CN109581240A - Lithium ion battery failure analysis method based on AC impedence method - Google Patents
Lithium ion battery failure analysis method based on AC impedence method Download PDFInfo
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The security performance of lithium ion battery is concerned, and analysis lithium easily occurs on negative electrode of lithium ion battery under abuse conditions, forms Li dendrite, battery thermal runaway is caused even to explode.Present invention employs the methods of electrochemical AC impedance test, analyze the relationship of AC impedance spectrum signal and cell internal environment, the variation of SEI film resistance can be analyzed from ac impedance spectroscopy, to realize in the case where not damaging battery, it quick and precisely predicts the dendrite internal short-circuit state of battery, and then assesses service life and the safety of battery.
Description
Technical field
The present invention relates to the analysis sides that lithium ion battery safety testing field more particularly to a kind of lithium ion battery fail
Method.
Background technique
The features such as lithium ion battery is because of its energy density height, good cycle and without memory effect, in consumption electricity
It is rapidly developed in sub- product scope, is most widely used one kind rechargeable battery in portable electronic device.With lithium ion
The development of battery technology is gradually used in the fields such as electric car, military affairs and aerospace.
However, lithium ion battery understands ageing failure, even there is security risk after recycling for a long time.Come from current research
See, the abuse conditions such as overcharge, short circuit, collision and overheat will cause the security risk of lithium ion battery, may cause lithium from
A series of sub- potential exothermic reactions of inside battery.Wherein, battery Carbon anode surface is easy to happen the deposition of lithium metal and is formed
Dendrite, dendritic growth can penetrate diaphragm to a certain extent and cause internal short-circuit, to cause battery failure even thermal runaway.Research is aobvious
Show, high current, low temperature, highly charged state (including overcharge) are the main reason for causing lithium ion batteries anodes failure.?
Under above-mentioned condition, it is easy to insufficient insertion of the lithium ion on cathode is caused, so that it is deposited on surface, it is raw in the form of dendrite
It is long, cause irreversible capacity attenuation even internal short-circuit.Therefore, the detection side of lithium ion batteries anodes lithium dendrite growth is found
Method prevents thermal runaway caused by battery internal short-circuit, has certain realistic meaning.
Direct dismantling is depended on currently, generally detecting battery and lithium deposition whether occurring, after circulation some cycles
Battery is directly disassembled, and whether observe on cathode pole piece has silvery white precipitate.This method has destructiveness, cannot achieve to using
The analysis or detection of middle battery.R.Bouchet et al. (R.Bouchet et al.An EIS Study of the Anode
Li/PEO-LiTFSI of a Li Polymer Battery.Journal of the Electrochemical,2003,
150:A1385-A1389) battery there may be Li dendrite is tested with AC impedance spectrum analysis (EIS) method,
Corresponding fitting circuit is established according to result.Tetsuya Osaka et al. (Tetsuya Osaka et al.Proposal
of novel equivalent circuit for electrochemical impedance analysis of
commercially available lithium ion battery.Journal of Power Sources,2012,205:
A1483-A1486) system is modeled with equivalent circuit appropriate, which includes that positive electrode different-grain diameter is brought
Various diffusion parameters, negative terminal surface solid electrolyte interface and electrochemical reaction and conductance part, it is various to what is used
The residual error that Study on Equivalent Circuit is generated by data fitting, analyzes industrial lithium ion cell electrode in different state-of-charges
Under electrochemical impedance, the circuit of proposition is evaluated.The above method can relatively accurately reflect in battery really
The variation of the relevant parameters such as resistance, so that predict that the generation of internal Li dendrite is possibly realized, but involved by the above method
Relevant parameter it is more, analytic process is relatively complicated, and operate larger workload.
Summary of the invention
In view of the deficiencies of the prior art, the object of the present invention is to provide a kind of lithium-ion electrics based on AC impedence method
Pond failure analysis method, impedance variations rule when analyzing Li dendrite deposition by ac impedance measurement method, thus to ion battery
The behavior failed because generating dendrite is judged, and the performance improvement for later period battery provides foundation and direction.
