CN113540573A - Method for pulse forming lithium battery SEI film - Google Patents

Method for pulse forming lithium battery SEI film Download PDF

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Publication number
CN113540573A
CN113540573A CN202110636899.6A CN202110636899A CN113540573A CN 113540573 A CN113540573 A CN 113540573A CN 202110636899 A CN202110636899 A CN 202110636899A CN 113540573 A CN113540573 A CN 113540573A
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lithium battery
sei film
pulse
battery
formation
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唐谊平
江晨浩
单海鹏
张建力
陈强
侯广亚
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Zhejiang University of Technology ZJUT
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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
    • 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
    • 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
    • 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

In order to solve the problems that the conventional lithium battery negative electrode SEI film has poor electron isolation, and the battery capacity, the cycle performance and the rate performance are rapidly and obviously reduced due to continuous thickening and/or falling off in the charging and discharging processes of the battery, the invention provides a method for forming the SEI film of the lithium battery by pulse, wherein when the lithium battery is formed, pulse current is applied to charge the lithium battery; the pulse current setting duty ratio is more than or equal to 20%, the frequency is less than or equal to 5Hz, and the formation current multiplying power is controlled to be 0.05-0.15C. Method 1) of the present invention promotes Li and O by using a pulse current for formation of a battery2In Li2O2The diffusion frequency of the surface is increased, thereby promoting uniform mass transfer; 2) by accelerating the uniform mass transfer on the surface of the electrode, the formation and densification of an SEI film on the surface of the lithium negative electrode of the lithium battery can be accelerated; 3) the compactness of an SEI film on the surface of the lithium cathode of the lithium battery is improved, and the cycle stability and the rate performance of the lithium battery can be effectively improved.

