CN109081326A - A kind of high power lithium ion cell negative electrode material and preparation method thereof - Google Patents
A kind of high power lithium ion cell negative electrode material and preparation method thereof Download PDFInfo
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- CN109081326A CN109081326A CN201810968176.4A CN201810968176A CN109081326A CN 109081326 A CN109081326 A CN 109081326A CN 201810968176 A CN201810968176 A CN 201810968176A CN 109081326 A CN109081326 A CN 109081326A
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The present invention relates to a kind of high power lithium ion cell negative electrode materials and preparation method thereof, and the preparation method comprises the following steps: (1) noncrystalline carbon precursor is crushed, after be dried, obtain precursor powder；(2) precursor powder obtained by step (1) is further crushed, obtains refinement precursor powder；(3) refinement precursor powder obtained by step (2) is obtained into modified precursor powder after high-temperature calcination；(4) modified precursor powder obtained by step (3) is obtained into high power lithium ion cell negative electrode material again through graphitization processing.The preparation method is to carrying out drying and processing after noncrystalline carbon precursor coarse crushing, it can reduce moisture therein, promote the stability in refinement crushing process, so that raw material crushes yield and improves, cost is reduced, and thinning process further reduced particle size simultaneously, the power-performance of material can be increased substantially, in addition, preparation method of the invention is simple, the prospect with industrialized production.
Description
Technical field
The present invention relates to battery material fields, and in particular to a kind of high power lithium ion cell negative electrode material and its preparation side
Method.
Background technique
The cathode of lithium ion battery is by carbon element or non-carbon material, adhesive and additive mixing system
Copper foil two sides are uniformly applied at paste adhesive, through drying, are rolled.Negative electrode material is the master of lithium ion battery storage lithium
Body is embedded in lithium ion in charge and discharge process and abjection.When lithium battery charges, lithium atom is ionized into lithium ion and electricity in anode
Son, and lithium ion moves and electronic synthesis lithium atom to cathode.When electric discharge, lithium atom negative terminal surface out of graphite crystal is ionized
At lithium ion and electronics, and lithium atom is synthesized at anode.Negative electrode material mainly influences the first charge discharge efficiency of lithium battery, cycle performance
The performance of lithium battery is also directly affected Deng, the performance of negative electrode material, therefore studies the emphasis that ion cathode material lithium has become field
Direction.
Summary of the invention
It is of the existing technology in order to solve the problems, such as, the present invention provides a kind of high power lithium ion cell negative electrode material and
Preparation method.The preparation method can be improved amorphous by coarse crushing, drying, refinement, high-temperature calcination and graphitization processing
The stability and crushing yield of matter carbon precursor.The electrochemical performance of the high power lithium ion cell negative electrode material, warp
Verifying rate of charge reaches as high as 15C.
The solution of the present invention is to provide a kind of preparation method of high power lithium ion cell negative electrode material, including walk as follows
It is rapid:
(1) noncrystalline carbon precursor is crushed, after be dried, obtain precursor powder；
(2) precursor powder obtained by step (1) is further crushed, obtains refinement precursor powder；
(3) refinement precursor powder obtained by step (2) will be obtained modified precursor powder after high-temperature calcination；
(4) modified precursor powder obtained by step (3) is obtained into high power lithium ion cell cathode material again through graphitization processing
Material.
Preferably, in step (1), the noncrystalline carbon precursor is pitch coke or petroleum coke.
Preferably, in step (1), the drying temperature is 150~350 DEG C, and drying time is 0.5~4h, is dried when dry
Dry machine revolving speed is 2~20r/min.
Preferably, in step (1), granularity≤2mm of the precursor powder.
Preferably, in step (2), grating disk is used further to crush for the roll squeezer of roller pearl structure to precursor powder.
Because the squeeze roller group that roll squeezer is rotated synchronously in opposite directions by two is at being squeezed pressure roller continuous band when material is fed above two rollers
Between entering roller, after the high pressure effect of 100~150MPa, become to be discharged under closely knit material cake slave.Material particles through crushing
Particle obtained from its granularity is crushed compared with standard machinery with distribution is smaller narrower.
