CN107749454A - A kind of lithiation of lithium ion battery silicium cathode piece - Google Patents
A kind of lithiation of lithium ion battery silicium cathode piece Download PDFInfo
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- CN107749454A CN107749454A CN201611101961.7A CN201611101961A CN107749454A CN 107749454 A CN107749454 A CN 107749454A CN 201611101961 A CN201611101961 A CN 201611101961A CN 107749454 A CN107749454 A CN 107749454A
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- lithium
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- paper tinsel
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01M4/04—Processes of manufacture in general
- H01M4/043—Processes of manufacture in general involving compressing or compaction
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/44—Methods for charging or discharging
- H01M10/446—Initial charging measures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention relates to technical field of lithium ion, disclose a kind of lithiation of lithium ion battery silicium cathode piece, 1/3~2/3 on lithium paper tinsel thickness direction is partially submerged into by silicium cathode piece by roll-in, and lithium paper tinsel is discharged lithium by cell activation and infiltrate silicium cathode piece to realize the lithiumation of silicium cathode piece, 25~40 DEG C of roll temperature, the thickness of lithium paper tinsel is 3~25 um, and the quality of lithium paper tinsel is 1.0~1.2 times of the lifting target theoretical calculation dosage needed for efficiency first.Both ensured to be tightly fastened between lithium paper tinsel and silicium cathode piece in lithium paper tinsel thickness direction upper part insertion silicium cathode piece, while the side for avoiding lithium paper tinsel from reclining with silicium cathode piece can not be fully utilized by silicium cathode piece, cause the dendrite of lithium to occur, and cause lithium utilization rate low.Silicium cathode piece after lithiumation can be by improved efficiency 10~15% first of lithium ion battery, and the coulombic efficiency after circulating 50 times is 99.5~99.9%.
Description
Technical field
The present invention relates to technical field of lithium ion, and in particular to a kind of silicium cathode piece as negative electrode of lithium ion battery
Lithiation.
Background technology
Lithium ion battery is widely used in electric automobile, electronic work due to the features such as energy density is high, and service life is long
Tool and consumer electronics field, and high-energy-density demand promotes the negative material of lithium ion battery from carbon-based material to silicon-carbon at present
Composite direction is developed.Lithium ion battery lithium ion when charging occurs in first charge-discharge process is deviate from and entered by positive pole
Negative pole, deviate from by negative pole and enter " the rocking chair course of reaction " of positive pole during electric discharge, cause positive plate or negative plate surface formed it is solid
Body dielectric film(SEI), negative pole will not be returned again to by being formed in SEI lithium discharge process, lithium ion battery is had with initially filling
Electricity compares less capacity, causes lithium ion battery to produce 10~20% loss of specific capacity first (Initial Capacity
Loss, ICL), efficiency is low first for battery.Need to carry out lithiumation to the electrode material of lithium ion battery for this, i.e., in lithium-ion electric
Lithium is added in advance in the positive pole in pond, negative pole or barrier film, and the lithium of SEI consumption is formed with compensation.Chinese patent CN106129315A, specially
Sharp a kind of lithium ion battery composite separation membrane of title and preparation method thereof, lithium ion battery, it is date of publication on November 16th, 2016, public
A kind of lithium ion battery composite separation membrane for being coated in matrix surface and mending lithium layer has been opened, has mended in lithium layer and contains lithium powder, negative pole can be supplemented
Piece surface forms the lithium of SEI consumption, so as to reduce specific capacity loss first, improves the efficiency first of lithium ion battery.But make
Had the following disadvantages with lithium powder:Lithium powder disperses uneven to cause membrane properties uneven;Lithium powder easily produces more dust, exists
Potential safety hazard;Generally there is passivation layer in lithium powder surface, can leave hole after the dissolving of lithium powder in barrier film or pole piece or make surface
It is uneven, so as to reduce conduction and compacted density.
The content of the invention
For using lithium powder lithiumation in lithium ion battery material, the scattered inequality of lithium powder be present, produce dust and cause battery
The problems such as material conducting power declines, it is press-fitted it is an object of the invention to provide one kind in silicium cathode piece surface roll into lithium paper tinsel, so
Post activation lithium paper tinsel makes the lithiation of the lithium ion battery silicium cathode piece of silicium cathode piece lithiumation, and the present invention can make silicon from lithium paper tinsel
The uniform lithiumation in negative plate surface, and avoid the occurrence of dust, and roll-in mode operate it is succinct, safe efficient.
