coated natural graphite; the asphalt is coal-series asphalt, the softening point of the asphalt is 50-200 ℃, and the particle size D50 is 3-10 μm.
(3) Carbonizing:
and (3) placing the coated natural graphite obtained in the step (2) in a nitrogen atmosphere protective furnace for sintering, raising the temperature to 1100 ℃ at the heating rate of 2 ℃/min, preserving the heat for 3 hours, and removing magnetism and screening to obtain the low-expansion long-cycle graphite cathode material.
Example 6
(1) Gas-phase densification:
putting natural graphite into a high-pressure carbonization furnace, introducing carbon source gas, raising the pressure and the temperature, raising the temperature to 550 ℃ at the temperature raising speed of 20 ℃/min under 18MPa, and keeping the temperature and the pressure for 3.5 hours to obtain gas-phase densified natural graphite; the natural graphite is spherical graphite, and the D50 is 5-20 mu m; the carbon source gas is a mixture of methane, acetylene and ethane.
(2) Coating:
putting the gas-phase densified natural graphite obtained in the step (1) and asphalt into a high-efficiency mixer according to the mass ratio of 100:7 for mixing for 30min, so that the asphalt is coated on the surface of the natural graphite to obtain coated natural graphite; the asphalt is coal-series asphalt, the softening point of the asphalt is 50-200 ℃, and the particle size D50 is 3-10 μm.
(3) Carbonizing:
and (3) placing the coated natural graphite obtained in the step (2) in a nitrogen atmosphere protective furnace for sintering, raising the temperature to 1500 ℃ at the heating rate of 25 ℃/min, preserving the heat for 10 hours, and removing magnetism and screening to obtain the low-expansion long-cycle graphite cathode material.
Performance testing
The low expansion long cycle graphite negative electrode material obtained in each example was subjected to a performance test with the graphite negative electrode material obtained in comparative example 1, which was not subjected to gas phase densification and was otherwise the same as in each example, and the test performance was as shown in table 1 below.
TABLE 1
As can be seen from Table 1, the prepared low-expansion long-cycle graphite cathode material has a small specific surface, realizes internal and external modification, and has excellent capacity performance, cycle performance, first charge-discharge efficiency, low expansion performance and rate capability. The low-expansion long-cycle graphite cathode material can replace artificial graphite to prepare a battery cathode material, and is suitable for lithium ion batteries for consumer electronic equipment such as mobile phones and digital cameras and power lithium ion batteries for electric vehicles, so that the cost is greatly reduced.
And, as can be seen from fig. 1 and 2, after the gas carbon source is densified, the large area of the gap is reduced, and the internal and external modification of the low-expansion long-cycle graphite anode material is proved.
Test method
(1) The specific surface area of the material was measured using a Micromeritics TriStar II 3020 specific surface area apparatus from Mach instruments, USA;
(2) the anode material, SBR (solid content 50%), CMC and Super-p (weight ratio) of the above examples and comparative examples are mixed with a proper amount of deionized water to form slurry, the slurry is coated on a copper foil and dried in a vacuum drying oven for 12 hours to prepare an anode piece, electrolyte is 1M, LiPF is added6And the/EC + DEC + DMC is 1: 1, the polypropylene microporous membrane is a diaphragm, the counter electrode is a lithium sheet, and the battery is assembled. And (3) carrying out a constant-current charge and discharge experiment in the LAND battery test system, limiting the charge and discharge voltage to be 0.01-3.0V, carrying out data acquisition and control by using a charge and discharge cabinet controlled by a computer, and measuring the pole piece bounce under full power.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the technical scope of the present invention, so that any minor modifications, equivalent changes and modifications made to the above embodiment according to the technical spirit of the present invention are within the technical scope of the present invention.
Claims (4)
1. A preparation method of a low-expansion long-cycle graphite cathode material for a lithium ion battery is characterized by comprising the following steps of: the method comprises the following steps:
(1) gas-phase densification:
placing natural graphite into a high-pressure carbonization furnace, introducing carbon source gas, raising the pressure and raising the temperature, raising the temperature to 500-700 ℃ at the temperature rise speed of 20 ℃/min under the pressure of 1-20 MPa, and keeping the temperature and the pressure for 1-4h to obtain gas-phase densified natural graphite;
(2) coating:
putting the gas-phase densified natural graphite obtained in the step (1) and asphalt into a high-efficiency mixer according to the mass ratio of 100 (2-10) for mixing for 20-80min, so that the asphalt is coated on the surface of the natural graphite to obtain coated natural graphite;
(3) carbonizing:
and (3) placing the coated natural graphite obtained in the step (2) in a nitrogen atmosphere protective furnace for sintering, raising the temperature to 1100-1500 ℃ at the heating rate of 2-25 ℃/min, preserving the heat for 3-10 hours, and removing magnetism and screening to obtain the low-expansion long-cycle graphite cathode material.
2. The preparation method of the low-expansion long-cycle graphite negative electrode material for the lithium ion battery according to claim 1, characterized in that: the natural graphite in the step (1) is spherical graphite, and D50=5-20 μm.
3. The preparation method of the low-expansion long-cycle graphite negative electrode material for the lithium ion battery according to claim 1, characterized in that: the carbon source gas in the step (1) is one or a mixture of more than one of methane, acetylene, ethane, propyne and propane.
4. The preparation method of the low-expansion long-cycle graphite negative electrode material for the lithium ion battery according to claim 1, characterized in that: the asphalt in the step (2) is one or a mixture of coal-series asphalt and oil-series asphalt, the softening point of the asphalt is 50-200 ℃, and the particle size of the asphalt D50=3-10 μm.
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