Preferably, in step (2), the refinement precursor powder granularity D50 value is 4~7 μm.
Preferably, in step (3), the heating mode of the high-temperature calcination are as follows: since room temperature, with 1.0~6.0 DEG C/min
Rate be warming up to 500~600 DEG C.
Preferably, in step (3), the high-temperature calcination is in 500~600 DEG C of 60~180min of maintenance.
Preferably, in step (4), the graphitization processing mode are as follows: by modified precursor powder at 2800~3000 DEG C
At a temperature of fire 1~2h.
As a general technical idea, the present invention also provides a kind of high-power lithium being prepared by the above method from
Sub- cell negative electrode material.
The invention has the benefit that
The preparation method of high power lithium ion cell negative electrode material of the present invention, to noncrystalline carbon precursor coarse crushing
After carry out drying and processing, can reduce moisture therein, promote the stability in refinement crushing process, so that raw material crushes yield
It improves, cost reduces, and thinning process further reduced particle size simultaneously, can increase substantially the power of material
Can, high-temperature calcination modification and graphitization processing successively are carried out to refinement precursor powder later, finally obtained lithium ion battery is negative
The battery first discharge specific capacity of pole material can accomplish that 160C discharges in 330mAh/g or more；In addition, preparation of the invention
Method is simple, the prospect with industrialized production.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, technical solution of the present invention will be carried out below
Detailed description.Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Base
Embodiment in the present invention, those of ordinary skill in the art are obtained all without making creative work
Other embodiment belongs to the range that the present invention is protected.
Embodiment 1
The present embodiment provides a kind of preparation methods of high power lithium ion cell negative electrode material, include the following steps:
(1) pitch coke is crushed, after in dryer with 1.5h dry under conditions of the revolving speed of 2r/min, 200 DEG C,
Obtain granularity≤2mm precursor powder；
(2) it uses grating disk further to crush for the roll squeezer of roller pearl structure to precursor powder obtained by step (1), obtains grain
Spend the refinement precursor powder that D50 value is 6~7 μm；
(3) refinement precursor powder obtained by step (2) is warming up to 600 DEG C since room temperature with the rate of 1.0 DEG C/min
It is calcined, constant temperature keeps 60min, obtains modified precursor powder；
(4) modified precursor powder obtained by step (3) is fired under the conditions of 2800 DEG C processing 2h, obtains high-power lithium ion
Cell negative electrode material.
Embodiment 2
The present embodiment provides a kind of preparation methods of high power lithium ion cell negative electrode material, include the following steps:
(1) petroleum coke is crushed, after in dryer with dry under conditions of the revolving speed of 20r/min, 200 DEG C
1.5h obtains granularity≤2mm precursor powder；
(2) it uses grating disk further to crush for the roll squeezer of roller pearl structure to precursor powder obtained by step (1), obtains grain
Spend the refinement precursor powder that D50 value is 4~5 μm；
(3) refinement precursor powder obtained by step (2) is warming up to 600 DEG C since room temperature with the rate of 6.0 DEG C/min
It is calcined, constant temperature keeps 180min, obtains modified precursor powder；
(4) modified precursor powder obtained by step (3) is fired under the conditions of 3000 DEG C processing 1h, obtains high-power lithium ion
Cell negative electrode material.
Embodiment 3
The present embodiment provides a kind of preparation methods of high power lithium ion cell negative electrode material, include the following steps:
(1) petroleum coke is crushed, after in dryer with dry under conditions of the revolving speed of 10r/min, 200 DEG C
1.5h obtains granularity≤2mm precursor powder；
(2) it uses grating disk further to crush for the roll squeezer of roller pearl structure to precursor powder obtained by step (1), obtains grain
Spend the refinement precursor powder that D50 value is 6~7 μm；
(3) refinement precursor powder obtained by step (2) is warming up to 600 DEG C since room temperature with the rate of 3.0 DEG C/min
It is calcined, constant temperature keeps 120min, obtains modified precursor powder；
(4) modified precursor powder obtained by step (3) is fired under the conditions of 2800 DEG C processing 2h, obtains high-power lithium ion
Cell negative electrode material.