The present invention provides following technical scheme:
A kind of lithium ion battery lithiation of silicium cathode piece, comprises the following steps:
(1)Physics roll-in:The side of lithium paper tinsel is fitted in silicium cathode piece surface, then by roll squeezer roll-in, makes lithium paper tinsel thickness
Being partially submerged into silicium cathode piece for the 1/3~2/3 of direction forms compound silicon chip, and the pressure of roll squeezer is 500~1000MPa;
(2)Assembled battery:Compound silicon chip and positive plate, barrier film, electrolyte are put into shell and are assembled into interim Li-ion batteries piles;
(3)Cell activation:Interim Li-ion batteries piles are carried out with the precharge that electric charge is less than 0.2 C, then 35~45 DEG C of environment
It is middle to stand 20~30 hours so that silicium cathode piece is fully infiltrated by the lithium that lithium paper tinsel discharges.
The thickness direction of lithium paper tinsel is partially submerged into silicium cathode piece, has both ensured to be tightly fastened between lithium paper tinsel and silicium cathode piece, together
When avoid the excessive side for causing lithium paper tinsel to be reclined with silicium cathode piece of lithium paper tinsel insertion can not be completely by silicon during cell activation
Negative plate utilizes, and causes the dendrite of lithium to occur, causes lithium utilization rate low.The process of precharge is the activation process of lithium paper tinsel,
The lithium paper tinsel release lithium of lithium concentration official post covering silicium cathode piece in temporary batteries group be present, and diffuse into silicium cathode piece, Jin Erfen
The whole silicium cathode piece of cloth, reach overall pre- lithium effect, being stood for a period of time after precharge makes lithium paper tinsel release lithium completely and born by silicon
Pole piece makes full use of.
As a modification of the present invention, the thickness of the lithium paper tinsel is 3~25 um, the lithium paper tinsel covering part silicium cathode
The surface of piece, the quality of the lithium paper tinsel are 1.0~1.2 times of the lifting target theoretical calculation dosage needed for efficiency first.
Lithium paper tinsel is more thin, and lithium is distributed to the better but excessively thin lithium paper tinsel of even results of silicium cathode piece and added during cell activation
Work cost is high, while yielding, softening in nipping process, influences the effect of lithiumation.Therefore the certain thickness bar of lithium paper tinsel is being ensured
Lithium paper tinsel is covered to the part surface of silicium cathode piece, to realize making full use of for lithium paper tinsel under part.Lifting target is first needed for efficiency
Theoretical calculation dosage refers to the compensation rate of the lithium needed under the efficiency first that the needs in setting are lifted, and actual interpolation amount is with the benefit
1.0~1.2 times of the amount of repaying are suitable.
As a modification of the present invention, it is characterised in that the opposite side of the lithium paper tinsel is provided with polyolefin protection film layer, institute
Polyolefin diaphragm is stated to tear after roll-in obtains compound silicon chip.Polyolefin protection film layer protects lithium paper tinsel roll-in intact first, together
When avoid lithium paper tinsel from being bonded on roll squeezer.
As a modification of the present invention, roll temperature is 25~40 DEG C, and roll-in speed is 0.2~0.35 m/s.Big
Roll-in can cause lithium paper tinsel in nipping process to deviate from lithium at a temperature of the roll temperature scope, and make the part of silicium cathode piece by lithium
Change, the part that so during further cell activation silicium cathode piece can be caused to be lithiated lithium enrichment occurs, caused
The scattered inequality of lithium in silicium cathode piece, influence the lithiumation effect of silicium cathode piece.The m/s of control roll-in speed 0.2~0.35 can be protected effectively
Lithium paper tinsel uniform force is demonstrate,proved, can be partially submerged into thickness direction in silicium cathode piece.
As a modification of the present invention, roll-in is 25 ± 2 DEG C, entered in drying shed of the relative humidity less than 5% in temperature
OK.Dry environmental benefits are embedded in silicium cathode piece well in lithium paper tinsel, while avoid lithium paper tinsel surface from meeting water passivation.
As a modification of the present invention, pre-charge process is small electric charge ladder charging process, is followed successively by:0.01 C charges
30 minutes, 0.02 C charge 30 minutes, 0.05 C charge 30 minutes, 0.1 C charge 30 minutes, charge cutoff voltage 4.3V.
Realize that lithium diffusion process is stable by the electric discharge of small electric charge ladder to carry out, while avoided polarization phenomena caused by large charge.
As a modification of the present invention, using the both sides of the compound silicon chip of clamp, fixture during cell activation
Pressure is 290~300 N.Ensure that lithium paper tinsel is stably embedded in silicium cathode piece in activation process, and avoid lithium paper tinsel and silicium cathode piece swollen
It is swollen.
