CN113921917B - Electrolyte infiltration method of lithium ion battery - Google Patents
Electrolyte infiltration method of lithium ion battery Download PDFInfo
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- CN113921917B CN113921917B CN202111164914.8A CN202111164914A CN113921917B CN 113921917 B CN113921917 B CN 113921917B CN 202111164914 A CN202111164914 A CN 202111164914A CN 113921917 B CN113921917 B CN 113921917B
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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
- H01M10/05—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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- 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
Abstract
The invention belongs to the technical field of lithium ion battery preparation, and particularly relates to an electrolyte infiltration method of a lithium ion battery. The invention provides an electrolyte infiltration method of a lithium ion battery pole piece, which comprises the following steps: high-pressure liquid injection, primary placement, primary pre-charging, secondary placement, secondary pre-charging, tertiary placement, liquid supplementing and limitation on the secondary pre-charging step. The method is suitable for all lithium ion batteries, especially square lithium batteries, and solves the problem that the infiltration effect of a thick and large square battery is difficult to improve. By adopting the method provided by the invention, the infiltration effect of the battery can be obviously improved, the liquid absorption amount of the electrolyte is obviously improved, and the internal resistance of the battery is obviously reduced.
Description
Technical Field
The invention belongs to the technical field of lithium ion battery preparation, and particularly relates to an electrolyte infiltration method of a lithium ion battery.
Background
At present, the market of lithium ion batteries is getting bigger, the requirements of customers on the energy density of the batteries are getting higher, the requirements on the size of the batteries are getting bigger, and in order to improve the quick charging capacity, the coating thickness in the batteries is continuously reduced, so that the space for soaking pole piece active substances and electrolyte is getting smaller; in order to improve the energy density, the free space in the battery is continuously reduced, so that the electrolyte can be stored everywhere. Along with the requirement on the stability of the battery, the application of nickel single crystals and high-nickel single crystal materials in the positive electrode is more and more, and the problem that the pole piece cannot be completely soaked is gradually generalized.
The pole piece soaking difficulty can cause the battery to have cycle water jump, even the lithium releasing and embedding capacity of different positions of the pole piece is inconsistent, partial area lithium separation is caused, and thermal runaway is more serious. At present, the traditional lithium ion infiltration process is that liquid is injected at a time under high pressure, a pole piece is naturally placed at high temperature, pre-charged and finally subjected to liquid supplementing and formation. The method aims at the problem that the existing small cylindrical, small soft package and small square batteries cannot be soaked difficultly, but the existing thick and large square batteries cannot be soaked well, the electrolyte is injected once, but the electrolyte can be sucked out by negative-pressure pre-charging, the soaking is not good, the pre-charging is carried out again, an area which can be found that the positive center of a positive pole piece and the negative pole piece cannot be soaked is formed, and a gluing diaphragm is used for ensuring that the positive interface and the negative interface of the pole piece are well jointed, so that the pole piece is difficult to soak.
At present, the problem of electrolyte infiltration of a pole piece is difficult to further improve by using a traditional method, and particularly for a square thick and large battery for power application, the difficulty of improving the infiltration performance of the pole piece is more important.
Disclosure of Invention
Therefore, the technical problem to be solved by the present invention is to overcome the defects that the conventional lithium ion battery pole piece infiltration method in the prior art is not suitable for a relatively thick and large square battery, and the infiltration effect is difficult to further improve, thereby providing an electrolyte infiltration method for a lithium ion battery.
Therefore, the invention provides the following technical scheme:
the invention provides an electrolyte infiltration method of a lithium ion battery, which comprises the following steps: injecting liquid at high pressure, placing for one time, pre-charging for one time, placing for the second time, pre-charging for the second time, placing for the third time and supplementing liquid, wherein the pre-charging step for the second time comprises the following stages:
an initial stage: charging to 3.0-3.2V by using multiplying current of 0.05-0.2C, setting at least one pulse discharge process in the charging process, wherein the vacuum degree is-50 to-70 kPa;
an intermediate stage: charging to 3.2-3.5V by using multiplying current of 0.1-0.5C, setting at least one pulse discharge process in the charging process, wherein the vacuum degree is-60 to-80 kPa;
and (3) final stage: charging to 3.5-battery cut-off voltage by using multiplying current of 0.3-0.5C, and setting at least one pulse discharge process in the charging process, wherein the vacuum degree is-70 to-100 kPa.
Optionally, the discharge rate of the initial stage is 0.05-0.1C, and the discharge time is 2-15 s;
the discharge rate of the intermediate stage is 0.1-0.5C, and the discharge time is 2-15 s;
the discharge multiplying power of the final stage is 0.3-0.5C, and the discharge time is 2-15 s.
Optionally, the initial stage, the intermediate stage and the final stage are respectively provided with 2-5 times of pulse discharge.
Optionally, the initial stage, the intermediate stage and the final stage are respectively kept still for 1-10 min.
Optionally, the operating temperature of the secondary pre-charging step is 35-55 ℃; the cell is pressurized for 500-1000N.
