CN110061299A - A kind of method of lithium ion cell electrode pre- embedding lithium in situ - Google Patents
A kind of method of lithium ion cell electrode pre- embedding lithium in situ Download PDFInfo
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- CN110061299A CN110061299A CN201910379409.1A CN201910379409A CN110061299A CN 110061299 A CN110061299 A CN 110061299A CN 201910379409 A CN201910379409 A CN 201910379409A CN 110061299 A CN110061299 A CN 110061299A
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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
- H01M10/05—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
- 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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- 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
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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Abstract
The present invention relates to a kind of methods of lithium ion cell electrode pre- embedding lithium in situ, include: S1, on the top of metal electrode, connection lithium metal forms reference electrode, and reference electrode is immersed in battery electrolyte by the aperture insertion of lid surface, is not contacted with battery core；S2, using battery cathode as cathode, reference electrode is anode, using low current charge, carries out the pre- embedding lithium of cathode；S3, the variation of real-time monitoring cathode potential；When terminating current potential lower than first, stop the pre- embedding lithium of cathode；S4, using anode as cathode, reference electrode is anode, using low current charge, carries out the pre- embedding lithium of anode；S5, the variation of real-time monitoring anodic potentials；When terminating current potential lower than second, stop the pre- embedding lithium of anode.The present invention carries out pre- embedding lithium in situ after battery completes ageing, and individually controls the pre- embedding lithium of positive and negative electrode, while real-time monitoring positive and negative electrode current potential, is reasonably controlled lithium-inserting amount, and quickly judge neutralization electrode when positive and negative electrode occurs abnormal.
Description
Technical field
The present invention relates to a kind of methods of lithium ion cell electrode pre- embedding lithium in situ, belong to technical field of lithium ion.
Background technique
With the development of modern industrial society, the consumption of fossil fuel increased dramatically, and wherein communications and transportation is to fuel oil
Consumption it is especially prominent.Lithium ion battery is as a kind of novel electric energy storage carrier, specific energy height, safety high with its voltage
Property it is good and pollution-free the advantages that paid close attention to by people.
The initial coulomb efficiency of high-capacity square lithium ion battery is an important indicator of evaluation single battery performance, and
Its interface performance and cycle life are closely related.When lithium ion battery carries out preliminary filling, active lithium-ion therein is from just
The abjection of pole, lithium ion first can form SEI (solid electrolyte interface, Solid in graphite surface when being embedded in graphite
Electrolyte Interface) film, participate in film forming lithium ion can not return to anode in after discharge.In addition, positive and negative
Material structure during embedding de- lithium in pole can change, reduce in material can embedding de- lithium position, part lithium ion
It can not freely be embedded in and deviate from and form " dead lithium ", lead to irreversible capacitance loss, it is relatively low to further result in coulombic efficiency.
The pre- embedding lithium technique of traditional battery is that pre- embedding lithium is individually carried out to positive and negative electrode before battery assembly.It is pre- for cathode
Embedding lithium technique, cathode is connect with lithium piece and is charged, is melted into advance, or passivation of lithium powder is added in cathode, also or negative
Lithium source is introduced before pole graphite and copper foil.And the pre- embedding lithium technique of anode is usually the rich lithium material of addition in anode, such as
Li5FeO4, lithium ion can be discharged in preliminary filling, but the reaction occurred is irreversible, and the LiFeO generated2To be retained in lithium from
In sub- battery, the energy density of lithium ion battery will certainly be reduced.It should be noted that these methods are to positive and negative plate
Pre- embedding lithium is carried out, is assembled again later, high to environmental requirement, technique is also extremely complex.
In view of this, the method that the present invention proposes a kind of lithium ion cell electrode pre- embedding lithium in situ, in battery according to normal stream
Pre- embedding lithium, while the positive and negative electrode potential of real-time monitoring are carried out after journey assembly, fluid injection, ageing to it, prevents too little or too much embedding lithium,
Lithium-inserting amount is reasonably controlled, and quickly judges neutralization electrode when positive and negative electrode occurs abnormal, to effectively solve existing
There are disadvantage present in technology and limitation.