Beneficial effects of the present invention are as follows:
The lithiation of the lithium ion battery silicium cathode piece of the present invention, 1)By the way that the roll-in of lithium paper tinsel is embedded in silicium cathode piece, and
Lithium paper tinsel is discharged lithium and uniformly lithiumation silicium cathode piece by cell activation, effectively lift the efficiency first of lithium ion battery, drop
The low loss of specific capacity first, while operate more safe and reliable;2)Lithium paper tinsel covering part silicium cathode piece, and lithium paper tinsel thickness direction portion
Divide insertion to effectively improve the utilization ratio of lithium paper tinsel, avoid the occurrence of the dendrite of lithium;3)From roll-in in the range of 25~40 DEG C
It can effectively avoid occurring lithiumation in roll-in, ensure that silicium cathode piece lithiumation is uniform.
Brief description of the drawings
Fig. 1 is the structural representation of lithium paper tinsel covering part silicium cathode piece.
Fig. 2 is the profile that lithium paper tinsel thickness direction is partially submerged into silicium cathode piece.
In figure:1st, compound silicon chip, 2, silicium cathode piece, 3, lithium paper tinsel.
Embodiment
Just the embodiment of the present invention is described further below in conjunction with the accompanying drawings:
Unless otherwise specified, if not the present invention employed in device or raw material refers in particular to be commercially available or this area
Conventional, the method in following embodiments is the conventional method of this area.
The present invention nipping process temperature be 25 ± 2 DEG C, relative humidity less than 5% drying shed in carry out, roll squeezer
Operating pressure is 500~1000 MPa.One side of lithium paper tinsel is provided with polyolefin protection film layer.
Embodiment 1:
A kind of lithium ion battery lithiation of silicium cathode piece, comprises the following steps:
(1)Physics roll-in:As shown in figure 1, the side that lithium paper tinsel 3 is not set to polyolefin protection film layer is fitted in the surface of silicium cathode piece 2
And compound silicon chip 1, thickness preferably 3 um of lithium paper tinsel, lithium paper tinsel covering part silicium cathode piece are formed by roll squeezer roll-in.Such as Fig. 2 institutes
Show, in lithium paper tinsel thickness direction upper part insertion silicium cathode piece, preferably the 1/3 of lithium paper tinsel thickness direction is partially submerged into.To ensure roll-in
Stable to carry out avoiding that lithiumation phenomenon occurs in roll-in simultaneously, the operation temperature of roll squeezer is 25 DEG C, and roll-in speed is 0.2 m/s;
(2)Assembled battery:Compound silicon chip and positive plate, barrier film, electrolyte are put into shell and are assembled into interim Li-ion batteries piles,
The effect of the temporary batteries group is the occasion for providing activated li paper tinsel;
(3)Cell activation:It is electro-active less than 0.2 C preliminary filling that interim Li-ion batteries piles are carried out with electric charge, preferably by following suitable
The small electric charge ladder electricizing activation that sequence is carried out:0.01 C charge 30 minutes, 0.02 C charge 30 minutes, 0.05 C charge 30 points
Clock, 0.1 C charge 30 minutes, and charge cutoff voltage is 4.3 V, then stands 20 hours in 35 DEG C of environment, makes silicium cathode piece
Fully infiltrated by the lithium discharged in lithium paper tinsel.Stably it is embedded in for guarantee lithium paper tinsel in silicium cathode piece and avoids expanding, cell activation
During use the compound silicon chip of clamp both sides, chucking pressure is 290 N.
Through step(3)Silicium cathode piece after infiltration is the silicium cathode piece after lithiumation, silicium cathode piece surface color uniform one
Cause.