Optionally, the high-pressure electrolyte injection operation is to inject electrolyte with a designed electrolyte injection amount of 90-100% into the battery by adopting a vacuum and high-pressure circulating electrolyte injection mode;
optionally, one cycle of the vacuum and high-pressure circulating injection mode is as follows: negative pressure of-50 to-100 kPa, pressure maintaining of 10 to 30s, positive pressure of 500 to 800kPa, pressure maintaining of 10 to 30s, and electrolyte injection, wherein the cycle time is 4 to 10 times.
Optionally, the first laying aside and the second laying aside are carried out at the temperature of 35-55 ℃ for 4-10 h;
and carrying out vibration operation in the three times of laying.
Optionally, the operation temperature of the primary pre-charging is 25-45 ℃, and the primary pre-charging is charged to 2.5-2.7V by using a multiplying current of 0.01-0.1C.
Optionally, the liquid supplementing step is normal-pressure liquid supplementing, and the liquid supplementing is carried out until the designed liquid injection amount is reached.
Optionally, the lithium ion battery is a square lithium battery, the battery case is made of aluminum, steel or plastic, the length of the battery is greater than or equal to 100mm, the height of the battery is greater than or equal to 80mm, and the thickness of the battery is greater than or equal to 30mm.
Optionally, the length of the battery is 100-1200 mm, the height is 80-200 mm, and the thickness is 30-100 mm.
Preferably, the method for infiltrating the electrolyte into the lithium ion battery pole piece provided by the invention comprises the following steps:
injecting liquid at high pressure: injecting the electrolyte into the square battery by adopting multiple cycles, wherein the injection amount is 90-100% of the designed injection amount; one circulation is that the vacuum pumping is carried out under the negative pressure of-100 kPa, the pressure is maintained for 30s, the positive pressure is 800kPa, and the electrolyte is injected under the pressure maintained for 10 s; the cycle times are 4-10.
The design injection amount is calculated by the method that the electrolyte amount = the battery capacity and the injection coefficient is 2.0-4.0.
Primary shelving: the battery is placed for 4-10 h in an environment with the temperature of 35-55 ℃ to ensure that the active substances of the pole piece are preliminarily soaked by the electrolyte.
Primary pre-charging: the battery is charged to 2.5V-2.7V by using 0.05C current in an environment of 25-45 ℃, and the aim is to enable the negative coating to release internal stress, promote physical expansion to be released, increase internal pores and absorb electrolyte.
Secondary shelving: the battery is placed for 4 to 10 hours again in an environment with the temperature of 35 to 55 ℃ so as to ensure that the pole piece active substances which have fully absorbed the electrolyte are completely soaked by the electrolyte.
Secondary pre-charging: fully activating active materials in the battery, further controlling the stability of an SEI film of the battery, and adopting the following requirements for charging:
the secondary pre-charging condition is that the large surface is pressurized for 500-1000N, in order to ensure that the thickness of the battery is controlled, the interface contact of the surfaces of the positive electrode and the negative electrode is good, and the occurrence of lithium precipitation is avoided;
the pre-charging process is carried out in an environment of 35-55 ℃, so that the high quality and stability of the formed film of the negative electrode SEI film at the temperature are ensured;
the pre-charging process adopts the step-type vacuum pumping of-50 to-100 kPa, so that harmful gas of side reaction in the pre-charging process is discharged, and meanwhile, the electrolyte cannot be sucked out;
in the initial stage, 0.05-0.2C is used for charging to 3.2V, two pulse discharging processes are added in the charging process, for example, 10-second low-current discharging is carried out when the voltage reaches 2.8 and 3.2V, and the discharging multiplying power is 0.05-0.1C; the vacuum of-50 to-70 kPa in the whole process ensures that the film formation of the negative electrode is fully compact; standing for 1min after finishing;
in the middle stage, 0.1-0.5C is used for charging to 3.5V, two pulse discharging processes are added in the charging process, for example, 10-second low-current discharging is carried out when the voltage reaches 3.3V and 3.5V, and the discharging multiplying power is 0.1-0.5C; the whole process is carried out under vacuum of-60 to 80kPa, and then standing is carried out for 1min;
in the final stage, charging to 3.7V by using 0.3-0.5C, and adding two pulse discharging processes in the charging process, for example, discharging at low current for 10 seconds when the voltage reaches 3.6V and 3.7V, wherein the discharging multiplying power is 0.3-1C; the whole process is carried out under vacuum of-70-100 kPa, and then the mixture is kept stand for 1min.
Standing for three times: placing the battery in an environment of 35-55 ℃ for 4-10 h again, placing the battery on a vibration table under the condition of continuously bearing 500-1000N clamping pressure, synchronously applying a certain waveform to vibrate, such as sine waveform, logarithmic sweep frequency and the like, and the frequency: 1-300 Hz, and the amplitude is less than 1mm; the battery can vibrate for 1-6h in three directions of XYZ, and aims to ensure that pole piece active substances which have fully absorbed the electrolyte are completely soaked by the electrolyte, and the positive and negative electrodes are tightly attached to the interface of the diaphragm, so that the internal resistance of the battery can be obviously reduced.