The technical solution used in order to solve the technical problem:
1. a kind of lithium ion battery failure analysis method based on AC impedence method, comprising the following steps:
1) select completely new lithium ion battery as sample to be tested, after chemical conversion, using constant current charge-discharge or constant current-
Constant pressure charge and discharge electrical method carries out normal charge and discharge cycles, is recycled to n1Circle, battery charge state is in 80%-100% after circulation terminates
Between SOC；
2) to being recycled to n1The battery of circle carries out EIS test using CHI660e electrochemical workstation, to EIS test result
Simulating equivalent circuit is constructed, which is connected by solution resistance, interface impedance, electric charge transfer and Warburg impedance three parts, molten
Liquid resistance is indicated by Re；Interface impedance is caused by negative terminal surface solid electrolyte membrane, by capacitor CSEIWith resistance RSEIIt composes in parallel,
It is expressed as CSEI//RSEI；Charge transfer portion is connected by a charge transfer resistance Rct with Warburg impedance Z w, then with permanent phase
Bit unit CPE is in parallel, and wherein Rct reflects the electric charge transfer step impedance of electrode, and Zw reflects the diffusional resistance of electrode diffusion layer, base
In analog circuit matched curve, resistance R is obtainedSEI, recycle n1The resistance of circle is denoted as RSEI,n1。
3) continue to carry out battery charge and discharge cycles to n2Circle repeats step 2), obtains resistance RSEI,n2, recycle later
To n3Circle repeats step 2), obtains RSEI,n3, by the above method, when to battery progress charge and discharge cycles to niWhen circle, it there are
To RSEI,n1-RSEI,niI R altogetherSEIResistance value；
4) R is drawnSEI,niAbout circulating ring number ni curve, R is obtainedSEIWith circulating cycle number change rule, overall trend and
Speech, RSEIIt is become larger with circulating cycle number, but in some circulating cycle number ngAfterwards, RSEIReduce suddenly, i.e. circulating cycle number ng
For the time that dendrite internal short-circuit will occur, Li dendrite produces destruction to SEI film in battery at this time.
Further, n1,n2,n3…niFor arithmetic progression.
Further, homemade LiCoO is used in step 1)2- MCMB system button cell, with LiCoO2It is living as anode
Property material, MCMB is as negative electrode active material, by 80%LiCoO2, 10%SuperP conductive black and 10% polyvinyladine floride
(PVDF) binder mixes, and with n-methyl-2-pyrrolidone (NMP) for solvent, obtains slurry after ball milling, is coated on aluminium foil,
Obtain anode pole piece；By 90%MCMB, 10%PVDF binder, equally using NMP as solvent, it is coated on copper foil, obtains after ball milling
To cathode pole piece, roll-in after positive and negative anodes pole piece is dry strikes out the pole piece of diameter 10mm, and diaphragm material is poly- the third of diameter 16mm
Alkene diaphragm, electrolyte are 1M LiPF6It is dissolved in ethylene carbonic ether (EC) and carbovinate rouge (DEC), dimethyl carbonate
(DMC) mixed solvent system, battery in glove box inert gas environment after the assembly is completed, with the low current of C/10 multiplying power into
Row 3 times circulations, are melted into.
Further, positive electrode LiCoO2It is 1.2:1,1.3:1 or 1.4:1 with cathode MCMB microballoon equivalent mass ratio.
Further, it is 4.4V or 4.6V that blanking voltage is overcharged in step 3).
Further, the AC signal amplitude that EIS is tested in step 2) is 5mV, and the frequency of scanning is 100kHz-
0.01Hz。
The present invention compared with prior art possessed by the utility model has the advantages that
Present invention employs the methods of electrochemical AC impedance test, analyze AC impedance spectrum signal and inside battery ring
The relationship in border can analyze the variation of SEI film resistance from ac impedance spectroscopy, thus realize in the case where not damaging battery,
It quick and precisely predicts the dendrite internal short-circuit state of battery, and then assesses service life and the safety of battery.
Detailed description of the invention
Fig. 1 is the electrochemical impedance spectroscopy (a) and RC analog circuit (b) that specific embodiment is tested.
Fig. 2 is the diffusion impedance R of 4.4V overcharge battery in embodiment 1SEIWith circulating cycle number relationship.
Fig. 3 is the optical microscopy and scanning electron microscope (SEM) photograph after battery overcharge to 4.4V.