Summary of the invention
The object of the present invention is to provide a kind of methods of lithium ion cell electrode pre- embedding lithium in situ, after battery completes ageing
Pre- embedding lithium in situ is carried out, and individually controls the pre- embedding lithium of positive and negative electrode, while real-time monitoring positive and negative electrode current potential, lithium-inserting amount is closed
The control of reason, and neutralization electrode is quickly judged when positive and negative electrode occurs abnormal.
To achieve the above object, the present invention provides a kind of method of lithium ion cell electrode pre- embedding lithium in situ, comprising following
Step:
S1, under low humidity conditions, on the top of metal electrode, connection lithium metal forms reference electrode, by the reference electrode
Across the aperture of the lid surface of lithium ion battery, lithium metal is made to be inserted into and be immersed in the electrolyte of inside lithium ion cell,
And it is not contacted with battery core；
S2, using the cathode of lithium ion battery as cathode, reference electrode is anode, right using low current charge certain time
The cathode of lithium ion battery carries out pre- embedding lithium；
S3, during the pre- embedding lithium of the cathode to lithium ion battery, using voltage measuring apparatus real-time monitoring lithium ion
The cathode potential of battery changes；When the cathode potential of lithium ion battery terminates current potential lower than first, stop the pre- embedding lithium of cathode, it is real
The independent control of embedding lithium now pre- to cathode；
S4, with lithium ion battery just extremely cathode, reference electrode are anode, it is right using low current charge certain time
The anode of lithium ion battery carries out pre- embedding lithium；
S5, during the positive pre- embedding lithium to lithium ion battery, using voltage measuring apparatus real-time monitoring lithium ion
The anodic potentials of battery change；When the anodic potentials of lithium ion battery terminate current potential lower than second, stop the pre- embedding lithium of anode, it is real
Now to the independent control of the pre- embedding lithium of anode.
In the S1, metal electrode is using platinum electrode or copper electrode or silver electrode or nickel electrode.
In the S1, the shape of metal electrode is cylinder, and diameter is less than the opening diameter of lid surface.
In the S1, lithium metal pressed by physics it is attached, or plating, or package adhesive tape mode be fixedly connected on metal electricity
The top outer surface of pole.
In the S2 and S4, using constant current charge-discharge instrument carry out low current charge, and the electric current used be 10mA~
100mA。
In the S3, first terminates current potential as 0.1V~0.25V.
In the S5, second terminates current potential as 2.0V~3.0V.
In the S3 and S5, during the positive or negative pole to lithium ion battery carries out pre- embedding lithium, reference electrode
It can extract out at any time, lithium metal is being replenished in time and then is being inserted into the inside of lithium ion battery.
The present invention carries out pre- embedding lithium in situ after lithium ion battery assembly, fluid injection, aging step, without in positive and negative electrode
It is assembled again after pre- embedding lithium.
In conclusion the method for lithium ion cell electrode provided by the present invention pre- embedding lithium in situ, it can be to the anode of battery
Or cathode individually controls and carries out pre- embedding lithium, reduces the consumption of lithium ion battery active lithium in preliminary filling, improves electrode interface characteristic,
Improve initial coulomb efficiency；Positive and negative electrode current potential can be monitored in the pre- embedding lithium of battery, stopped when reaching preset termination current potential pre-
Embedding lithium, prevents too little or too much embedding lithium, is reasonably controlled lithium-inserting amount；And quickly judge to lose in appearance potential exception
Imitate electrode；Pre- embedding lithium in situ can be carried out after lithium ion battery assembly, fluid injection, aging step；It is simple and reliable, it is time-consuming short, at
This is low, is effectively improved electrode interface.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the reference electrode in the present invention；
Fig. 2 is the structural schematic diagram of the cover board of the lithium ion battery in the present invention；
Fig. 3 is the schematic diagram that the current potential in the pre- process of intercalation of cathode of the lithium ion battery in the present invention changes over time；
Fig. 4 is the flow chart of the lithium ion cell electrode method of pre- embedding lithium in situ in the present invention.
Specific embodiment
Below in conjunction with FIG. 1 to FIG. 4, by preferred embodiment to technology contents of the invention, construction feature, reached purpose
And effect is described in detail.It should be understood that these embodiments are merely to illustrate the present invention rather than limit protection of the invention
Range.In the following examples, the experimental methods for specific conditions are not specified, usually according to normal condition, or is built according to manufacturer
The condition of view carries out.