Embodiment 2:
A kind of lithium ion battery lithiation of silicium cathode piece, comprises the following steps:
(1)Physics roll-in:As shown in figure 1, the side that lithium paper tinsel 3 is not set to polyolefin protection film layer is fitted in the surface of silicium cathode piece 2
And compound silicon chip 1, thickness preferably 8 um of lithium paper tinsel, lithium paper tinsel covering part silicium cathode piece are formed by roll squeezer roll-in.Such as Fig. 2 institutes
Show, in lithium paper tinsel thickness direction upper part insertion silicium cathode piece, preferably the 1/2 of lithium paper tinsel thickness direction is partially submerged into.To ensure roll-in
Stable to carry out avoiding that lithiumation phenomenon occurs in roll-in simultaneously, the operation temperature of roll squeezer is 40 DEG C, and roll-in speed is 0.28 m/
s;
(2)Assembled battery:Compound silicon chip and positive plate, barrier film, electrolyte are put into shell and are assembled into interim Li-ion batteries piles,
The effect of the temporary batteries group is the occasion for providing activated li paper tinsel;
(3)Cell activation:It is electro-active less than 0.2 C preliminary filling that interim Li-ion batteries piles are carried out with electric charge, preferably by following suitable
The small electric charge ladder electricizing activation that sequence is carried out:0.01 C charge 30 minutes, 0.02 C charge 30 minutes, 0.05 C charge 30 points
Clock, 0.1 C charge 30 minutes, and charge cutoff voltage is 4.3 V, then stands 24 hours in 40 DEG C of environment, makes silicium cathode piece
Fully infiltrated by the lithium discharged in lithium paper tinsel.Stably it is embedded in for guarantee lithium paper tinsel in silicium cathode piece and avoids expanding, cell activation
During use the compound silicon chip of clamp both sides, chucking pressure is 295 N.
Through step(3)Silicium cathode piece after infiltration is the silicium cathode piece after lithiumation, silicium cathode piece surface color uniform one
Cause.
Embodiment 3:
A kind of lithium ion battery lithiation of silicium cathode piece, comprises the following steps:
(1)Physics roll-in:As shown in figure 1, the side that lithium paper tinsel 3 is not set to polyolefin protection film layer is fitted in the surface of silicium cathode piece 2
And compound silicon chip 1, thickness preferably 15 um of lithium paper tinsel, lithium paper tinsel covering part silicium cathode piece are formed by roll squeezer roll-in.Such as Fig. 2
Shown, in lithium paper tinsel thickness direction upper part insertion silicium cathode piece, preferably the 3/5 of lithium paper tinsel thickness direction is partially submerged into.To ensure roller
Pressure is stable to be carried out avoiding that lithiumation phenomenon occurs in roll-in simultaneously, and the operation temperature of roll squeezer is 35 DEG C, and roll-in speed is 0.3 m/
s;
(2)Assembled battery:Compound silicon chip and positive plate, barrier film, electrolyte are put into shell and are assembled into interim Li-ion batteries piles,
The effect of the temporary batteries group is the occasion for providing activated li paper tinsel;
(3)Cell activation:It is electro-active less than 0.2 C preliminary filling that interim Li-ion batteries piles are carried out with electric charge, it is preferred to use by such as
The small electric charge ladder electricizing activation that lower order is carried out:0.01 C charge 30 minutes, 0.02 C charge 30 minutes, 0.05 C charging 30
Minute, 0.1 C charge 30 minutes, charge cutoff voltage 4.3V, then stand 28 hours in 40 DEG C of environment, make silicium cathode
Piece is fully infiltrated by the lithium discharged in lithium paper tinsel.Stably it is embedded in for guarantee lithium paper tinsel in silicium cathode piece and avoids expanding, battery is lived
The both sides of the compound silicon chip of clamp are used during change, chucking pressure is 298 N.
Through step(3)Silicium cathode piece after infiltration is the silicium cathode piece after lithiumation, silicium cathode piece surface color uniform one
Cause.
Embodiment 4:
A kind of lithium ion battery lithiation of silicium cathode piece, comprises the following steps:
(1)Physics roll-in:As shown in figure 1, the side that lithium paper tinsel 3 is not set to polyolefin protection film layer is fitted in the surface of silicium cathode piece 2
And compound silicon chip 1, thickness preferably 25 um of lithium paper tinsel, lithium paper tinsel covering part silicium cathode piece are formed by roll squeezer roll-in.Such as Fig. 2
Shown, in lithium paper tinsel thickness direction upper part insertion silicium cathode piece, preferably the 2/3 of lithium paper tinsel thickness direction is partially submerged into.To ensure roller
Pressure is stable to be carried out avoiding that lithiumation phenomenon occurs in roll-in simultaneously, and the operation temperature of roll squeezer is 40 DEG C, and roll-in speed is 0.35
m/s;
(2)Assembled battery:Compound silicon chip and positive plate, barrier film, electrolyte are put into shell and are assembled into interim Li-ion batteries piles,
The effect of the temporary batteries group is the occasion for providing activated li paper tinsel;
(3)Cell activation:It is electro-active less than 0.2 C preliminary filling that interim Li-ion batteries piles are carried out with electric charge, preferably by following suitable
The small electric charge ladder electricizing activation that sequence is carried out:0.01 C charge 30 minutes, 0.02 C charge 30 minutes, 0.05 C charge 30 points
Clock, 0.1 C charge 30 minutes, and charge cutoff voltage is 4.3 V, then stands 30 hours in 45 DEG C of environment, makes silicium cathode piece
Fully infiltrated by the lithium discharged in lithium paper tinsel.Stably it is embedded in for guarantee lithium paper tinsel in silicium cathode piece and avoids expanding, cell activation
During use the compound silicon chip of clamp both sides, chucking pressure is 300 N.