Fig. 4 is the diffusion impedance R of 4.4V and 4.6V overcharge battery in embodiment 2SEIWith circulating cycle number relationship.
Fig. 5 be in embodiment 3 different quality than lower diffusion impedance RSEIWith circulating cycle number relationship.
Specific embodiment
For the ease of analysis, specific embodiment uses homemade LiCoO2- MCMB system button cell, with LiCoO2Make
For positive electrode active materials, MCMB is as negative electrode active material, by 80%LiCoO2, 10%SuperP conductive black and 10% poly- inclined
The mixing of fluorine ethylene (PVDF) binder obtains slurry after ball milling, is coated on aluminium with n-methyl-2-pyrrolidone (NMP) for solvent
On foil, anode pole piece is obtained；By 90%MCMB, 10%PVDF binder, equally using NMP as solvent, copper foil is coated on after ball milling
On, obtain cathode pole piece.Roll-in after positive and negative anodes pole piece is dry, strikes out the pole piece of diameter 10mm.Diaphragm material is diameter 16mm
Polypropylene diaphragm (Celgard), electrolyte be 1M LiPF6It is dissolved in ethylene carbonic ether (EC) and carbovinate rouge
(DEC), the mixed solvent system of dimethyl carbonate (DMC).Battery is in glove box inert gas environment (+5% hydrogen of 95% argon gas
Gas) in after the assembly is completed, 3 circulations are carried out with the low current of C/10 multiplying power, are melted into.
Battery is tested using battery charging and discharging test macro, and carries out EIS using CHI660e electrochemical workstation
It tests, AC signal amplitude is 5mV in EIS test, and the frequency of scanning is 100kHz-0.01Hz, is being charged to overcharge battery
EIS test is carried out under state, is constructed simulating equivalent circuit (as shown in Figure 1), the circuit is by solution resistance, interface impedance, charge
Transfer and the series connection of Warburg impedance three parts, solution resistance are indicated by Re；Interface impedance is mainly by negative terminal surface solid electrolyte
Film causes, by capacitor CSEIWith resistance RSEIIt composes in parallel, is expressed as CSEI//RSEI；Charge transfer portion is by an electric charge transfer electricity
Resistance Rct connects with Warburg impedance Z w, then in parallel with permanent phase element CPE, and wherein Rct reflects the electric charge transfer step of electrode
Impedance, Zw reflect the diffusional resistance of electrode diffusion layer.Overcharge circulating cycle number, mistake are analyzed using above-mentioned simulating equivalent circuit respectively
Charging voltage, positive and negative anodes are with the influence for comparing EIS result.
Embodiment 1
Battery is under 1C circulation, and using 4.4V as overcharge blanking voltage, the diffusion resistance of rechargeable battery is obtained in test
RSEIWith circulating cycle number change curve, as shown in Fig. 2, R under 4.4V overchargeSEINumerical value is very fast as circulating cycle number increases to be increased,
Before charge and discharge cycles in 30 weeks, superficial layer diffusion impedance RSEIGradually 224.2 Ω, table are increased to by 44.56 Ω after 10 weeks
It is bright in 4.4V by voltage under the conditions of overcharging, significant change occurs for material granule surface texture, SEI film with circulating cycle number increasing
Adding and obviously thickens, film resistance increases, and when being recycled to 40 weeks, RSEIValue becomes 157.3 Ω, reduces suddenly compared with 30 weeks, subsequent RSEI
585.4 Ω when continuing to increase to 50 weeks.
In order to be verified to prediction, to there is RSEIAfter value starts the battery dismantling of reduced inflection point, pass through optical microphotograph
Mirror and scanning electron microscopic observation cathode pole piece (as shown in figure 3, being the picture shot under different scale respectively), it can be found that pole piece table
There is the Li dendrite of cluster-shaped in face, illustrates that the unexpected reduction of RSEI is that Li dendrite causes, the growth of Li dendrite causes SEI film
Local failure, to reduce lithium ion in the diffusion impedance value of superficial layer.And Li dendrite only occurs in regional area at this time, still
Battery internal short-circuit is not directly contributed, and SEI film is repaired again in subsequent circulation, and film resistance continues to increase, but battery is subsequent quickly
Failure.Therefore, RSEIThe appearance of inflection point implies that Li dendrite generates destruction to SEI film in battery, prompts battery that will occur short in dendrite
Road.