Description

Method for pulse forming lithium battery SEI film
Technical Field
The invention belongs to the field of lithium batteries, and particularly relates to a method for forming a lithium battery SEI film by pulsing.
Background
The lithium-oxygen battery has the advantages of high working voltage, high specific capacity, good safety performance, strong environmental compatibility, no memory effect, wide working temperature range, small self-discharge, long cycle life and the like, and is widely applied to important fields of computers, portable electronic equipment, electric automobiles, medical technology, national defense industry, even aerospace and the like. Rechargeable lithium-oxygen battery systems have received much attention in recent years because they have an ultra-high theoretical energy density, which can provide about 5 times the energy density of conventional lithium-ion batteries.
However, the low rate performance, high charging voltage and poor cycling stability of the lithium-oxygen battery are the biggest challenges in practical application. The formation of lithium batteries is an important process that affects the battery performance, because metal lithium inevitably forms a passivation thin layer covering the electrode surface on the phase interface between the negative electrode and the electrolyte during the first charging process of the battery, which is called as the solid electrolyte phase interface or SEI film. The SEI film outer layer mainly consists of LiOH and Li2CO3The inner layer is mainly composed of Li2O, and the surface film has certain stability in organic electrolyte. In the battery cycle process, if the electron isolation characteristic of the SEI film is poor, electrons can contact with the electrolyte, the reduction reaction can further proceed, the content of lithium in the battery is consumed, the SEI film is continuously generated, and the cycle life of the battery is poor. Meanwhile, the SEI film can generate two phenomena of falling and thickening in the circulating process, fragments of the SEI film generated in the falling process enter an electrolyte, the electrophoresis phenomenon is generated under the action of voltage, and the generated fragments can be deposited on the surface of an electrode particularly in high-rate discharge; in the high-rate cycle process of the lithium ion battery, an SEI film of a negative electrode can obviously thicken. The two phenomena increase the surface resistance of the electrode, influence the extraction of lithium ions, and further influence the rate performance of the lithium ion battery.
At present, in the industrial production, two-stage low-current charging is mostly adopted for battery formation, the charging is carried out by using 0.02C low current to form an SEI film with better quality and interface but poor instability, then the charging is carried out by using 0.1C, and the charging is carried out by using a little larger current after the SEI film is basically formed, so that more time is saved, the formed SEI film is compact and has better thermal stability, the electrolyte is completely separated from a negative electrode by the SEI film at the moment, and only ions pass through the SEI film to reach the negative electrode. However, the rate performance of the battery is easily adversely affected by the dense SEI film formed in this manner, and high-rate charge and discharge cannot be achieved, or the SEI film is easily damaged under high-rate charge and discharge conditions.
Disclosure of Invention
The invention provides a method for forming a lithium battery SEI film by pulse, which aims to solve the problems that the existing lithium battery negative electrode SEI film is poor in electron isolation, and the capacity, the cycle performance and the rate performance of a battery are rapidly and obviously reduced due to continuous thickening and/or falling in the charging and discharging processes of the battery.
The invention aims to:
firstly, accelerating the formation rate of an SEI film on the surface of a negative electrode of a lithium battery;
secondly, improving the density of SEI on the surface of the negative electrode of the lithium battery;
and thirdly, improving the cycle performance and the rate capability of the lithium battery by improving the SEI film of the negative electrode of the lithium battery.
In order to achieve the purpose, the invention adopts the following technical scheme.
A method of pulsing an SEI film for a lithium battery,
the method comprises the following steps:
when the lithium battery is formed, pulse current is applied to charge the lithium battery;
the pulse current setting duty ratio is more than or equal to 20%, the frequency is less than or equal to 5Hz, and the formation current multiplying power is controlled to be 0.05-0.15C.
The invention carries out the formation of the battery by using the pulse current, and the high-frequency current enables Li and O2In Li2O2The diffusion frequency of the surface is increased, thereby promoting uniform mass transfer at the electrode surface. The pulsed current of the present invention should preferably be square wave pulses in practice.
In addition, the theory of the double diffusion layers considers that the pulse current with high frequency is short in electrifying time in a single cycleResulting in a diffusion layer caused by the pulse (pulse diffusion layer) not having time to spread to the convective boundary of the bulk solution. During the pulse, the concentration of the reaction particles in the pulse diffusion layer on the surface of the electrode is reduced, the pulse diffusion layer is supplemented by the main solution, the local concentration of the reaction particles in the main solution is reduced, and the deeper main solution is supplemented to the local part, which means that a new diffusion layer is built in the main solution of the electrolyte; during the pulse interval, the reactive particles are transported through this new diffusion layer to the pulse diffusion layer at the electrode surface, thereby raising the reactive particle concentration back in the pulse diffusion layer, as shown in fig. 4, Cs-CeIs a pulse diffusion layer, Ce-C0Is a new diffusion layer. Homogeneous transfer is realized, particle conveying is stably formed, concentration polarization formed by a main solution is avoided, uniform mass transfer process can promote uniform formation of an SEI film on the surface of an electrode, rapid formation of the SEI film is effectively promoted, and the structure is more compact.
Also, in the above scheme, the most critical parameter is the frequency of the pulse current. Under the condition of high frequency, a new diffusion layer established and formed in the electrolyte solution is difficult to keep stable, the uniformity of an SEI film on the surface of an electrode is influenced, and under the action of low-frequency pulse current, the double diffusion layer effect cannot be generated, so that the SEI film on the surface of the negative electrode of the lithium battery cannot be effectively improved actually. Comprehensive tests show that the double diffusion layers can be formed only marginally if the pulse current frequency is at least equal to or more than 0.8Hz, and further, the good effect of optimizing the SEI film on the surface of the lithium battery cathode is realized.
As a preference, the first and second liquid crystal compositions are,
the duty ratio of the pulse current is 45-55%, and the frequency is 1.0-1.5 Hz.
The duty cycle of the pulse current also has some effect on the formation of the double diffused layer. If the duty ratio is too high, the concentration of the reactive particles in the pulse diffusion layer becomes too high, and a new diffusion layer is easily lost, and concentration polarization is also easily caused. If the duty ratio is too low, concentration polarization tends to be formed in the host solution itself, and the quality of the SEI film tends to deteriorate.
As a preference, the first and second liquid crystal compositions are,
the duty ratio of the pulse current is 50%, and the frequency is 1 Hz.
The duty cycle and frequency described above can produce an optimal effect of pulsing into SEI films.
As a preference, the first and second liquid crystal compositions are,
the formation cut-off voltage is more than or equal to 4.0V.
Setting a higher cut-off voltage can facilitate the completion of SEI formation.
As a preference, the first and second liquid crystal compositions are,