As shown in figure 4, including following step for a kind of method of lithium ion cell electrode provided by the invention pre- embedding lithium in situ
It is rapid:
S1, under low humidity conditions, as depicted in figs. 1 and 2, on the top of metal electrode 2, connection lithium metal 1 is to form ginseng
Than electrode, which is passed through to the aperture 31 on 3 surface of cover board of lithium ion battery, inside lithium ion cell is inserted into, makes gold
Belong to lithium 1 to be immersed in the electrolyte of inside lithium ion cell, and is not contacted with battery core；
In a preferred embodiment of the invention, above-mentioned steps are needed in < 2%RH (relative humidity, Relative
Humidity it is operated under low-moisture conditions)；
S2, using the cathode of lithium ion battery as cathode, reference electrode is anode, right using low current charge certain time
The cathode of lithium ion battery carries out pre- embedding lithium；
S3, during the pre- embedding lithium of the cathode to lithium ion battery, it is real-time using voltage measuring apparatus (such as multimeter)
Monitor the cathode potential variation of lithium ion battery；When the cathode potential of lithium ion battery terminates current potential lower than first, stop negative
Extremely pre- embedding lithium, it can be achieved that embedding lithium pre- to cathode independent control；
In a preferred embodiment of the invention, the positive terminal of voltage measuring apparatus is connected into reference electrode, voltage is surveyed
The cathode for measuring the negative terminal connection lithium ion battery of device, realizes real-time monitoring；
S4, with lithium ion battery just extremely cathode, reference electrode are anode, it is right using low current charge certain time
The anode of lithium ion battery carries out pre- embedding lithium；
S5, during the positive pre- embedding lithium to lithium ion battery, it is real-time using voltage measuring apparatus (such as multimeter)
Monitor the anodic potentials variation of lithium ion battery；When the anodic potentials of lithium ion battery terminate current potential lower than second, stop just
Extremely pre- embedding lithium is, it can be achieved that independent control to the pre- embedding lithium of anode
In a preferred embodiment of the invention, the negative terminal of voltage measuring apparatus is connected into reference electrode, voltage is surveyed
The anode for measuring the positive terminal connection lithium ion battery of device, realizes real-time monitoring.
In the S1, metal electrode 2 is made of the metal that not reacting with lithium, as the pole of reference electrode,
It can be by 1 electronic conduction of lithium metal to external circuit.In a preferred embodiment of the invention, the metal electrode 2 uses
Platinum electrode, because metal platinum has the characteristics that performance stabilization, good conductivity.It is described in other preferred embodiments of the invention
Metal electrode 2 can also use copper electrode or silver electrode or nickel electrode etc..
In the S1, lithium metal 1 uses lithium piece or lithium band or lithium block etc., for providing the lithium source of pre- embedding lithium.At this
In the preferred embodiment of invention, the lithium metal 1 uses lithium piece, with a thickness of 0.1mm~1mm.
In the S1, the shape of metal electrode 2 is cylinder, and diameter is less than the diameter of the aperture 31 on 3 surface of cover board,
Ensure that top is connected with the metal electrode 2 of lithium metal 1 and can smoothly be inserted into the aperture 31 on 3 surface of cover board and enter lithium ion battery
Inside.In a preferred embodiment of the invention, the diameter of the metal electrode 2 is 1mm~10mm；3 table of cover board
The diameter of the aperture 31 in face is 2mm~12mm.Further, the aperture 31 is located at the negative pole and anode of lithium ion battery
Between pole.
In the S1, lithium metal 1 presses attached, or plating, or the package modes such as adhesive tape to be fixedly connected on metal by physics
The top outer surface of electrode 2.In a preferred embodiment of the invention, press attached mode that lithium piece is pressed abd fixed on gold by physics
Belong to the top outer surface of electrode 2, it is ensured that good contact between the two.
In the S2 and S4, low current charge is carried out using constant current charge-discharge instrument (such as new prestige battery test system),
And the electric current used is 10mA~100mA.Wherein, the low current of 10mA~100mA can reduce the positive and negative electrode of lithium ion battery
Polarization guarantees that lithium metal 1 is slowly dissolved, is embedded into lithium ion more uniformly in the positive or negative pole of battery, effectively improves electricity
The initial coulomb efficiency in pond.
In the S2, the cathode of lithium ion battery is using in natural graphite, artificial graphite, hard carbon, carbonaceous mesophase spherules
One or more of materials be made.In a preferred embodiment of the invention, the cathode of lithium ion battery is made of artificial graphite.
