CN104538591B - Pre-lithiation method of lithium ion battery negative electrode material - Google Patents
Pre-lithiation method of lithium ion battery negative electrode material Download PDFInfo
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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
- H01M4/64—Carriers or collectors
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- 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
- H01M10/058—Construction or manufacture
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H—ELECTRICITY
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- H—ELECTRICITY
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Abstract
The invention discloses a pre-lithiation method of a lithium ion battery negative electrode material. The method is characterized in that by adopting a method of coating or covering the surface of metal lithium with a lithium ion barrier layer and/or controlling a resistance value of a connection conductor, the pre-lithiated current magnitude is limited, and the reaction speed of a primary battery between metal lithium and negative electrode materials is regulated so as to regulate the lithium-intercalation speed of the negative electrode material and formation speed of surface SEI films, and the circulation performance of the negative electrode material is improved based on the improvement on coulombic efficiency for the first time of the negative electrode material; moreover, the method is simple in process and easy to operate, and suitable for pre-lithiation of the commercial lithium ion battery negative electrode material; lithium consumed by irreversible reaction is supplemented, so that the coulombic efficiency for the first time and the capacity of the battery are increased, and the circulation performance of the battery is improved.
Description
Technical field
The present invention relates to the prelithiation method field of lithium ion battery material, particularly to a kind of lithium ion battery negative material
The prelithiation method of material.
Background technology
With the fast development of electronic product, high-energy, the demand of high power density lithium ion battery increase year by year, non-stone
Inkization material with carbon element, oxide material and composite etc. receive much concern because of high power or high power capacity.However, such material exists not
Reversible capacity is high, and the low serious problems of coulombic efficiency first are easily caused capacity of lithium ion battery and are decreased obviously.At present, in order to
Coulombic efficiency is low first to solve the problems, such as lithium ion battery negative material, people developed chemical reduction method, artificial sei embrane method and
Electrochemistry prelithiation method, wherein electrochemistry prelithiation method are that one kind the most directly solves the low storehouse first of lithium ion battery negative material
The method of human relations efficiency.
In the patent of cn200480021793.x, disclose one kind by lithium and electrode material directly contact, then by former
Cell reaction realizes the prelithiation method of electrode material.However, the method easily produces " dead lithium ", that is, the lithium adding can not be filled
Divide and utilize；And lithium and electrode material directly contact can cause lithiumation electric current excessive, cause electrode material structural deterioration and densification
And stable sei film difficult to form, ultimately result in the cycle performance decline of electrode material.
In the patent of cn200910188470.4, disclose one kind and by lithium deposition or snap non-dressing on a current collector
Area, the method recycling galvanic interaction to realize electrode material prelithiation, improve the utilization rate of lithium, solve " dead lithium " and ask
Topic.But, lithium is to be connected by the very little collector of resistance with electrode material, and lithiumation electric current will be very big, equally easily
The cycle performance causing electrode material declines.
In the patent of cn201210573270.2, for the big problem of lithiumation electric current, disclose a kind of low temperature fluid injection side
Method, makes galvanic interaction carry out at a lower temperature, controls the embedding lithium speed of material, thus improving material coulombic efficiency first
While with capacity, improve the cycle performance of material.However, the method needs low-temperature operation, technique is more complicated, high cost, and
And the electrolysis fluid viscosity under low temperature increases, fluid injection operating difficultiess.
Content of the invention
It is an object of the invention to provide a kind of process is simple, with low cost, prelithiation electric current can be efficiently controlled, carry
The coulombic efficiency first of high negative material, and significantly improve the lithium ion battery negative material prelithiation side of its cycle performance
Method.
