CN109950495A - Preparation method, negative electrode material and the lithium ion battery of high magnification graphite cathode material - Google Patents
Preparation method, negative electrode material and the lithium ion battery of high magnification graphite cathode material Download PDFInfo
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Abstract
The present embodiments relate to preparation method, negative electrode material and the lithium ion batteries of a kind of high magnification graphite cathode material, comprising: mixes the first carbon source material with powdery oxygen metal compound, obtains the first mixture；By the first mixture in 2000~3300 DEG C of progress graphitization processings, graphite material is obtained；Under room temperature or Elevated Temperature Conditions, graphite material is uniformly mixed with second carbon source material, obtains the second mixture；Second mixture is carbonized at 700~1300 DEG C, obtains negative electrode material after cooling, screening.With carbon material redox reaction occurs for the present invention at high temperature using oxygen metal compound, and the hole formed in carbon material surface, and it is effectively reduced using carbonization cladding and compares table, and then coat exposed graphite port, it can effectively improve the rate of charge of lithium ion battery, shorten the charging time, obtains high-energy density fast charge lithium ion battery.
Description
Technical field
The present invention relates to field of material technology more particularly to a kind of preparation methods of high magnification graphite cathode material, cathode
Material and lithium ion battery.
Background technique
With the continuous growth of global fuel vehicle quantity, automobile is more severe to environment and energy bring pressure.And it is new
Energy automobile is able to solve this problem, therefore is more taken seriously in the world, and many countries are even more to have formulated comprehensively
Prohibit the plan of first fuel vehicle.Under policy environment and the double requirements of Pressure on Energy, China Automobile Industry will undoubtedly welcome new energy
The development wave in source.However, new-energy automobile is there is also many short slabs, course continuation mileage is short, charging rate is slow etc., especially
Being that big multiplying power is easy to charge analyses lithium on negative electrode material surface, generates serious safety problem.The key of new-energy automobile development exists
In the breakthrough of battery technology, and the update of battery technology is the innovation of material.Artificial plumbago negative pole material has energy density
Height, the features such as having extended cycle life, its rate of charge of the artificial graphite of various specifications is not quite similar.
The rate of charge of lithium ion battery how is improved, shortens the charging time, obtains high-energy density fast charge lithium-ion electric
Pond is the problem to be solved in the present invention.
Summary of the invention
The purpose of the present invention is in view of the drawbacks of the prior art, provide a kind of preparation side of high magnification graphite cathode material
Using oxygen metal compound redox reaction occurs at high temperature with carbon material for method, negative electrode material and lithium ion battery, and
It is effectively reduced in the hole that carbon material surface is formed, and using carbonization cladding than table, and then coats exposed graphite port,
It can effectively improve the rate of charge of lithium ion battery, shorten the charging time, obtain high-energy density fast charge lithium ion battery.
In view of this, in a first aspect, the embodiment of the invention provides a kind of preparation method of high magnification graphite cathode material,
Include: to mix the first carbon source material by the weight ratio of 100:1~50 with powdery oxygen metal compound, it is mixed to obtain first
Close material；
By first mixture in 2000~3300 DEG C of progress graphitization processings, graphite material is obtained；
Under room temperature or Elevated Temperature Conditions, the graphite material is mixed with second carbon source material by the weight ratio of 100:0~10
It closes uniformly, obtains the second mixture；Wherein, the warming temperature is no more than 700 DEG C；
Second mixture is carbonized at 700~1300 DEG C, obtains negative electrode material after cooling, screening.
Preferably, the granular size of the first carbon source material is 5 μm~30 μm.
It is further preferred that first carbon source material include carbonaceous mesophase spherules, petroleum coke, pitch coke, needle coke or
One of coke is a variety of.
Preferably, the powdery oxygen metal compound includes ferroso-ferric oxide, di-iron trioxide, ferrous oxide, hydrogen-oxygen
Change iron, aluminium hydroxide, aluminum oxide, copper oxide, basic copper carbonate, zinc oxide, calcium oxide, manganese dioxide, manganese heptoxide,
Potassium permanganate is one or more.
Preferably, the second carbon source material includes asphalt powder and/or toner.
Preferably, the toner includes one of Kynoar, phenolic resin, polyethylene or a variety of.