the formation cut-off voltage is 4.4-4.7V.
Under the above-mentioned cut-off voltage conditions, the integrity and compactness of the SEI film are relatively high, and the thickness is moderate.
As a preference, the first and second liquid crystal compositions are,
the formation cut-off voltage is 4.6V.
The above-mentioned cutoff voltage is the optimum, most commonly used cutoff voltage. A relatively optimal technical effect can be produced.
As a preference, the first and second liquid crystal compositions are,
the formation current multiplying factor is 0.1C.
The formation current multiplying power actually influences the formation of a double diffusion layer in the pulse formation process and the processes of diffusion and particle transportation.
The invention has the beneficial effects that:
1) promotion of Li and O by cell formation using pulsed current2In Li2O2The diffusion frequency of the surface is increased, thereby promoting uniform mass transfer;
2) by accelerating the uniform mass transfer on the surface of the electrode, the formation and densification of an SEI film on the surface of the lithium negative electrode of the lithium battery can be accelerated;
3) the compactness of an SEI film on the surface of the lithium cathode of the lithium battery is improved, and the cycle stability and the rate performance of the lithium battery can be effectively improved.
Drawings
FIG. 1 is a graph comparing the cycle performance of lithium batteries of example 1 of the present invention with that of comparative example 1.
Fig. 2 is a graph of the cycle performance and the rate performance of example 2 with the trend of the pulse duty ratio.
FIG. 3 is a graph showing the relationship between the cycle performance and the rate performance of example 3 and the pulse frequency.
Fig. 4 is a theoretical concentration-potential diagram of a double diffusion layer.
Detailed Description
The invention is described in further detail below with reference to specific embodiments and the attached drawing figures. Those skilled in the art will be able to implement the invention based on these teachings. Moreover, the embodiments of the present invention described in the following description are generally only some embodiments of the present invention, and not all embodiments. Therefore, all other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without any creative effort shall fall within the protection scope of the present invention.
Unless otherwise specified, the raw materials used in the examples of the present invention are all commercially available or available to those skilled in the art; unless otherwise specified, the methods used in the examples of the present invention are all those known to those skilled in the art.
The invention adopts a test battery with the standard 2025 button cell specification as a test object for pulse formation.
Example 1
A method of pulsing into a lithium battery SEI film, the method comprising:
when the lithium battery is formed, pulse current is applied to charge the lithium battery;
the duty ratio of the pulse current is set to be 50%, the frequency is 1Hz, and the multiplying power of the formed current is controlled to be 0.10C.
Comparative example 1
The specific procedure was the same as in example 1, except that:
the formation is carried out by constant current without pulse.
The cycle performance test (1C) was performed for example 1 and comparative example 1. The test results are shown in FIG. 1.
As can be seen from fig. 1, in the first about 40 cycles, actually, the batteries of example 1 and comparative example 1 maintain relatively close performance, and the first 40 cycles can basically maintain 100% of the specific capacity with the second cycle as the standard specific capacity, but the specific capacity of comparative example 1 is obviously reduced in 41-60 cycles, while example 1 can basically maintain 100% of the specific capacity, and the relatively obvious reduction is not generated until about 74 cycles. At cycle 160, the specific capacity retention of the battery of example 1 was about 79.7%, while the specific capacity of the battery of comparative example 1 remained only about 59.4%, creating a large difference, with the decrease in specific capacity of comparative example 1 being about 2 times that of example 1.
Further, a high-rate charge-discharge cycle test was carried out, and the charge-discharge rate was 2C.
The comparative example 1 cell started producing a significant drop at about cycle 18 in the 2C cycle test, while the example 1 cell was able to remain up to about cycle 62, indicating that the example 1 cell had very good rate performance. Meanwhile, under the 2C test condition and at the 160 th cycle, the specific capacity retention rate of the embodiment 1 is about 71.4%, while the specific capacity retention rate of the comparative example 1 is only remained 41.3%, and the specific capacity reduction amplitude of the comparative example 1 is about 204% of that of the embodiment 1.
By combining the 1C normal-rate cycle and 2C high-rate cycle performance detection, it can be obviously seen that the lithium battery prepared by the pulse formation method provided by the invention has better electrochemical performance, and the SEI film on the surface of the negative electrode of the lithium battery is more compact and uniform.
Example 2
The specific operation was the same as example 1, except that the pulse current duty cycle was changed to set the test group shown in the following table, wherein the duty cycle was 0%, which is equivalent to the test group of comparative example 1, and the same 1C constant rate cycle and 2C high rate cycle performance tests as described above were performed. In the following table, the "standard capacity cycle number" is the standard capacity cycle number, which is the cycle number basically reaching 100% specific capacity retention rate, and the "capacity retention rate" is the retention rate of actual specific capacity at 160 cycles.
Figure BDA0003106122780000051
The specific trend is shown in fig. 2. It is evident from the above data and fig. 2 that a very significant performance peak exists at a duty cycle of 45-55%, mainly because a good double diffusion layer matching can be achieved with a suitable duty cycle. Not all double diffusion layer pulsing can be formed to produce good performance optimization effect on the battery.
Example 3
The specific operation was the same as example 1, except that the pulse current frequency setting was changed to the test group shown in the following table, and the same 1C constant rate cycle and 2C high rate cycle performance tests as described above were performed. In the following table, the "standard capacity cycle number" is the standard capacity cycle number, which is the cycle number basically reaching 100% specific capacity retention rate, and the "capacity retention rate" is the retention rate of actual specific capacity at 160 cycles.
Figure BDA0003106122780000052
The trend graph of specific cycle performance and rate performance versus pulse frequency is shown in fig. 3. As is apparent from the above table and fig. 3, the pulse frequency of the current has a very significant effect on the final pulsing effect of the lithium battery. In the initial stage, the formation effect increases first and then decreases with increasing frequency, and the effect is more significant in both cycle performance and rate performance. As can be seen from fig. 3, the influence of the pulse frequency on the capacity retention rate is more significant in practice, and particularly, the capacity retention rate at a high rate. In the range of 0.5-1.0 Hz, the capacity retention rate of a 2C high-rate cycle test is exponentially improved, and then the capacity retention rate is rapidly reduced after the capacity retention rate is higher than 2.0 Hz. In the aspects of normal multiplying power and high multiplying power, the frequency of pulse formation is more obvious for optimizing the electrochemical performance of the battery under the high multiplying power test condition.
And compared with the duty ratio of the pulse current, the influence of the frequency of the pulse current on the performance of the battery is obvious.
In conclusion, it can be seen from the examples, comparative examples and comparative tests that the formation method of the present invention can achieve a very excellent optimization effect on the performance of the lithium battery.