For this reason, technical scheme is as follows:
A kind of prelithiation method of lithium ion battery negative material, comprises the steps:
(1) snapping the cladding of the metallic lithium surface on collector or superscribing lithium ion barrier layer, then be coated with bearing
The collector of pole slurry is connected on described collector or described lithium metal by the conductor of resistance value r≤0.1 ω；
Or snapping the cladding of the metallic lithium surface part on collector or superscribing lithium ion barrier layer, then it is coated with
The collector of cathode size 1 is by resistance value r > conductor of 0.1 ω is connected on described collector or described lithium metal；
Or snap lithium metal on a current collector, then it is coated with the collector of cathode size by resistance value r > 0.1 ω
Conductor is connected on described collector or described lithium metal；
Wherein, described barrier layer does not dissolve in and is formed with least one micropore on electrolyte and described barrier layer；
(2) negative electrode processing through described step () and anelectrode are assembled into lithium ion battery.
(3) by the lithium ion battery standing activation of assembling in described step (two), formed between lithium metal and negative material
Galvanic interaction, when reaction to lithium metal consumes completely, that is, completes the prelithiation of lithium ion battery negative material.
In step (), in metallic lithium surface cladding or to superscribe the effect of lithium ion barrier layer be limiting lithium ion
Diffusion velocity；The effect of conductor is to build electronics path between lithium metal and negative pole to form galvanic element, limits prelithiation
Size of current.Two methods are all conducive to adjusting the galvanic interaction speed between lithium metal and negative material, to be regulated and controled with this
The embedding lithium speed of negative material and surface sei film form speed, thus the basis in the coulombic efficiency first improving negative material
On, improve the cycle performance of negative material.
In step (), two kinds of prelithiation methods with conductor resistance value r=0.1 ω carry out description be because to lithium from
Sub- battery carries out in short circuit safety energy testing experiment, and the conductor being typically less than 0.1 ω with resistance is tested, and in electricity
During pond is actually used, conductor resistance should be greater than 0.1 ω.
The collector snapping lithium metal and be coated with cathode size collector can for identical metal or
Different metal.
In step (three), lithium ion battery stands activation process, forms galvanic element between lithium metal and negative material
React and consume completely process to lithium metal, this process can complete in the case of standing it is also possible to directly use in energising
Complete in journey.
Preferably, the micropore size of porosity≤80% of described barrier layer, or barrier layer is not more than 5mm.By to not
Quantity and micropore size with the micropore being formed on the barrier layer that material is made are controlled, can be to the diffusion speed of lithium ion
Degree is adjusted.
Preferably, the material of described barrier layer is plastic foil, hard paraffin, Copper Foil or the micropore being not involved in electrochemical reaction
Barrier film.Described barrier layer can also be able to be multilamellar for monolayer.
Preferably, described conductor by least one conductive metal or nonmetallic is made；It is highly preferred that leading described in making
The metal of body or nonmetallic be all not involved in the reaction of embedding lithium.
Described conductor and described lithium ion barrier layer, they pass through resistance respectively and hole passes to electronics in prelithiation circuit
Defeated and lithium ion transport limits, thus limiting prelithiation response speed.This is because in prelithiation reaction, electronics and lithium ion
Both participate in galvanic interaction, limit either or both, all can limit prelithiation response speed.
Additionally, can also relatively efficiently regulate and control the prelithiation depth of negative material by the adjustment of the consumption to lithium metal,
The i.e. degree of the raising of material initial coulomb efficiency.If the consumption of lithium metal exceedes the first week electrochemical reaction consumption of negative material
Lithium and battery standing soak time long enough, then the open-circuit voltage of battery eventually drops to 0v, and the lithium metal of excess is then
The lithium that during progressively discharging with replenishment cycles in follow-up cyclic process, irreversible reaction consumes, but negative material
The improvement of initial coulomb efficiency and cycle performance is unaffected, and the coulombic efficiency of its later cycles will reach or slightly super
Cross 100%.