In the S4, the anode of lithium ion battery uses LiFePO4, cobalt acid lithium, LiMn2O4, nickel-cobalt-manganese ternary material
One or more of material be made.In a preferred embodiment of the invention, the anode of lithium ion battery uses LiFePO4 system
At.
In the S3, first terminates current potential (the termination current potential of pre- embedding lithium is carried out to cathode) as 0.1V~0.25V.This
First terminates current potential of the current potential lower than the generation of SEI film and is lower than the intercalation potential of artificial graphite (negative electrode material), it is ensured that gold
Belong to the dissolved part of lithium 1 and reacts generation SEI film with electrolyte, and rest part is embedded into artificial graphite interlayer.
In the S5, the second termination current potential (the termination current potential of pre- embedding lithium is carried out to anode) is 2.0V~3.0V.Phosphorus
The embedding de- lithium reaction platform of sour iron lithium (positive electrode) is 3.2V, and when carrying out embedding lithium to it, current potential can be reduced, therefore is arranged
Second termination current potential enable to lithium to be enriched in positive interpolar, to form the anode of rich lithium.
In the S3 and S5, during the positive or negative pole to lithium ion battery carries out pre- embedding lithium, reference electrode
It can extract out at any time, lithium metal is being replenished in time and then is being inserted into the inside of lithium ion battery.
The method of lithium ion cell electrode of the present invention pre- embedding lithium in situ, can lithium ion battery aging step it
After carry out, therefore the process of entire pre- embedding lithium be it is in situ, without as described in the prior art, after embedding lithium pre- to positive and negative electrode
It is assembled again.
Below by way of two specific embodiments, lithium ion cell electrode that the present invention will be described in detail provides pre- embedding lithium in situ
Method.
Embodiment 1
By taking rectangular aluminum-shell battery as an example, anode is made of LiFePO4, and cathode is made of graphite.It is made with platinum
Metal electrode 2, a diameter of 8mm form reference electrode in the lithium piece of its top outer surface package 1mm thickness；Reference electrode is inserted
Enter inside battery, guarantees that lithium piece is immersed in electrolyte.After the completion, using the cathode of battery as cathode, reference electrode is anode, even
It is connected to new prestige battery test system, low current charge certain time carries out pre- embedding lithium to cathode.Real-time monitoring is negative in the process
Electrode potential stops the pre- embedding lithium of cathode when cathode potential reaches 0.15V, extracts reference electrode out.And observe cathode in whole process
Current potential prevents the appearance of partial short-circuit with the presence or absence of exception.As shown in figure 3, at any time for current potential in the pre- process of intercalation of cathode
Change curve.1C cyclic charging and discharging test then is carried out to battery, voltage range is 2.5V~3.65V.
Embodiment 2
By taking rectangular aluminum-shell battery as an example, anode is made of LiFePO4, and cathode is made of graphite.It is made with platinum
Metal electrode 2, a diameter of 8mm form reference electrode in the lithium piece of its top outer surface package 1mm thickness.Reference electrode is inserted
Enter inside battery, guarantees that lithium piece is immersed in electrolyte.After the completion, with battery just extremely cathode, reference electrode are anode, even
It is connected to new prestige battery test system, low current charge certain time carries out pre- embedding lithium to anode.Real-time monitoring is being just in the process
Electrode potential stops the pre- embedding lithium of anode, extracts reference electrode out when anodic potentials reach 2.5V.And it observes positive in whole process
Current potential prevents the appearance of partial short-circuit with the presence or absence of exception.1C cyclic charging and discharging test then is carried out to battery, voltage range is
2.5V~3.65V.
Following table shows 1C initial charge capacity and the 1C discharge capacity, and library for the first time for the first time of embodiment 1 and embodiment 2
Logical sequence efficiency.
From above table as can be seen that using the independent pre- embedding lithium of positive or negative pole of the present invention to lithium ion battery, energy
Enough effectively improve initial coulomb efficiency.