Preferably, the Elevated Temperature Conditions are at the uniform velocity heating or the combination heating of multistage speed change, the heating rate are 1~10
℃/min。
Second aspect, the embodiment of the invention provides a kind of stones prepared using preparation method described in above-mentioned first aspect
Black negative electrode material.
The third aspect, the embodiment of the invention provides a kind of lithiums including graphite cathode material described in above-mentioned second aspect
Ion battery.
Preparation method, negative electrode material and the lithium-ion electric of a kind of high magnification graphite cathode material provided in an embodiment of the present invention
Using oxygen metal compound redox reaction occurs at high temperature with carbon material for pond, and in the hole that carbon material surface is formed
Hole, and be effectively reduced using carbonization cladding than table, and then coat exposed graphite port, it can effectively improve lithium-ion electric
The rate of charge in pond shortens the charging time, obtains high-energy density fast charge lithium ion battery.
Detailed description of the invention
Fig. 1 is a kind of preparation method flow chart of high magnification graphite cathode material provided in an embodiment of the present invention；
Fig. 2 is the embedding lithium schematic diagram of graphite particle charging after oxidation pore-creating provided in an embodiment of the present invention；
Fig. 3 is the embedding lithium schematic diagram of untreated graphite granule charging；
Fig. 4 is the scanning electron microscope (SEM) photograph for the negative electrode material that the embodiment of the present invention 1 provides；
Fig. 5 is the scanning electron microscope (SEM) photograph for the negative electrode material that the embodiment of the present invention 2 provides；
Fig. 6 is the scanning electron microscope (SEM) photograph for the negative electrode material that the embodiment of the present invention 3 provides；
Fig. 7 is the scanning electron microscope (SEM) photograph for the negative electrode material that the embodiment of the present invention 4 provides；
Fig. 8 is the scanning electron microscope (SEM) photograph for the negative electrode material that comparative example 1 of the present invention provides；
Fig. 9 is the scanning electron microscope (SEM) photograph for the negative electrode material that comparative example 2 of the present invention provides；
Figure 10 is the scanning electron microscope (SEM) photograph for the negative electrode material that comparative example 3 of the present invention provides；
Figure 11 is the scanning electron microscope (SEM) photograph for the negative electrode material that comparative example 4 of the present invention provides.
Specific embodiment
Below by drawings and examples, technical scheme of the present invention will be described in further detail.
Fig. 1 is a kind of preparation method, negative electrode material and the lithium of high magnification graphite cathode material provided in an embodiment of the present invention
Ion battery flow chart, as shown in Figure 1, which comprises
Step 101, the first carbon source material is mixed with powdery oxygen metal compound by the weight ratio of 100:1~50
It closes, obtains the first mixture.
Specifically, the granular size of the first carbon source material is 5 μm~30 μm, including carbonaceous mesophase spherules, petroleum coke, pitch
One of burnt, needle coke or coke are a variety of.
Powdery oxygen metal compound includes ferroso-ferric oxide, di-iron trioxide, ferrous oxide, iron hydroxide, hydroxide
Aluminium, aluminum oxide, copper oxide, basic copper carbonate, zinc oxide, calcium oxide, manganese dioxide, manganese heptoxide, potassium permanganate one
Kind is a variety of.
Step 102, the first mixture is obtained into graphite material in 2000~3300 DEG C of progress graphitization processings.
Graphitization when, oxygen metal compound at high temperature with the first carbon source material occur redox reaction, and
First carbon source material surface oxidation corrodes circular hole out, and the circular hole effect of formation is to open a plurality of lithium ion to enter
The channel of graphite, to increase the charge rate of material.
Step 103, under room temperature or Elevated Temperature Conditions, graphite material and second carbon source material are pressed to the weight of 100:0~10
Than being uniformly mixed, the second mixture is obtained.
The graphite particle of surface hole, exposed graphitic layers outside increase, in high temperature charge and discharge, graphite flake
The carbon atom of layer port is easy to collapse or side reaction occurs with electrolyte, to reduce battery performance.Therefore it needs with the second carbon
Source material coats the exposed carbon atom of these graphite flake layers, shields, to improve cycle performance and check electricity
Pond high temperature side reaction, while second carbon source material is carbonized the soft carbon to be formed, and is equivalent to the effect of funnel, and lithium ion is facilitated to enter
In circular hole and graphite flake layer.