The prelithiation method of this lithium ion battery negative material, by coating in metallic lithium surface or superscribing lithium ion resistance
Interlayer and/or the method carrying out resistance value control to connection conductor, limit the size of current of prelithiation, adjust lithium metal and negative pole
Galvanic interaction speed between material, and the embedding lithium speed to regulate and control negative material with this and surface sei film form speed, from
And on the basis of the coulombic efficiency first improving negative material, improve the cycle performance of negative material；And the present invention is adopted
Process is simple, easily operated, it is suitable for the prelithiation of commercial Li-ion battery negative material, supplement because of irreversible reaction
The lithium consuming, thus improving the coulombic efficiency first of battery, capacity, and improves its cycle performance.
Brief description
Fig. 1 is the structural representation of negative material prelithiation electrode in embodiments of the invention 1；
Fig. 2 is the structural representation of negative material prelithiation electrode in embodiments of the invention 2；
Fig. 3 is the structural representation of negative material prelithiation electrode in the comparative example 2 of the present invention；
Fig. 4 is the structural representation of negative material prelithiation electrode in the comparative example 3 of the present invention；
When Fig. 5 is the comparative example 1～3 of the present invention and the open-circuit voltage of battery prepared by embodiment 1～2 and standing activation
Between graph of a relation.
Specific embodiment
Below in conjunction with the accompanying drawings the prelithiation method of the lithium ion battery negative material of the present invention is described in detail, but this
Invention is not limited solely to following examples.
As shown in Fig. 1～2, the prelithiation method of this lithium ion battery negative material, comprise the steps:
(1) in lithium metal 3 Surface coating snapping on collector 21 or superscribe lithium ion barrier layer 5, then will coat
The collector 22 having cathode size 1 is connected to described collector 21 or described lithium metal 3 by the conductor 4 of resistance value r≤0.1 ω
On；
Or in the lithium metal 3 surface portion cladding snapping on collector 21 or superscribe lithium ion barrier layer 5, then will apply
The collector 22 being covered with cathode size 1 passes through resistance value r > conductor 4 of 0.1 ω is connected to described collector 21 or described lithium metal
On 3；
Or lithium metal 3 is snapped on collector 21, then it is coated with the collector 22 of cathode size 1 by resistance value r >
The conductor 4 of 0.1 ω is connected on described collector 21 or described lithium metal 3；
Wherein, described barrier layer 5 material does not dissolve in and is formed with least one micropore on electrolyte and described barrier layer 5；
(2) negative electrode processing through described step () and anelectrode are assembled into lithium ion battery.
(3) by the lithium ion battery standing activation of assembling in described step (two), formed between lithium metal and negative material
Galvanic interaction, when reaction to lithium metal consumes completely, that is, completes the prelithiation of lithium ion battery negative material.
Wherein, porosity≤80% of described barrier layer.Described barrier layer 5 material is the plastics being not involved in electrochemical reaction
Film, hard paraffin, Copper Foil or micro-pore septum.Described barrier layer 5 is single or multiple lift.Described conductor 4 can be conductive by least one
Metal or nonmetallic make.The metal making described conductor 4 is not involved in embedding lithium reaction.
All using having good chemical property silicon-Si oxide-in example 1 below～4 and comparative example 1～3
Carbon compound cathode materials (method with reference to disclosed patent cn201310683767.4 is prepared from), as active material, are made
2032 type button cells, to assess the improvement to lithium ion battery negative material chemical property for the prelithiation method.Wherein,
The cathode size 1 being coated on collector 22 by silicon-Si oxide-carbon compound cathode materials, conductive agent, pvdf with weight ratio is
8:1:1 forms, and metal lithium sheet is made to electrode, 1mol/l lipf6The solution of ec/dmc (volume ratio be 1:1) make electrolyte,
Cellgard2400 micro-pore septum makees barrier film, and collector 21 and collector 22 are Copper Foil.