Liquid supplementing: and (3) supplementing the rest electrolyte which is not injected, and if the electrolyte is lost in the pre-charging stage, adding the electrolyte amount lost in the pre-charging in the first two steps to ensure that the electrolyte injection amount of the battery is consistent, wherein high-pressure electrolyte injection is not needed in the process, and the conventional pressure electrolyte injection is only needed.
The technical scheme of the invention has the following advantages:
the invention provides an electrolyte infiltration method of a lithium ion battery pole piece, which comprises the following steps: high-pressure liquid injection, primary placement, primary pre-charging, secondary placement, secondary pre-charging, tertiary placement, liquid supplementing, and limits the secondary pre-charging steps, the internal stress of the internal pole pieces of the battery can be fully released after the electrolyte is injected, the porosity of the positive pole piece and the porosity of the negative pole piece are increased, the electrolyte is in more full contact with internal particles, the suction capacity of the electrolyte is increased, and the infiltration effect is improved.
The electrolyte infiltration method of the lithium ion battery pole piece provided by the invention has the advantages that the discharge multiplying power and the discharge time are limited, the polarization of the electrolyte is eliminated in the pre-charging process, the side reaction can be reduced on the surface of the negative electrode, the orderly and uniform SEI film is formed, the electrolyte is further distributed more uniformly, and the infiltration effect is improved.
According to the electrolyte infiltration method for the lithium ion battery pole piece, provided by the invention, the standing is carried out at each stage of secondary pre-charging, so that the molecular diffusion capacity of the electrolyte under high temperature and vibration is enhanced, and the effect that the electrolyte enters the pole piece deeper can be further improved.
According to the electrolyte infiltration method of the lithium ion battery pole piece, the operation temperature of the secondary pre-charging step is 35-55 ℃; the battery is pressurized for 500-1000N, so that the thickness of the battery can be controlled, the surface interfaces of the positive and negative electrodes are in good contact, and the occurrence of lithium precipitation is avoided.
According to the electrolyte infiltration method for the lithium ion battery pole piece, provided by the invention, high-pressure injection is carried out by adopting a vacuum and high-pressure circulating injection mode, internal air is more thoroughly evacuated by vacuumizing, the electrolyte can be injected into the place which is most difficult to infiltrate by the high-pressure injection, meanwhile, the working procedure time is reduced, and the productivity is improved.
According to the electrolyte infiltration method of the lithium ion battery pole piece, provided by the invention, the vibration operation is carried out in the three-time laying process, so that the pole piece active substances which have fully absorbed the electrolyte are completely infiltrated by the electrolyte, and the positive electrode and the negative electrode are tightly attached to the diaphragm interface.
The electrolyte infiltration method of the lithium ion battery pole piece is suitable for all lithium ion batteries, is particularly suitable for square lithium batteries, and solves the problem that the infiltration effect of the square batteries with larger thickness is difficult to improve. By adopting the method provided by the invention, the infiltration effect of the battery can be obviously improved, the liquid absorption amount of the electrolyte is obviously improved, and the internal resistance of the battery is obviously reduced.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the prior art descriptions will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a process flow diagram of an electrolyte infiltration method for a lithium ion battery pole piece according to the present invention;
FIG. 2 is a photograph of the negative electrode sheet after impregnation in example 1 of the present invention;
fig. 3 is a photograph of the negative electrode sheet after impregnation in comparative example 1 of the present invention.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
Example 1
The embodiment provides an electrolyte infiltration method of a lithium ion battery, which comprises the following specific operations:
high-pressure liquid injection, namely injecting electrolyte into a square battery with the model of 2MEB (44.3 × 220 × 122) by adopting 10 times of circulation, wherein the capacity of the battery is 180Ah, and the battery mainly comprises a battery structural member, a diaphragm, the electrolyte, a positive electrode and a negative electrode. The structural component is an external structure formed by welding an aluminum cover plate and an aluminum shell, a positive plate, a negative plate and a diaphragm are stacked layer by layer in the shell, and electrolyte is injected into the shell through a liquid injection hole reserved in the cover plate to infiltrate the positive plate, the negative plate and the diaphragm. The electrolyte is DMC: and (EC): DEC: EMC =1:1:1:1, wherein the injection amount is 90% of the design injection amount 540 g; the positive plate composition was NCM 811/conductive agent/binder =97:1:2, the negative plate composition is graphite/conductive agent/binder =96:1:3, the diaphragm is PE + ceramic + PVDF, the total thickness is 16um (the thickness ratio of the three is 12.
And (3) laying aside for one time, and placing the battery for 4 hours in an environment of 45 ℃ to ensure that the active substances of the pole piece are preliminarily soaked by the electrolyte.
The battery is charged to 2.5V and cut off by pre-charging at a time, and the current of 0.05C is used in the environment of 45 ℃, so that the internal stress of the negative coating is released, the physical expansion is promoted to be released, the internal pores are increased, and the electrolyte is absorbed.