Through step(3)Silicium cathode piece after infiltration is the silicium cathode piece after lithiumation, silicium cathode piece surface color uniform one
Cause.
The efficiency first of the lithium ion battery of negative pole is used as using the silicium cathode piece after the lithiation lithiumation of the present invention
10~15% can be lifted, and the coulombic efficiency after cycle charge-discharge 50 times is 99.5~99.9%.
Claims (7)
1. a kind of lithium ion battery lithiation of silicium cathode piece, comprises the following steps:
(1)Physics roll-in:The side of lithium paper tinsel is fitted in silicium cathode piece surface and then by roll squeezer roll-in, makes lithium paper tinsel thickness side
To 1/3~2/3 be partially submerged into silicium cathode piece and form compound silicon chip, the pressure of roll squeezer is 500~1000MPa;
(2)Assembled battery:Compound silicon chip and positive plate, barrier film, electrolyte are put into shell and are assembled into interim Li-ion batteries piles;
(3)Cell activation:Interim Li-ion batteries piles are carried out with the precharge that electric charge is less than 0.2 C, then 35~45 DEG C of environment
It is middle to stand 20~30 hours so that silicium cathode piece is fully infiltrated by the lithium that lithium paper tinsel discharges.
2. a kind of lithiation of lithium ion battery silicium cathode piece according to claim 1, the thickness of the lithium paper tinsel is 3
~25 um, the surface of the lithium paper tinsel covering part silicium cathode piece, the quality of the lithium paper tinsel is needed for lifting target first efficiency
1.0~1.2 times of theoretical calculation dosage.
A kind of 3. lithiation of lithium ion battery silicium cathode piece according to claim 1 or 2, it is characterised in that institute
The opposite side for stating lithium paper tinsel is provided with polyolefin protection film layer, and the polyolefin diaphragm is torn after roll-in obtains compound silicon chip.
A kind of 4. lithiation of lithium ion battery silicium cathode piece according to claim 1, it is characterised in that roll-in temperature
Spend for 25~40 DEG C, roll-in speed is 0.2~0.35 m/s.
A kind of 5. lithiation of lithium ion battery silicium cathode piece according to claim 1 or 4, it is characterised in that roller
Temperature is pressed in be carried out in 25 ± 2 DEG C, drying shed of the relative humidity less than 5%.
A kind of 6. lithiation of lithium ion battery silicium cathode piece according to claim 1, it is characterised in that precharge
For small electric charge ladder charging process, it is followed successively by:0.01 C charge 30 minutes, 0.02 C charge 30 minutes, 0.05 C charge 30 points
Clock, 0.1 C charge 30 minutes, charge cutoff voltage 4.3V.
A kind of 7. lithiation of lithium ion battery silicium cathode piece according to claim 1 or 6, it is characterised in that
The both sides of the compound silicon chip of clamp are used during cell activation, chucking pressure is 290~300 N.
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Cited By (5)
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CN109148827A (en) * | 2018-09-26 | 2019-01-04 | 西北工业大学 | A kind of prelithiation method of electrode of lithium cell |
CN111261836A (en) * | 2019-12-23 | 2020-06-09 | 中国科学院宁波材料技术与工程研究所 | Method for pre-lithiating negative electrode of lithium ion battery and preparation method of pre-lithiated lithium ion battery |
CN112701254A (en) * | 2020-12-29 | 2021-04-23 | 惠州亿纬锂能股份有限公司 | Lithium-sulfur soft package battery and preparation method thereof |
CN112952184A (en) * | 2019-12-11 | 2021-06-11 | 通用汽车环球科技运作有限责任公司 | Method of lithiating metal anodes using electrolytes |
CN113272995A (en) * | 2018-10-26 | 2021-08-17 | 株式会社Lg新能源 | Method for producing negative electrode for lithium secondary battery |
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CN112952184A (en) * | 2019-12-11 | 2021-06-11 | 通用汽车环球科技运作有限责任公司 | Method of lithiating metal anodes using electrolytes |
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CN112701254A (en) * | 2020-12-29 | 2021-04-23 | 惠州亿纬锂能股份有限公司 | Lithium-sulfur soft package battery and preparation method thereof |
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