Embodiment 1
As shown in figure 1, having snapped thickness in copper foil current collector 21 is 0.1mm lithium metal thin layer, then it is coated with negative pole
The cr that the copper foil current collector 22 of slurry 1 is 1 ω by resistance value20ni80Resistance wire is connected in described copper foil current collector 21, its
In, the weight of lithium metal thin layer is the 10% of silicon-Si oxide-carbon compound cathode materials weight, then by through above-mentioned process
Negative electrode and anelectrode are assembled into lithium ion battery, standing activation 24h.
Embodiment 2
As shown in Fig. 2 being 0.1mm lithium metal thin layer surface tight one snapping the thickness in copper foil current collector 21
Layer Copper Foil is as lithium ion barrier layer, and is punctured with the micropore that two apertures are 0.5mm on the Copper Foil as barrier layer, then will
The copper foil current collector 22 being coated with cathode size 1 is connected to described copper foil current collector 21 by the copper wire of resistance value r=0.005 ω
On, wherein, the weight of lithium metal thin layer is the 10% of silicon-Si oxide-carbon compound cathode materials weight, then will be through above-mentioned place
The negative electrode of reason and anelectrode are assembled into lithium ion battery, standing activation 24h.
Embodiment 3
It is that one layer of paraffin of 0.1mm lithium metal thin layer 3 surface tight is made snapping the thickness in copper foil current collector 21
For lithium ion barrier layer, and the micropore that 1 aperture is 0.2mm is punctured with the paraffin as barrier layer, then is coated with bearing
The copper foil current collector 22 of pole slurry 1 is connected in described copper foil current collector 21 by the copper wire of resistance value r=0.005 ω, wherein,
The weight of lithium metal thin layer is the 10% of silicon-Si oxide-carbon compound cathode materials weight, then by the negative electricity through above-mentioned process
Pole and anelectrode are assembled into lithium ion battery, standing activation 24h.
Embodiment 4
It is four layers of cellgard of tight on 0.1mm lithium metal thin layer snapping in the thickness in copper foil current collector 21
2400 micro-pore septums are as lithium ion barrier layer, then to be coated with the copper foil current collector 22 of cathode size 1 be 0.1 by resistance value
The resistance wire of ω is connected in described copper foil current collector 21, and wherein, the weight of lithium metal thin layer is that silicon-Si oxide-carbon is combined
Then negative electrode through above-mentioned process and anelectrode are assembled into lithium ion battery, standing activation by the 5% of negative material weight
24h.
Comparative example 1
The cathode size 1 being coated with silicon-Si oxide-carbon compound cathode materials preparation in copper foil current collector is as negative
Pole, is assembled into lithium ion battery, standing activation 24h with anelectrode.
Comparative example 2
As shown in figure 3, coating in copper foil current collector 22 by the negative pole of silicon-Si oxide-carbon compound cathode materials preparation
Slurry 1, and the lithium metal thin layer 3 that thickness is 0.1mm has been snapped on the part surface of affiliated negative material, lithium metal thin layer
Weight is the 10% of silicon-Si oxide-carbon compound cathode materials weight, then by the negative electrode through above-mentioned process and anelectrode group
Dress up lithium ion battery, standing activation 24h.
Comparative example 3
As shown in figure 4, uncoated silicon-Si oxide-carbon compound cathode materials are formed with copper foil current collector 22 obtaining not
Dressing area, and the lithium metal thin layer that thickness is 0.1mm has been snapped on non-dressing area, its weight is that silicon-Si oxide-carbon is combined
Then negative electrode through above-mentioned process and anelectrode are assembled into lithium ion battery, standing activation by the 10% of negative material weight
24h.
Performance test:
Coulombic efficiency test first:
The first charge-discharge coulombic efficiency of lithium ion battery can directly reflect the chemical property of this battery system, one
As cell negative electrode material the low performance that can affect its corresponding positive electrode capacity of efficiency.Therefore first charge-discharge coulombic efficiency for
Assessment battery performance plays a crucial role.
Coulombic efficiency test condition first to each embodiment and comparative example in this embodiment: room temperature condition
Under, battery is carried out under the electric current density of 100ma/g constant current charge-discharge, voltage range is 0.01～3.0v, record battery is first
Secondary coulombic efficiency.