And (4) laying aside for the second time, and placing the battery for 4 hours again in an environment of 45 ℃ to ensure that the pole piece active substances which have fully absorbed the electrolyte are completely soaked by the electrolyte.
Secondary pre-charging, fully activating active materials in the battery, further controlling the stability of an SEI film of the battery, and charging by adopting the following requirements:
the pre-charging condition of the battery is that the large surface is pressurized for 1000N, in order to ensure that the thickness of the battery is controlled, the surface interfaces of the positive and negative electrodes are in good contact, and the occurrence of lithium separation is avoided;
the pre-charging process is carried out in an environment of 45 ℃, so that the high quality and stability of the formed film of the negative electrode SEI film at the temperature are ensured;
the pre-charging process adopts the step-type vacuum pumping of-50 to-100 kPa, so that harmful gas of side reaction in the pre-charging process is discharged, and meanwhile, the electrolyte cannot be sucked out;
an initial stage:
a precharge procedure initially charges to 2.8V using a 0.05C rate,
b discharge at 0.1C rate for 10 seconds,
c is charged to 3.2V using a rate of 0.05C,
d, performing 0.1C rate discharge for 10 seconds,
the discharge mainly eliminates the concentration polarization of lithium ions that are not fully formed during the pre-charging process, and promotes the reduction of side reactions. The vacuum of-50 kPa in the whole process ensures that the film formation of the cathode is fully compact; standing for 1min after completion;
an intermediate stage:
a is charged to 3.3V using a rate of 0.1C,
b discharge at 0.5C rate for 10 seconds,
c is charged to 3.5V using a rate of 0.1C,
d, performing 0.5C rate discharge for 10 seconds,
the whole process is carried out under vacuum of-60 kPa, and then standing is carried out for 1min;
and (3) final stage:
a is charged to 3.6V using a rate of 0.3C,
b discharge at 0.5C rate for 10 seconds,
c is charged to 3.7V using a 0.3C rate,
d, performing 0.5C rate discharge for 10 seconds,
the whole process is carried out under vacuum of-80 kPa, and then standing is carried out for 1min.
Laying aside for three times, placing the battery for 4 hours again in an environment of 45 ℃, continuously bearing the clamping pressure of 800N, placing the battery on a vibrating table in the placing process, and synchronously applying sine waveforms and frequencies: 1-100 Hz, amplitude 0.2mm, vibrating in XYZ three directions for 2h, and finishing.
Liquid supplementing: and (3) supplementing the rest electrolyte which is not injected, if the electrolyte is lost in the pre-filling stage, adding the electrolyte amount lost in the pre-filling stage in the first two steps to ensure that the electrolyte injection amount of the battery is consistent, and the process does not need high-pressure electrolyte injection and can be used for conventional pressure electrolyte injection.
The pre-charged square battery is continuously charged fully, disassembly is carried out to check the infiltration condition of the pole piece, fig. 2 is a photo of the cathode piece after infiltration, and the pole piece using the method has uniform color as can be seen from the photo. Other embodiments are close to the photographs of this embodiment and are not listed. The electrolyte absorption capacity is tested by adopting a method of disassembling the battery and weighing all pole pieces in the battery, the internal resistance of the battery is tested by adopting a method of discharging for 10s at 4C under the SOC of 50 percent, and specific results are shown in the following table.
Example 2
The embodiment provides an electrolyte infiltration method of a lithium ion battery, which comprises the following specific operations:
high-pressure liquid injection, namely injecting electrolyte into a square battery with the model of 2MEB (44.3 × 220 × 122) by adopting 10 times of circulation, wherein the capacity of the battery is 180Ah, and the battery mainly comprises a battery structural member, a diaphragm, the electrolyte, a positive electrode and a negative electrode. The structural member is an external structure formed by welding an aluminum cover plate and an aluminum shell, a positive plate, a negative plate and a diaphragm are mainly arranged in the shell and are stacked layer by layer through Z-shaped laminations, and electrolyte is injected into the shell through a liquid injection hole reserved in the cover plate to infiltrate the positive plate, the negative plate and the diaphragm. The electrolyte is DMC: EC: DEC: EMC =1:1:1:1, wherein the injection amount is 90% of the design injection amount 540 g; the positive plate composition was NCM 811/conductive agent/binder =97:1:2, the negative plate composition is graphite/conductive agent/binder =96:1:3, the diaphragm is PE + ceramic + PVDF, the total thickness is 16um (the thickness ratio of the three is 12.
And (3) laying aside for one time, and placing the battery for 4 hours in an environment of 45 ℃ to ensure that the active substances of the pole piece are preliminarily soaked by the electrolyte.
The battery is charged to 2.8V and cut off by pre-charging at a time, and the current of 0.1C is used in the environment of 45 ℃, so that the internal stress of the negative coating is released, the physical expansion is promoted to be released, the internal pores are increased, and the electrolyte is absorbed.
And (4) placing the battery for the second time in an environment of 45 ℃ for 4 hours again, and aiming at ensuring that the pole piece active substances which have fully absorbed the electrolyte are completely soaked by the electrolyte.