Embodiment 2
As fixed positive electrode LiCoO2When with cathode MCMB microballoon equivalent mass ratio being 1.2:1, in 4.4V, 4.6V is different
By under voltage to battery carry out charge-discharge test.As a result as shown in figure 4, when battery charge cutoff voltage is set as 4.4V,
Before charge and discharge cycles in 30 weeks, superficial layer diffusion impedance gradually increases to 74.04 Ω by 25.67 Ω after 10 weeks, shows
SEI film progressive additive in cyclic process, the R in subsequent cyclic processS EIValue is reduced to 60.55 Ω；And when battery charges
When blanking voltage is 4.6V, superficial layer diffusion impedance is substantially reduced when being recycled to 20 weeks, is shown under overcharging state with cut-off electricity
The raising of pressure, lithium ion battery impedance increases, but RSEIValue starts reduced inflection point to be occurred earlier, illustrates to have occurred earlier interior
Short circuit.
Embodiment 3
When battery charge cutoff voltage is set as 4.4V, respectively to positive electrode LiCoO2It is equivalent with cathode MCMB microballoon
The battery of mass ratio 1.2:1,1.3:1 and 1.4:1 are tested, and battery is during charge and discharge cycles, superficial layer diffusion impedance
Gradually increase (as shown in Figure 5).Work as LiCoO2It with cathode MCMB microballoon equivalent mass ratio is 1.2:1 and when 1.3:1, RSEIInflection point
Appear in 40 weeks；When mass ratio is 1.4:1, RSEIInflection point appears in 30 weeks.Illustrate to increase with positive electrode extra proportion, lithium
, there is internal short-circuit time advance in the aggravation of internal short-circuit problem caused by dendrite.
Although for illustrative purposes, it has been described that exemplary embodiments of the present invention, those skilled in the art
Member it will be understood that, can be in form and details in the case where the scope and spirit for not departing from invention disclosed in appended claims
On the change that carry out various modifications, add and replace etc., and all these changes all should belong to appended claims of the present invention
Protection scope, and each step in the claimed each department of product and method, can in any combination
Form is combined.Therefore, to disclosed in this invention the description of embodiment be not intended to limit the scope of the invention,
But for describing the present invention.Correspondingly, the scope of the present invention is not limited by embodiment of above, but by claim or
Its equivalent is defined.
Claims (6)
1. a kind of lithium ion battery failure analysis method based on AC impedence method, comprising the following steps:
1) select completely new lithium ion battery as sample to be tested, after chemical conversion, using constant current charge-discharge or constant current-constant pressure
Charge and discharge electrical method carries out normal charge and discharge cycles, is recycled to n1Circle, after circulation terminates battery charge state 80%-100%SOC it
Between；
2) EIS test is carried out using CHI660e electrochemical workstation, simulating equivalent circuit, the circuit is constructed to EIS test result
It is connected by solution resistance, interface impedance, electric charge transfer and Warburg impedance three parts, solution resistance is indicated by Re；Interface impedance
Caused by negative terminal surface solid electrolyte membrane, by capacitor CSEIWith resistance RSEIIt composes in parallel, is expressed as CSEI//RSEI；Electric charge transfer
Part is connected by a charge transfer resistance Rct with Warburg impedance Z w, then in parallel with permanent phase element CPE, and wherein Rct is anti-
The electric charge transfer step impedance of electrode is reflected, Zw reflects the diffusional resistance of electrode diffusion layer, is based on analog circuit matched curve, obtains
Resistance RSEI, recycle n1The resistance of circle is denoted as RSEI,n1。
3) continue to carry out battery charge and discharge cycles to n2Circle repeats step 2), obtains resistance RSEI,n2, it is recycled to n later3
Circle repeats step 2), obtains RSEI,n3, by the above method, when to battery progress charge and discharge cycles to niWhen circle, it is obtained
RSEI,n1-RSEI,niI R altogetherSEIResistance value；
4) R is drawnSEI,niAbout circulating ring number ni curve, R is obtainedSEIWith the rule that circulating cycle number changes, for overall trend,
RSEIIt is become larger with circulating cycle number, but in some circulating cycle number ngAfterwards, RSEIReduce suddenly, i.e. circulating cycle number ngFor
The time of dendrite internal short-circuit will occur, Li dendrite produces destruction to SEI film in battery at this time.