In conclusion the method for lithium ion cell electrode provided by the present invention pre- embedding lithium in situ, compared with prior art,
It has the advantages that
1, can the positive or negative pole to battery individually control and carry out pre- embedding lithium, it is active in preliminary filling to reduce lithium ion battery
The consumption of lithium improves electrode interface characteristic, improves initial coulomb efficiency；
2, positive and negative electrode current potential can be monitored in the pre- embedding lithium of battery, stops pre- embedding lithium when reaching preset termination current potential, prevented
Only too little or too much embedding lithium reasonably controls lithium-inserting amount；
3, positive and negative electrode state of interface can be monitored in the pre- embedding lithium of battery, when appearance potential exception quickly judges neutralization electrode；
4, pre- embedding lithium in situ can be carried out after lithium ion battery assembly, fluid injection, aging step, without to positive and negative electrode
It is assembled again after pre- embedding lithium；
5, simple and reliable, it is time-consuming short, it is at low cost, it is effectively improved electrode interface.
It is discussed in detail although the contents of the present invention have passed through above preferred embodiment, but it should be appreciated that above-mentioned
Description is not considered as limitation of the present invention.After those skilled in the art have read above content, for of the invention
A variety of modifications and substitutions all will be apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (9)
1. a kind of method of lithium ion cell electrode pre- embedding lithium in situ, which is characterized in that comprise the steps of:
S1, under low humidity conditions, on the top of metal electrode, connection lithium metal forms reference electrode, which is passed through
The aperture of the lid surface of lithium ion battery, makes lithium metal be inserted into and be immersed in the electrolyte of inside lithium ion cell, and not
It is contacted with battery core；
S2, using the cathode of lithium ion battery as cathode, reference electrode is anode, using low current charge certain time, to lithium from
The cathode of sub- battery carries out pre- embedding lithium；
S3, during the pre- embedding lithium of the cathode to lithium ion battery, using voltage measuring apparatus real-time monitoring lithium ion battery
Cathode potential variation；When the cathode potential of lithium ion battery terminates current potential lower than first, stop the pre- embedding lithium of cathode, realization pair
The independent control of the pre- embedding lithium of cathode；
S4, with lithium ion battery just extremely cathode, reference electrode are anode, using low current charge certain time, to lithium from
The anode of sub- battery carries out pre- embedding lithium；
S5, during the positive pre- embedding lithium to lithium ion battery, using voltage measuring apparatus real-time monitoring lithium ion battery
Anodic potentials variation；When the anodic potentials of lithium ion battery terminate current potential lower than second, stop the pre- embedding lithium of anode, realization pair
The independent control of the pre- embedding lithium of anode.
2. the method for lithium ion cell electrode as described in claim 1 pre- embedding lithium in situ, which is characterized in that in the S1,
Metal electrode is using platinum electrode or copper electrode or silver electrode or nickel electrode.
3. the method for lithium ion cell electrode as described in claim 1 pre- embedding lithium in situ, which is characterized in that in the S1,
The shape of metal electrode is cylinder, and diameter is less than the opening diameter of lid surface.
4. the method for lithium ion cell electrode as described in claim 1 pre- embedding lithium in situ, which is characterized in that in the S1,
Lithium metal presses attached, or plating, or the mode of package adhesive tape to be fixedly connected on the top outer surface of metal electrode by physics.
5. the method for lithium ion cell electrode as described in claim 1 pre- embedding lithium in situ, which is characterized in that the S2 and S4
In, low current charge is carried out using constant current charge-discharge instrument, and the electric current used is 10mA~100mA.
6. the method for lithium ion cell electrode as described in claim 1 pre- embedding lithium in situ, which is characterized in that in the S3,
First terminates current potential as 0.1V~0.25V.
7. the method for lithium ion cell electrode as described in claim 1 pre- embedding lithium in situ, which is characterized in that in the S5,
Second terminates current potential as 2.0V~3.0V.
8. the method for lithium ion cell electrode as described in claim 1 pre- embedding lithium in situ, which is characterized in that the S3 and S5
In, during the positive or negative pole to lithium ion battery carries out pre- embedding lithium, reference electrode can be extracted out at any time, be replenished in time
Lithium metal and then the inside for being inserted into lithium ion battery.
9. the method for lithium ion cell electrode as described in claim 1 pre- embedding lithium in situ, which is characterized in that in lithium ion battery
Pre- embedding lithium in situ is carried out after assembly, fluid injection, aging step.
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| CN113640362A (en) * | 2021-07-15 | 2021-11-12 | 清华大学 | Reference electrode implantation method and three-electrode battery |
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