Secondary pre-charging, fully activating active materials in the battery, further controlling the stability of an SEI film of the battery, and charging by adopting the following requirements:
the pre-charging condition of the battery is that the large surface is pressurized for 1000N, and in order to ensure that the thickness of the battery is controlled, the interface contact of the surfaces of a positive electrode and a negative electrode is good, and the occurrence of lithium precipitation is avoided;
the pre-charging process is carried out in an environment of 45 ℃, so that the high quality and stability of the formed film of the negative electrode SEI film at the temperature are ensured;
the pre-charging process adopts the step-type vacuum pumping of-50 to-100 kPa, so that harmful gas of side reaction in the pre-charging process is discharged, and meanwhile, the electrolyte cannot be sucked out;
an initial stage:
a precharge procedure initially charges to 2.8V using a 0.1C rate,
b discharge at 0.2C rate for 10 seconds,
c is charged to 3.2V using a 0.1C rate,
d, performing 0.2C rate discharge for 10 seconds,
the discharge is mainly to eliminate the concentration polarization of lithium ions that are not fully formed during the pre-charging, and to promote the reduction of side reactions. The vacuum of-50 kPa in the whole process ensures that the film formation of the cathode is fully compact; standing for 1min after completion;
an intermediate stage:
a charge to 3.3V using a rate of 0.2C,
b discharge at 0.7C rate for 10 seconds,
c is charged to 3.5V using a 0.2C rate,
d, performing 0.7C rate discharge for 10 seconds,
the whole process is carried out under vacuum of-60 kPa, and then standing is carried out for 1min;
and (3) final stage:
a is charged to 3.6V using a rate of 0.5C,
b discharge at 0.7C rate for 10 seconds,
c is charged to 3.7V using a 0.5C rate,
d, performing 0.7C rate discharge for 10 seconds,
the whole process is carried out under vacuum of-80 kPa, and then standing is carried out for 1min.
Laying aside for three times, placing the battery for 4 hours again in an environment of 45 ℃, continuously bearing 800N clamping pressure, placing the battery on a vibration table in the placing process, and synchronously applying sine waveforms and frequencies: 1-100 Hz, amplitude 0.2mm, vibrating in XYZ three directions for 2h, and finishing.
Fluid infusion: and (3) supplementing the rest electrolyte which is not injected, and if the electrolyte is lost in the pre-charging stage, adding the electrolyte amount lost in the pre-charging in the first two steps to ensure that the electrolyte injection amount of the battery is consistent, wherein high-pressure electrolyte injection is not needed in the process, and the conventional pressure electrolyte injection is only needed.
And continuously fully charging the pre-charged square battery, and disassembling to check the infiltration condition of the pole piece. The amount of electrolyte absorbed was measured by weighing all the pole pieces inside the battery by disassembling the battery, and the internal resistance of the battery was measured by discharging 4C for 10s at 50% SOC, the specific results are shown in the following table.
Example 3
The embodiment provides an electrolyte infiltration method of a lithium ion battery, which comprises the following specific operations:
high-pressure liquid injection, namely injecting electrolyte into a square battery with the model of 2MEB (44.3 × 220 × 122) by adopting 10 times of circulation, wherein the capacity of the battery is 180Ah, and the battery mainly comprises a battery structural member, a diaphragm, the electrolyte, a positive electrode and a negative electrode. The structural component is an external structure formed by welding an aluminum cover plate and an aluminum shell, a positive plate, a negative plate and a diaphragm are stacked layer by layer in the shell, and electrolyte is injected into the shell through a liquid injection hole reserved in the cover plate to infiltrate the positive plate, the negative plate and the diaphragm. The electrolyte is DMC: and (EC): DEC: EMC =1:1:1:1, wherein the injection amount is 90% of the design injection amount 540 g; the positive plate composition was NCM 811/conductive agent/binder =97:1:2, the negative plate composition is graphite/conductive agent/binder =96:1:3, the diaphragm is PE + ceramic + PVDF, the total thickness is 16um (the thickness ratio of the three is 12.
And (3) laying aside for one time, and placing the battery for 4 hours in an environment of 45 ℃ to ensure that the active substances of the pole piece are preliminarily soaked by the electrolyte.
The battery is charged to 2.5V and cut off by pre-charging at a time, and the current of 0.05C is used in the environment of 45 ℃, so that the internal stress of the negative coating is released, the physical expansion is promoted to be released, the internal pores are increased, and the electrolyte is absorbed.
And (4) placing the battery for the second time in an environment of 45 ℃ for 4 hours again, and aiming at ensuring that the pole piece active substances which have fully absorbed the electrolyte are completely soaked by the electrolyte.