Reversible capacity is tested:
To the cycle performance of battery, effective evaluation can be carried out to the reversible capacity test after circulating battery some cycles, its
Reversible capacity after circulation some cycles is less with the difference of reversible capacity first, and its reversible capacity conservation rate is higher, i.e. energy
Loss speed slower it was demonstrated that this battery usage cycles is longer.
After in this embodiment first all reversible capacities of each embodiment and comparative example being tested and are circulated for 100 weeks
Reversible capacity test condition: under room temperature condition, battery is carried out under the electric current density of 100ma/g constant current charge-discharge, voltage model
Enclose for 0.01～3.0v, and circulate 100 cycles, record battery first week reversible capacity and circulation in 100 weeks after reversible capacity, calculating
Capability retention after circulation in 100 weeks.
The electrochemical property test result of 2032 type button cells prepared by table 1. comparative example 1～3 and embodiment 1～4:
Comparative example 2 and comparative example 3 are the existing schemes that negative material is carried out with prelithiation, can see compared with comparative example 1
Go out, coulombic efficiency and cycle performance first can be effectively improved by negative material is carried out with prelithiation.And compared with comparative example 2
The prelithiation method to negative material that comparative example 3 is adopted has more preferable cycle performance.
Embodiment 1～4 be technical solution of the present invention disclosed in prelithiation is carried out to improve coulomb first to negative material
Efficiency and the specific embodiment of cycle performance.
Embodiment 1 is by snapping lithium metal on a current collector, then is coated with the collector of cathode size 1 and passes through resistance
Value r > method that the conductor of 0.1 ω is connected on described collector or described lithium metal completes to carry out prelithiation to negative material.
The method passes through the resistance value connecting conductor is defined reaching with the restriction to prelithiation electric current, that is, adjust lithium metal and bear
Galvanic interaction speed between the material of pole.Compared with comparative example 3, its first coulombic efficiency be still maintained at more than 100%, no
Loss；And after it circulates 100 weeks, reversible capacity only drops to 569.6mah/g by 623.7mah/g, its reversible capacity conservation rate
For 91.3%, with respect to comparative example 3, there is more excellent cycle performance.
Embodiment 2～4 be by snap the metallic lithium surface on collector cladding or superscribe lithium ion barrier layer,
The collector being coated with cathode size 1 again is connected to described collector or described metal by the conductor of resistance value r≤0.1 ω
Method on lithium completes to carry out prelithiation to negative material.The method is arrived by the dissolution rate that lithium ion barrier layer limits lithium
Reach the restriction to prelithiation electric current, that is, adjust the galvanic interaction speed between lithium metal and negative material.
Compared with comparative example 3, embodiment 2 adopt Copper Foil as lithium ion barrier layer, its first coulombic efficiency still keep
More than 100%, free of losses；And reversible capacity only drops to 601.6mah/g by 607.0mah/g after it circulates 100 weeks, its
Reversible capacity conservation rate is 99.1%, and that is, cycle performance of battery is obviously improved.
Compared with comparative example 3, embodiment 3 as lithium ion barrier layer and is punctured with two apertures thereon and is using paraffin
The micropore of 0.5mm, its first coulombic efficiency be 81.5, have certain electricity damage, after its circulation 100 weeks reversible capacity by
626.5mah/g drops to 557.4mah/g, and its reversible capacity conservation rate is 89.9%, and that is, cycle performance of battery has also been lifted.
Compared with comparative example 3, on embodiment 4 lithium metal thin layer, four layers of cellgard 2400 micro-pore septum of tight are made
For lithium ion barrier layer, its first coulombic efficiency be 98.0%, electric loss is less, after its circulation 100 weeks reversible capacity only by
620.8mah/g drops to 574.2mah/g, and its reversible capacity conservation rate is 92.5%, and that is, cycle performance of battery is effectively carried
Rise.