Specifically, second carbon source material includes asphalt powder and/or toner, wherein toner includes gathering inclined fluorine
One of ethylene, phenolic resin, polyethylene are a variety of.
Here graphite material can be in room temperature or Elevated Temperature Conditions both of these case with being uniformly mixed for second carbon source material
Lower progress.
The first situation, at room temperature, the graphitized material and second carbon source material that step 102 is obtained are according to weight
Amount is than being uniformly mixed, to obtain the second mixture.
Second situation, under Elevated Temperature Conditions, warming temperature is no more than 700 DEG C, and can choose in temperature-rise period even
Speed heating or the combination heating of multistage speed change, heating rate are 1~10 DEG C/min, and graphitized material and second carbon source material side are heated up
Become mixing, the speed that control covering melts can be evenly coated under the conditions of corresponding, if heating is too fast, will cause
Covering has little time cladding and has just been carbonized.
It should be noted that being uniformly mixed here can be realized by modes such as stirrings, can will be sintered after graphitization
Or hardened graphite material is broken, is sufficiently mixed with covering.
Step 104, the second mixture is carbonized at 700~1300 DEG C, obtains negative electrode material after cooling, screening.
The preparation method of a kind of high magnification graphite cathode material provided in an embodiment of the present invention, using oxygen metal compound
Redox reaction, and the hole formed in carbon material surface occurs with carbon material at high temperature, and effective using carbonization cladding
It reduces than table, and then coats exposed graphite port, capacity is big, have extended cycle life, that rate of charge is high is negative to be made
Pole material.
Fig. 2 is the embedding lithium schematic diagram of graphite particle charging after oxidation pore-creating provided in an embodiment of the present invention, and Fig. 3 is untreated stone
The embedding lithium schematic diagram of black particle charging, in conjunction with Fig. 2 and Fig. 3 it is found that stone made from the preparation method provided through the embodiment of the present invention
Black negative electrode material, by redox reaction in graphite surface pore-creating, these micropores provide during the charging process for lithium ion embedding
Enter the channel of graphite flake layer, to improve Embedding efficiency.In addition, being effectively reduced using carbonization cladding than table, and then coat exposed
Graphite port outside, plays the role of funnel, rapidly flows toward lithium ion between micropore or graphite flake layer, to further increase
Rate of charge.
Graphite cathode material provided in this embodiment can be used as the negative electrode material of lithium ion battery or as its negative electrode material
A part.
In the following, by some specific embodiments, to the system of high magnification graphite cathode material provided in an embodiment of the present invention
Standby process and the application of high magnification graphite cathode material obtained, performance are described in more detail.
Embodiment 1
Step 1,20 μm of petroleum cokes are uniformly mixed with powdery iron hydroxide by the weight ratio of 100:40, obtains mixture I；
Step 2, mixture I is obtained into graphite material in 3250 DEG C of progress graphitization processings；
Step 3, obtained graphite material is uniformly mixed with asphalt powder by 100:6 at room temperature, obtains mixture II；
Step 4, mixture II is carbonized at 900 DEG C, obtains finished product after cooling screening.
Electronic Speculum detection is scanned to finished product, testing result is as shown in Figure 4.
It is made into half-cell using obtained negative electrode material to be tested, testing result is as shown in table 1 below.
Embodiment 2
Step 1,20 μm of petroleum cokes are uniformly mixed with powdery iron hydroxide by the weight ratio of 100:40, obtains mixture I；
Step 2, mixture I is obtained into graphite material in 3250 DEG C of progress graphitization processings；
Step 3, obtained graphite material is mixed in the case where covering is not added, obtains mixture II；Wherein, here
Mixing sintered graphite material can be crushed by modes such as stirrings, and be uniformly mixed, convenient for screening；
Step 4, finished product is obtained after mixture II being sieved.
Electronic Speculum detection is scanned to finished product, testing result is as shown in Figure 5.
It is made into half-cell using obtained negative electrode material to be tested, testing result is as shown in table 1 below.