Secondary pre-charging, fully activating active materials in the battery, further controlling the stability of an SEI film of the battery, and charging by adopting the following requirements:
the pre-charging condition of the battery is that the large surface is pressurized for 1000N, and in order to ensure that the thickness of the battery is controlled, the interface contact of the surfaces of a positive electrode and a negative electrode is good, and the occurrence of lithium precipitation is avoided;
the pre-charging process is carried out in an environment of 45 ℃, so that the high quality and stability of the formed film of the negative electrode SEI film at the temperature are ensured;
the pre-charging process adopts the step-type vacuum pumping of-50 to-100 kPa, so that harmful gas of side reaction in the pre-charging process is discharged, and meanwhile, the electrolyte cannot be sucked out;
an initial stage:
a precharge procedure initially charges to 2.8V using a 0.05C rate,
b discharge at 0.1C rate for 10 seconds,
c is charged to 3.0V using a rate of 0.05C,
d, performing 0.1C rate discharge for 10 seconds,
e is charged to 3.2V using a rate of 0.05C,
f discharge at 0.1C rate for 10 seconds,
the discharge is mainly to eliminate the concentration polarization of lithium ions that are not fully formed during the pre-charging, and to promote the reduction of side reactions. The vacuum of-50 kPa in the whole process ensures that the film formation of the cathode is fully compact; standing for 1min after completion;
an intermediate stage:
a is charged to 3.3V using a rate of 0.1C,
b discharge at 0.5C rate for 10 seconds,
c is charged to 3.4V using a rate of 0.1C,
d, performing 0.5C rate discharge for 10 seconds,
e charged to 3.5V using a rate of 0.1C,
f discharge at 0.5C rate for 10 seconds,
the whole process is carried out under vacuum of-60 kPa, and then standing is carried out for 1min;
and (3) final stage:
a charge to 3.6V using a rate of 0.3C,
b discharge at 0.5C rate for 10 seconds,
c is charged to 3.7V using a 0.3C rate,
d, performing 0.5C rate discharge for 10 seconds,
e charged to 3.8V using a rate of 0.3C,
f discharge at 0.5C rate for 10 seconds,
the whole process is carried out under vacuum of-80 kPa, and then standing is carried out for 1min.
Laying aside for three times, placing the battery for 4 hours again in an environment of 45 ℃, continuously bearing the clamping pressure of 800N, placing the battery on a vibrating table in the placing process, and synchronously applying sine waveforms and frequencies: 1-100 Hz, amplitude 0.2mm, vibrating in XYZ three directions for 2h, and finishing.
Liquid supplementing: and (3) supplementing the rest electrolyte which is not injected, and if the electrolyte is lost in the pre-charging stage, adding the electrolyte amount lost in the pre-charging in the first two steps to ensure that the electrolyte injection amount of the battery is consistent, wherein high-pressure electrolyte injection is not needed in the process, and the conventional pressure electrolyte injection is only needed.
And continuously fully charging the pre-charged square battery, and disassembling to check the infiltration condition of the pole piece. The electrolyte absorption capacity is tested by adopting a method of disassembling the battery and weighing all pole pieces in the battery, the internal resistance of the battery is tested by adopting a method of discharging for 10s at 4C under the SOC of 50 percent, and specific results are shown in the following table.
Example 4
The embodiment provides an electrolyte infiltration method of a lithium ion battery, which comprises the following specific operations:
high-pressure liquid injection, namely injecting electrolyte into a square battery with the model of 2MEB (44.3 × 220 × 122) by adopting 10 times of circulation, wherein the capacity of the battery is 180Ah, and the battery mainly comprises a battery structural member, a diaphragm, the electrolyte, a positive electrode and a negative electrode. The structural component is an external structure formed by welding an aluminum cover plate and an aluminum shell, a positive plate, a negative plate and a diaphragm are stacked layer by layer in the shell, and electrolyte is injected into the shell through a liquid injection hole reserved in the cover plate to infiltrate the positive plate, the negative plate and the diaphragm. The electrolyte is DMC: EC: DEC: EMC =1:1:1:1, wherein the injection amount is 90% of the design injection amount 540 g; the positive plate composition was NCM 811/conductive agent/binder =97:1:2, the negative plate composition is graphite/conductive agent/binder =96:1:3, the diaphragm is PE + ceramic + PVDF, the total thickness is 16um (the thickness ratio of the three is 12.
And (3) placing the battery for 4 hours at 45 ℃ for one-time placement, and aiming at ensuring that the active substances of the pole piece are primarily soaked by the electrolyte.
The battery is charged to 2.5V and cut off by pre-charging at a time, and the current of 0.05C is used in the environment of 45 ℃, so that the internal stress of the negative coating is released, the physical expansion is promoted to be released, the internal pores are increased, and the electrolyte is absorbed.
And (4) placing the battery for the second time in an environment of 45 ℃ for 4 hours again, and aiming at ensuring that the pole piece active substances which have fully absorbed the electrolyte are completely soaked by the electrolyte.