In conjunction with Fig. 5, i.e. comparative example 1～3 and the open-circuit voltage of battery prepared by embodiment 1～2 and standing soak time
Graph of a relation be analyzed it can be seen that realize the prelithiation of negative material using the embodiment of prelithiation method of the present invention, electricity
The open-circuit voltage in pond declines slow, is conducive to negative material surface to form the stable and sei film of densification such that it is able to significantly improve
Its cycle performance.
Negative active core-shell material, in addition to the novel silicon-Si oxide-carbon compound cathode materials adopting in an embodiment, also adopts
Soft carbon and ferrum oxide etc. are as negative material, and carry out the preprocess method in embodiment such as and carry out pre- place to negative material
Reason, has carried out electrochemical property test, it may have good result simultaneously, that is, has effectively improved coulombic efficiency and cycle performance first.
Claims (4)
1. a kind of prelithiation method of lithium ion battery negative material is it is characterised in that comprise the steps:
(1) in lithium metal (3) Surface coating snapping on collector (21) or parcel lithium ion barrier layer (5), then will coat
The collector (22) having cathode size (1) is connected to described collector (21) or institute by the conductor (4) of resistance value r≤0.1 ω
State on lithium metal (3)；
Snap lithium metal (3) surface portion on collector (21) cladding or superscribe lithium ion barrier layer (5), then will
Be coated with cathode size (1) collector (22) pass through resistance value r > 0.1 ω conductor (4) be connected to described collector (21) or
On described lithium metal (3)；Or lithium metal (3) is snapped on collector (21), then the collector being coated with cathode size (1)
(22) passing through resistance value r > conductor (4) of 0.1 ω is connected on described collector (21) or described lithium metal (3)；
Wherein, the material of described barrier layer (5) is not dissolved in that to be formed with least one on electrolyte and described barrier layer (5) micro-
Hole；Porosity≤80% of described barrier layer (5)；Described barrier layer (5) material is plastic foil, hard paraffin, Copper Foil or micropore
Barrier film；
(2) negative electrode processing through described step () and anelectrode are assembled into lithium ion battery；
(3) by the lithium ion battery standing activation of assembling in described step (two), between lithium metal and negative material, form former electricity
Pond is reacted, and when reaction to lithium metal consumes completely, that is, completes the prelithiation of lithium ion battery negative material.
2. the prelithiation method of lithium ion battery negative material according to claim 1 is it is characterised in that described barrier layer
(5) it is single or multiple lift.
3. the prelithiation method of lithium ion battery negative material according to claim 1 is it is characterised in that described conductor
(4) by least one conductive metal or nonmetallic make.
4. the prelithiation method of the lithium ion battery negative material according to claims 1 to 3 any one claim, it is special
Levy and be, make the metal of described conductor (4) or nonmetallic be all not involved in the reaction of embedding lithium.
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| CN109314270B (en) * | 2016-06-15 | 2022-02-01 | 罗伯特·博世有限公司 | Lithium ion battery and preparation method thereof |
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| CN115050927B (en) * | 2022-06-29 | 2023-09-08 | 齐鲁中科电工先进电磁驱动技术研究院 | Pre-lithiation method and pre-lithiation system |
| CN115360437B (en) * | 2022-08-23 | 2023-04-14 | 楚能新能源股份有限公司 | Prelithiation method, method for manufacturing lithium secondary battery, and lithium secondary battery |
| CN115632106B (en) * | 2022-10-17 | 2024-04-09 | 江苏正力新能电池技术有限公司 | Composite negative plate and secondary battery |
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| KR20130007320A (en) * | 2011-06-30 | 2013-01-18 | 삼성전기주식회사 | Lithium plate, method for lithium of electrode and energy storage device |
| CN103915262B (en) * | 2013-01-04 | 2017-08-11 | 深圳清华大学研究院 | The method of the pre- embedding lithium of lithium-ion capacitor negative pole |
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