Embodiment 4
The present embodiment provides a kind of preparation methods of high power lithium ion cell negative electrode material, include the following steps:
(1) petroleum coke is crushed, after in dryer with dry under conditions of the revolving speed of 15r/min, 350 DEG C
0.5h obtains granularity≤2mm precursor powder；
(2) it uses grating disk further to crush for the roll squeezer of roller pearl structure to precursor powder obtained by step (1), obtains grain
Spend the refinement precursor powder that D50 value is 6~7 μm；
(3) refinement precursor powder obtained by step (2) is warming up to 500 DEG C since room temperature with the rate of 3.0 DEG C/min
It is calcined, constant temperature keeps 90min, obtains modified precursor powder；
(4) modified precursor powder obtained by step (3) is fired under the conditions of 2800 DEG C processing 2h, obtains high-power lithium ion
Cell negative electrode material.
Embodiment 5
The present embodiment provides a kind of preparation methods of high power lithium ion cell negative electrode material, include the following steps:
(1) petroleum coke is crushed, after in dryer with 4h dry under conditions of the revolving speed of 5r/min, 150 DEG C, obtain
Granularity≤2mm precursor powder；
(2) it uses grating disk further to crush for the roll squeezer of roller pearl structure to precursor powder obtained by step (1), obtains grain
Spend the refinement precursor powder that D50 value is 5~6 μm；
(3) refinement precursor powder obtained by step (2) is warming up to 600 DEG C since room temperature with the rate of 3.0 DEG C/min
It is calcined, constant temperature keeps 120min, obtains modified precursor powder；
(4) modified precursor powder obtained by step (3) is fired under the conditions of 2800 DEG C processing 2h, obtains high-power lithium ion
Cell negative electrode material.
Comparative example 1
This comparative example provides a kind of preparation method of high power lithium ion cell negative electrode material, includes the following steps:
(1) petroleum coke is crushed, obtains granularity≤2mm precursor powder；
(2) precursor powder obtained by step (1) is further crushed using standard machinery pulverizer, obtaining granularity D50 value is 8
~9 μm of refinement precursor powder；
(3) refinement precursor powder obtained by step (2) is warming up to 600 DEG C since room temperature with the rate of 1.0 DEG C/min
It is calcined, constant temperature keeps 60min, obtains modified precursor powder；
(4) modified precursor powder obtained by step (3) is fired under the conditions of 2800 DEG C processing 2h, obtains high-power lithium ion
Cell negative electrode material.
Comparative example 1 and the difference of embodiment are: in step (1), not drying after noncrystalline carbon precursor crushes；Step
(2) in, roll squeezer is replaced with into standard machinery pulverizer, precursor powder is further crushed.
Comparative example 2
This comparative example provides a kind of preparation method of high power lithium ion cell negative electrode material, includes the following steps:
(1) petroleum coke is crushed, obtains granularity≤2mm precursor powder；
(2) precursor powder obtained by step (1) is further crushed using standard machinery pulverizer, obtaining granularity D50 value is 9
~10 μm of refinement precursor powder；
(3) refinement precursor powder obtained by step (2) is fired under the conditions of 2800 DEG C processing 2h, obtains high-power lithium ion
Cell negative electrode material.
Comparative example 2 and the difference of embodiment are: in step (1), not drying after noncrystalline carbon precursor crushes；Step
(2) in, roll squeezer is replaced with into standard machinery pulverizer, precursor powder is further crushed；Not to refinement precursor
End is modified processing.
The electrochemistry of high power lithium ion cell negative electrode material is studied in experiment using the button cell of model CR2032
Performance.