Secondary pre-charging, fully activating active materials in the battery, further controlling the stability of an SEI film of the battery, and charging by adopting the following requirements:
the pre-charging condition of the battery is that the large surface is pressurized for 1000N, and in order to ensure that the thickness of the battery is controlled, the interface contact of the surfaces of a positive electrode and a negative electrode is good, and the occurrence of lithium precipitation is avoided;
the pre-charging process is carried out in an environment of 45 ℃, so that the high quality and stability of the formed film of the negative electrode SEI film at the temperature are ensured;
the pre-charging process adopts the step-type vacuum pumping of-50 to-100 kPa, so that harmful gas of side reaction in the pre-charging process is discharged, and meanwhile, the electrolyte cannot be sucked out;
an initial stage:
a precharge procedure initially charges to 2.8V using a 0.05C rate,
b discharge at 0.1C rate for 10 seconds,
c is charged to 3.2V using a rate of 0.05C,
d, performing 0.1C rate discharge for 10 seconds,
the discharge mainly eliminates the concentration polarization of lithium ions that are not fully formed during the pre-charging process, and promotes the reduction of side reactions. The vacuum of-50 kPa in the whole process ensures that the film formation of the cathode is fully compact; standing for 1min after finishing;
an intermediate stage:
a is charged to 3.3V using a rate of 0.1C,
b discharge at 0.5C rate for 10 seconds,
c is charged to 3.5V using a rate of 0.1C,
d, performing 0.5C rate discharge for 10 seconds,
the whole process is carried out under vacuum of-60 kPa, and then standing is carried out for 1min;
and (3) final stage:
a is charged to 3.6V using a rate of 0.3C,
b discharge at 0.5C rate for 10 seconds,
c is charged to 3.7V using a 0.3C rate,
d discharging at 0.5C rate for 10s,
the whole process is carried out under vacuum of-80 kPa, and then standing is carried out for 1min.
Laying aside for three times, placing the battery for 4 hours again in an environment of 45 ℃, continuously bearing the clamping pressure of 800N, placing the battery on a vibrating table in the placing process, and synchronously applying sine waveforms and frequencies: 1-200 Hz, amplitude 0.5mm, vibrating for 4h in XYZ three directions, and finishing.
Liquid supplementing: and (3) supplementing the rest electrolyte which is not injected, and if the electrolyte is lost in the pre-charging stage, adding the electrolyte amount lost in the pre-charging in the first two steps to ensure that the electrolyte injection amount of the battery is consistent, wherein high-pressure electrolyte injection is not needed in the process, and the conventional pressure electrolyte injection is only needed.
And continuously fully charging the pre-charged square battery, and disassembling to check the soaking condition of the pole piece. The amount of electrolyte absorbed was measured by weighing all the pole pieces inside the battery by disassembling the battery, and the internal resistance of the battery was measured by discharging 4C for 10s at 50% SOC, the specific results are shown in the following table.
Comparative example 1
The comparative example provides an electrolyte infiltration method of a lithium ion battery, which comprises the following specific operations:
high-pressure liquid injection, namely injecting electrolyte into a square battery with the model of 2MEB (44.3 × 220 × 122) by adopting 10 times of circulation, wherein the capacity of the battery is 180Ah, and the battery mainly comprises a battery structural member, a diaphragm, the electrolyte, a positive electrode and a negative electrode. The structural component is an external structure formed by welding an aluminum cover plate and an aluminum shell, a positive plate, a negative plate and a diaphragm are stacked layer by layer in the shell, and electrolyte is injected into the shell through a liquid injection hole reserved in the cover plate to infiltrate the positive plate, the negative plate and the diaphragm. The electrolyte is DMC: and (EC): DEC: EMC =1:1:1:1, wherein the injection amount is 90% of the design injection amount 540 g; the positive plate composition was NCM 811/conductive agent/binder =97:1:2, the negative plate composition is graphite/conductive agent/binder =96:1:3, the diaphragm is PE + ceramic + PVDF, the total thickness is 16um (the thickness ratio of the three is 12.
And (3) laying aside for one time, and placing the battery for 10 hours in an environment of 45 ℃ to ensure that the active substances of the pole piece are preliminarily soaked by the electrolyte.
The battery is charged by one-time pre-charging and in an environment of 45 ℃ by adopting the following requirements:
the pre-charging condition of the battery is that the large surface is pressurized by 800N, and in order to ensure that the thickness of the battery is controlled, the interface contact of the surfaces of a positive electrode and a negative electrode is good, and the occurrence of lithium precipitation is avoided;
the pre-charging process is carried out in an environment of 45 ℃, so that the high quality and stability of the formed film of the negative electrode SEI film at the temperature are ensured;
the pre-charging process adopts the step-type vacuumizing of-50 to-100 kPa, so that harmful gases generated by side reactions in the pre-charging process are discharged, and the electrolyte cannot be sucked out;
an initial stage:
the precharge procedure is initially charged to 2.8V using a 0.05C rate,
the discharge is mainly to eliminate the concentration polarization of lithium ions that are not fully formed during the pre-charging, and to promote the reduction of side reactions. The vacuum of-50 kPa in the whole process ensures that the film formation of the cathode is fully compact; standing for 1min after completion;
an intermediate stage:
charging to 3.3V using a rate of 0.1C,
the whole process is carried out under vacuum of-60 kPa, and then standing is carried out for 1min;
and (3) final stage:
charge to 3.7V using a rate of 0.3C,
the whole process is carried out under vacuum of-80 kPa, and then standing is carried out for 1min.