2. according to the method described in claim 1, it is characterized by: using homemade LiCoO in step 1)2- MCMB system button
Battery, with LiCoO2As positive electrode active materials, MCMB is as negative electrode active material, by 80%LiCoO2, 10%SuperP it is conductive
Carbon black and the mixing of 10% polyvinyladine floride (PVDF) binder, with n-methyl-2-pyrrolidone (NMP) for solvent, after ball milling
It to slurry, is coated on aluminium foil, obtains anode pole piece；By 90%MCMB, 10%PVDF binder, equally using NMP as solvent, ball
It is coated on copper foil after mill, obtains cathode pole piece, roll-in after positive and negative anodes pole piece is dry strikes out the pole piece of diameter 10mm, diaphragm
Material is the polypropylene diaphragm of diameter 16mm, and electrolyte is 1M LiPF6It is dissolved in ethylene carbonic ether (EC) and carbovinate rouge
(DEC), the mixed solvent system of dimethyl carbonate (DMC), battery in glove box inert gas environment after the assembly is completed, with C/
The low current of 10 multiplying powers carries out 3 circulations, is melted into.
3. according to the method described in claim 2, it is characterized by: positive electrode LiCoO2With cathode MCMB microballoon equivalent mass
Than for 1.2:1,1.3:1 or 1.4:1.
4. method according to claim 1-3, it is characterised in that: overcharged in step 3) blanking voltage be 4.4V or
4.6V。
5. method according to claim 1-4, it is characterised in that: the AC signal width that EIS is tested in step 2)
Value is 5mV, and the frequency of scanning is 100kHz-0.01Hz.
6. according to the method described in claim 1, it is characterized by: n1,n2,n3…niFor arithmetic progression.
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| CN110146826A (en) * | 2019-06-06 | 2019-08-20 | 南京航空航天大学 | Commercial li-ion battery electrode degradation analysis method based on three-electrode system |
| CN110568363A (en) * | 2019-07-29 | 2019-12-13 | 国网河南省电力公司电力科学研究院 | Method for prejudging lithium dendrite generation of retired battery based on SEI film impedance change |
| CN111458642A (en) * | 2020-04-22 | 2020-07-28 | 上海空间电源研究所 | Nondestructive testing method for lithium separation of lithium ion storage battery |
| CN111766527A (en) * | 2020-07-03 | 2020-10-13 | 上海大学 | Method for predicting capacity of all-solid-state polymer electrolyte lithium battery in physical aging process |
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| CN114142096A (en) * | 2021-10-20 | 2022-03-04 | 合肥国轩高科动力能源有限公司 | Method for reducing low SOC impedance of lithium ion battery |
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| CN110568363A (en) * | 2019-07-29 | 2019-12-13 | 国网河南省电力公司电力科学研究院 | Method for prejudging lithium dendrite generation of retired battery based on SEI film impedance change |
| CN114402473A (en) * | 2019-09-13 | 2022-04-26 | 日产自动车株式会社 | All-solid-state lithium ion secondary battery system and charging device for all-solid-state lithium ion secondary battery |
| CN111458642A (en) * | 2020-04-22 | 2020-07-28 | 上海空间电源研究所 | Nondestructive testing method for lithium separation of lithium ion storage battery |
| CN111766527A (en) * | 2020-07-03 | 2020-10-13 | 上海大学 | Method for predicting capacity of all-solid-state polymer electrolyte lithium battery in physical aging process |
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| CN113258151A (en) * | 2021-04-25 | 2021-08-13 | 同济大学 | Lithium ion battery charging method capable of avoiding lithium separation |
| CN113258151B (en) * | 2021-04-25 | 2022-10-25 | 同济大学 | Lithium ion battery charging method capable of avoiding lithium separation |
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| CN115524628B (en) * | 2022-10-11 | 2023-07-18 | 欣旺达电子股份有限公司 | Soft package lithium ion battery capacity decay failure analysis method and system |
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