Embodiment 3
Step 1,7 μm of rear needle coke of forging uniformly is mixed with powdery calcium oxide by the weight ratio of 100:10, is mixed
Material I；
Step 2, mixture I is obtained into graphite material in 2000 DEG C of progress graphitization processings；
Step 3, obtained graphite material is mixed into 30min by 100:6 with Kynoar at normal temperature, then presses 10
DEG C/min speed is warming up to 300 DEG C, then is warming up to 540 DEG C with 5 DEG C/min, 4h is kept the temperature, then cooled to room temperature, entire mistake
Journey is kept stirring 15 turns/min of speed, and heat preservation obtains mixture II；
Step 4, mixture II is carbonized at 1200 DEG C, obtains finished product after cooling screening.
Electronic Speculum detection is scanned to finished product, testing result is as shown in Figure 6.
It is made into half-cell using obtained negative electrode material to be tested, testing result is as shown in table 1 below.
Embodiment 4
Step 1,12 μm of life needle coke is uniformly mixed with powdery aluminum by the weight ratio of 100:5, obtains mixture
Ⅰ；
Step 2, mixture I is obtained into graphite material in 2600 DEG C of progress graphitization processings；
Step 3, obtained graphite material is uniformly mixed in the case where covering is not added, obtains mixture II；
Step 4, finished product is obtained after mixture II being sieved.
Electronic Speculum detection is scanned to finished product, testing result is as shown in Figure 7.
It is made into half-cell using obtained negative electrode material to be tested, testing result is as shown in table 1 below.
Comparative example 1
Comparative example 1 the difference from embodiment 1 is that not adding oxygen metal compound powdery iron hydroxide, join by other steps
Number is same as Example 1.
Electronic Speculum detection is scanned to finished product, testing result is as shown in Figure 8.
It is made into half-cell using obtained negative electrode material to be tested, testing result is as shown in table 1 below.
Comparative example 2
Comparative example 2 the difference from example 2 is that not plus oxygen metal compound powdery basic copper carbonate, other steps,
Parameter is same as Example 2.
Electronic Speculum detection is scanned to finished product, testing result is as shown in Figure 9.
It is made into half-cell using obtained negative electrode material to be tested, testing result is as shown in table 1 below.
Comparative example 3
The difference of comparative example 3 and embodiment 3 is not add oxygen metal compound powdery calcium oxide, other steps, parameter
It is same as Example 3.
Electronic Speculum detection is scanned to finished product, testing result is as shown in Figure 10.
It is made into half-cell using obtained negative electrode material to be tested, testing result is as shown in table 1 below.
Comparative example 4
The difference of comparative example 4 and embodiment 4 is not add oxygen metal compound powdery aluminum, other steps, parameter
It is same as Example 4.
Electronic Speculum detection is scanned to finished product, testing result is as shown in figure 11.
It is made into half-cell using obtained negative electrode material to be tested, testing result is as shown in table 1 below.
The negative electrode material of 1 embodiment 1-4 of table and comparative example 1-4 is made into half-cell the performance test results
As seen from Table 1, embodiment 1,2 is consistent with comparative example 1,2 raw materials, and treatment process is different, and comparison is real
Oxidation pore-creating meeting known to example 2 and comparative example 2 is applied so that the ratio table of finished product increases, cladding can known to comparative example 1 and embodiment 2
To be effectively reduced than table, this shows unanimously with SEM figure, it can be seen that the hole of embodiment 1 is wrapped by agent filling, therefore drops than table
It is low.
The 0.2C reversible capacity of embodiment 1 is more slightly lower than embodiment 2, leads this is because soft carbon cladding sacrifices a part of capacity
It causes, but under 10C multiplying power, DCIR is better than embodiment 2 under the embedding lithium capacity of embodiment 1 and 50%SOC, this is because soft carbon is in high power
Funnelling is played in rate process of intercalation, lithium ion is directed in hole or graphite flake layer, there is buffer function, thus high power
The embedding lithium capacity of rate charge condition packet carbon products is high.By embodiment 1,2 compared with comparative example 1,2, it is known that 0.2C multiplying power and 10C
Under the conditions of multiplying power, there are the embodiment 1 of oxidation pore-creating processing, 2 capacity higher, this mainly has benefited from hole and is in charge and discharge process
Lithium ion provides deintercalation channel, again as shown in Figure 1, therefore DCIR is smaller under the conditions of 50%SOC.