Claims (7)

1. A method of pulsing a lithium battery SEI film, the method comprising:
when the lithium battery is formed, pulse current is applied to charge the lithium battery;
the pulse current setting duty ratio is more than or equal to 20%, the frequency is less than or equal to 5Hz, and the formation current multiplying power is controlled to be 0.05-0.15C.
2. The method of claim 1, wherein the SEI film is formed by a pulse method,
the duty ratio of the pulse current is 45-55%, and the frequency is 1.0-1.5 Hz.
3. The method of claim 1, wherein the SEI film is formed by a pulse method,
the duty ratio of the pulse current is 50%, and the frequency is 1 Hz.
4. The method of claim 1, wherein the SEI film is formed by a pulse method,
the formation cut-off voltage is more than or equal to 4.0V.
5. The method of claim 1, wherein the SEI film is formed by a pulse method,
the formation cut-off voltage is 4.4-4.7V.
6. The method of claim 1, wherein the SEI film is formed by a pulse method,
the formation cut-off voltage is 4.6V.
7. The method of claim 1, wherein the SEI film is formed by a pulse method,
the formation current magnification was 0.1C.
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CN107146918A (en) * 2017-06-26 2017-09-08 浙江大学 A kind of pulse charge method applied to lithium metal battery
CN109390634A (en) * 2018-10-15 2019-02-26 珠海光宇电池有限公司 A kind of rapid forming method improving cathode SEI high-temperature stability
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US20200076010A1 (en) * 2018-09-05 2020-03-05 Faraday Technology, Inc. Pulse reverse current high rate electrodeposition and charging while mitigating the adverse effects of dendrite
CN111162332A (en) * 2019-12-20 2020-05-15 浙江大学 Pulse charging method based on characteristic frequency of power lithium ion battery

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4736150A (en) * 1986-07-09 1988-04-05 The United States Of America As Represented By The Secretary Of The Army Method of increasing the useful life of rechargeable lithium batteries
JPS6477432A (en) * 1987-09-16 1989-03-23 Mitsui Bussan Charge-and-discharge control of charging battery
JPH05114422A (en) * 1991-10-22 1993-05-07 Tokin Corp Lithium secondary battery
US7227336B1 (en) * 2002-04-02 2007-06-05 Van Schalkwijk Walter A Lithium ion rapid charging system and method
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Application publication date: 20211022