Experimental method: cathode is using NMP as solvent, and the formula of pole piece presses active material: PVDF:SP=92:8:2 is prepared
It is coated on copper foil at 45% slurry, 1.3g/cc is arrived in cold pressing；The LiPF6 solution that electrolyte in button cell is 1mol/L, it is molten
Agent uses volume ratio for the mixed solvent of EC, DEC and EMC of 1 ︰, 1 ︰ 1；Button cell is produced in the glove box of argon gas protection will
Lithium piece, isolation film, cathode pole piece, electrolyte and battery case are combined into button cell；Electro-chemical test using 0.1C/0.05C into
Row charge and discharge, charge and discharge blanking voltage are 0.005V/2.0V.
Embodiment and comparative example main distinction point are as shown in table 1, and confirmatory experiment test result is as shown in table 2.
1 embodiment of table and the comparative example technique main distinction
2 confirmatory experiment test result of table
Verification result:
1, it when being crushed using roll squeezer to noncrystalline carbon precursor, crushes yield and is apparently higher than mechanical crusher powder
Crushing yield when broken raw material shows that compared to mechanical crusher, roll squeezer by raw material granularity and can divide when grinding raw material
Cloth crush more it is small more evenly.
2, when grinding particle size D50 is smaller, rate of charge is then higher, and battery performance is better.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain
Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (10)
1. a kind of preparation method of high power lithium ion cell negative electrode material, which comprises the steps of:
(1) noncrystalline carbon precursor is crushed, after be dried, obtain precursor powder；
(2) precursor powder obtained by step (1) is further crushed, obtains refinement precursor powder；
(3) refinement precursor powder obtained by step (2) is obtained into modified precursor powder after high-temperature calcination；
(4) modified precursor powder obtained by step (3) is obtained into high power lithium ion cell negative electrode material again through graphitization processing.
2. the preparation method of high power lithium ion cell negative electrode material according to claim 1, which is characterized in that step
(1) in, the noncrystalline carbon precursor is pitch coke or petroleum coke.
3. the preparation method of high power lithium ion cell negative electrode material according to claim 1, which is characterized in that step
(1) in, the drying temperature is 150~350 DEG C, and drying time is 0.5~4h, and dryer revolving speed is 2~20r/ when dry
min。
4. the preparation method of high power lithium ion cell negative electrode material according to claim 1, which is characterized in that step
(1) in, granularity≤2mm of the precursor powder.
5. the preparation method of high power lithium ion cell negative electrode material according to claim 1, which is characterized in that step
(2) in, grating disk is used further to crush for the roll squeezer of roller pearl structure to precursor powder.
6. the preparation method of high power lithium ion cell negative electrode material according to claim 1, which is characterized in that step
(2) in, the refinement precursor powder granularity D50 value is 4~7 μm.
7. the preparation method of high power lithium ion cell negative electrode material according to claim 1, which is characterized in that step
(3) in, the heating mode of the high-temperature calcination are as follows: since room temperature, 500 are warming up to the rate of 1.0~6.0 DEG C/min~
600℃。
8. the preparation method of high power lithium ion cell negative electrode material according to claim 1, which is characterized in that step
(3) in, the high-temperature calcination is in 500~600 DEG C of 60~180min of maintenance.
9. the preparation method of high power lithium ion cell negative electrode material according to claim 1, which is characterized in that step
(4) in, the graphitization processing mode are as follows: modified precursor powder is fired into 1~2h at a temperature of 2800~3000 DEG C.
10. the high power lithium ion cell negative electrode material that any one of claim 1~9 the method is prepared.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113594450A (en) * | 2021-07-15 | 2021-11-02 | 山西沁新能源集团股份有限公司 | Preparation method of coal-based artificial graphite cathode material for lithium ion battery |
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| KR101138021B1 (en) * | 2010-11-29 | 2012-04-20 | 전자부품연구원 | Anode material for lithium ion capacitor and manufacturing method thereof |
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Application publication date: 20181225 |