Embodiment 3,4 and comparative example 3,4 also keep identical rule, have the product high rate performance of oxidation pore-creating processing more preferable.
In addition, the introducing of oxidant increases the trace element anomaly of product, this mainly has benefited from being graphitized
Foreign atom gasifies to escape at high temperature and disappear in journey.In addition, each product is made into the full electrical testing of Soft Roll, anode matches NCM, as a result
Display oxidation pore-creating reduces the cycle life of product.
Above-described specific embodiment has carried out further the purpose of the present invention, technical scheme and beneficial effects
It is described in detail, it should be understood that being not intended to limit the present invention the foregoing is merely a specific embodiment of the invention
Protection scope, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should all include
Within protection scope of the present invention.
Claims (9)
1. a kind of preparation method of high magnification graphite cathode material, which is characterized in that the described method includes:
First carbon source material is mixed with powdery oxygen metal compound by the weight ratio of 100:1~50, it is mixed to obtain first
Close material；
By first mixture in 2000~3300 DEG C of progress graphitization processings, graphite material is obtained；
Under room temperature or Elevated Temperature Conditions, the graphite material is mixed with second carbon source material by the weight ratio of 100:0~10
It is even, obtain the second mixture；Wherein, the warming temperature is no more than 700 DEG C；
Second mixture is carbonized at 700~1300 DEG C, obtains negative electrode material after cooling, screening.
2. the preparation method of high magnification graphite cathode material according to claim 1, which is characterized in that the first carbon source material
Granular size be 5 μm~30 μm.
3. the preparation method of high magnification graphite cathode material according to claim 1 or 2, which is characterized in that described first
Carbon source material includes one of carbonaceous mesophase spherules, petroleum coke, pitch coke, needle coke or coke or a variety of.
4. the preparation method of high magnification graphite cathode material according to claim 1, which is characterized in that the powdery is oxygen-containing
Metallic compound includes ferroso-ferric oxide, di-iron trioxide, ferrous oxide, iron hydroxide, aluminium hydroxide, aluminum oxide, oxygen
It is one or more to change copper, basic copper carbonate, zinc oxide, calcium oxide, manganese dioxide, manganese heptoxide, potassium permanganate.
5. the preparation method of high magnification graphite cathode material according to claim 1, which is characterized in that the second carbon source
Material includes asphalt powder and/or toner.
6. the preparation method of high magnification graphite cathode material according to claim 1, which is characterized in that the toner
Including one of Kynoar, phenolic resin, polyethylene or a variety of.
7. the preparation method of high magnification graphite cathode material according to claim 1, which is characterized in that the Elevated Temperature Conditions
For at the uniform velocity heat up or multistage speed change combination heating, the heating rate be 1~10 DEG C/min.
8. a kind of graphite cathode material using any preparation method preparation of the claims 1-7.
9. a kind of lithium ion battery including graphite cathode material described in the claims 8.
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| CN112875696A (en) * | 2021-01-29 | 2021-06-01 | 广东凯金新能源科技股份有限公司 | Low-cost high-rate graphite-like negative electrode material based on carbon material tailings and preparation method thereof |
| CN112952070A (en) * | 2021-04-08 | 2021-06-11 | 黑龙江省宝泉岭农垦溢祥新能源材料有限公司 | Graphite lithium battery negative electrode material and preparation method thereof |
| CN114400324A (en) * | 2022-01-20 | 2022-04-26 | 深圳市金润能源材料有限公司 | Preparation method of negative electrode material, negative electrode material and lithium ion battery |
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Effective date of registration: 20220622 Address after: No. 456, Tianlai 1st Road, new energy and new material industry functional zone, Tianfu new area, Qionglai, Chengdu, Sichuan 610200 Patentee after: Sichuan Zichen Technology Co.,Ltd. Address before: 213300 Second Floor of Building A, 218 Hongkou Road, Kunlun Street, Liyang City, Changzhou City, Jiangsu Province (in Zhongguancun Science and Technology Industrial Park, Jiangsu Province) Patentee before: LIYANG ZICHEN NEW MATERIAL TECHNOLOGY Co.,Ltd. |
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