Liquid supplementing: and (3) supplementing the rest electrolyte which is not injected, and if the electrolyte is lost in the pre-charging stage, adding the electrolyte amount lost in the pre-charging in the first two steps to ensure that the electrolyte injection amount of the battery is consistent, wherein high-pressure electrolyte injection is not needed in the process, and the conventional pressure electrolyte injection is only needed.
The pre-charged square battery is continuously charged fully, disassembly is carried out to check the infiltration condition of the pole pieces, fig. 3 is a photo of the cathode pieces after infiltration, and it can be seen from the picture that obvious black lines appear in the middle of the pole pieces without the use of the invention, the cathode is not fully infiltrated, and lithium can not be fully embedded in the cathode in the charging and discharging process. The electrolyte absorption capacity is tested by adopting a method of disassembling the battery and weighing all pole pieces in the battery, the internal resistance of the battery is tested by adopting a method of discharging for 10s at 4C under the SOC of 50 percent, and specific results are shown in the following table.
TABLE 1
| Liquid absorption of battery/g | Internal resistance of battery/m omega | |
| Example 1 | 476 | 0.68 |
| Example 2 | 473 | 0.68 |
| Example 3 | 475 | 0.67 |
| Example 4 | 477 | 0.64 |
| Comparative example 1 | 420 | 0.74 |
As can be seen from the data in the table, the method of the present invention can significantly improve the wetting compared with the comparative example, and the liquid absorption amount is increased by about 13%, and in addition, the internal resistance of the battery can be reduced.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the spirit or scope of the invention.
Claims (9)
1. The electrolyte infiltration method of the lithium ion battery is characterized by comprising the following steps: injecting liquid at high pressure, placing for one time, pre-charging for one time, placing for the second time, pre-charging for the second time, placing for the third time and supplementing liquid, wherein the pre-charging step for the second time comprises the following stages:
an initial stage: charging to 3.0-3.2V by using a multiplying current of 0.05C-0.2C, setting at least one pulse discharge process in the charging process, and controlling the vacuum degree to-50-70 kPa;
an intermediate stage: charging to 3.2 to 3.5V by using a multiplying current of 0.1C to 0.5C, setting at least one pulse discharge process in the charging process, and setting the vacuum degree to be-60 to-80 kPa;
and (3) final stage: charging to 3.5-battery cut-off voltage by using multiplying current of 0.3C-0.5C, setting at least one pulse discharge process in the charging process, wherein the vacuum degree is-70-100 kPa;
carrying out vibration operation in the third laying process;
the discharge multiplying power in the initial stage is 0.05 to 0.1C, and the discharge time is 2 to 15s;
the discharge multiplying power of the intermediate stage is 0.1-0.5C, and the discharge time is 2-15s;
the discharge multiplying power of the final stage is 0.3-0.5C, and the discharge time is 2-15s;
the operation of high-pressure liquid injection adopts a vacuum and high-pressure circulating liquid injection mode, and one cycle of the vacuum and high-pressure circulating liquid injection mode is as follows: and (4) keeping the pressure for 10 to 30s under negative pressure of-50 to-100 kPa, keeping the pressure for 10 to 30s under positive pressure of 500 to 800kPa, and injecting the electrolyte for 4 to 10 times.
2. The method for infiltrating the electrolyte into the lithium ion battery according to claim 1, wherein 2~5 pulse discharges are set in each of the initial stage, the intermediate stage and the final stage.
3. The method for infiltrating the electrolyte into the lithium ion battery according to claim 1, wherein the initial stage, the intermediate stage and the final stage are respectively kept still for 1-10min.
4. The method for impregnating the electrolyte solution in the lithium ion battery according to claim 1, wherein the operating temperature of the secondary precharging step is 35 to 55 ℃; pressurizing the battery for 500 to 1000N.
5. The electrolyte infiltration method of the lithium ion battery according to claim 1, wherein the high-pressure electrolyte injection is performed by injecting electrolyte with a designed electrolyte injection amount of 90-100% into the battery by adopting a vacuum and high-pressure circulating electrolyte injection mode.
6. The electrolyte infiltration method of the lithium ion battery according to claim 1, wherein the temperature of the first standing and the second standing are 35 to 55 ℃ and the time of the third standing is 4 to 10 hours.
7. The method for impregnating an electrolyte solution into a lithium ion battery according to claim 1, wherein the operating temperature of the one-time precharge is 25 to 45 ℃, and the battery is charged to 2.5 to 2.7V by using a current with a rate of 0.01 to 0.1C.
8. The method for infiltrating the electrolyte into the lithium ion battery according to claim 1, wherein the step of replenishing the electrolyte is replenishing the electrolyte at normal pressure, and the replenishing of the electrolyte is carried out to a designed electrolyte injection amount.
9. The method for infiltrating the electrolyte into the lithium ion battery according to any one of claims 1-8, wherein the lithium ion battery is a square lithium battery, the battery case is made of aluminum, steel or plastic, the length of the battery is greater than or equal to 100mm, the height of the battery is greater than or equal to 80mm, and the thickness of the battery is greater than or equal to 30mm.
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