CN109581240B - Lithium ion battery failure analysis method based on alternating current impedance method - Google Patents
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Abstract
The safety performance of the lithium ion battery is concerned, and lithium is easy to be separated out from the negative electrode of the lithium ion battery under an abuse condition to form lithium dendrite, so that the battery is out of control thermally and even explodes. The invention adopts an electrochemical alternating-current impedance test method, analyzes the relation between an alternating-current impedance spectrum signal and the internal environment of the battery, and can analyze the resistance change of the SEI film from the alternating-current impedance spectrum, thereby realizing the rapid and accurate prediction of the short circuit state in the dendritic crystal of the battery under the condition of not damaging the battery, and further evaluating the service life and the safety of the battery.
Description
Technical Field
The invention relates to the field of safety detection of lithium ion batteries, in particular to a method for analyzing failure of a lithium ion battery.
Background
Lithium ion batteries have been rapidly developed in the field of consumer electronics because of their high energy density, good cycling performance, and lack of memory effect, and are the most widely used type of rechargeable batteries in portable electronic devices. With the development of lithium ion battery technology, it is gradually applied to the fields of electric vehicles, military and aerospace, etc.
However, the lithium ion battery can age and fail after long-time circulation, and even has potential safety hazard. From the current research, the abuse conditions of overcharge, short circuit, collision, overheating and the like all cause the safety hazard of the lithium ion battery, and a series of potential exothermic reactions inside the lithium ion battery can be caused. The surface of the carbon cathode of the battery is easy to deposit metal lithium to form dendrite, and the dendrite can penetrate through a diaphragm to cause internal short circuit when growing to a certain degree, so that the battery failure and even thermal runaway are caused. Studies have shown that high current, low temperature, high state of charge (including overcharge) is the primary cause of failure of carbon cathodes in lithium ion batteries. Under the above conditions, insufficient intercalation of lithium ions on the negative electrode is easily caused, and thus, the lithium ions are deposited on the surface, grow in the form of dendrites, and cause irreversible capacity fade or even internal short circuit. Therefore, the method for detecting the growth of the lithium dendrite of the carbon cathode of the lithium ion battery is found, thermal runaway caused by short circuit in the battery is prevented, and the method has certain practical significance.
At present, generally, whether lithium deposition occurs in a battery is mainly determined by direct disassembly, the battery after being circulated for a certain period is directly disassembled, and whether silvery white precipitates exist on a negative electrode piece is observed. This method is destructive and does not allow analysis or detection of the battery in use. A battery which possibly generates lithium dendrites is tested by R.Bouchet al (R.Bouchet al.an EIS Study of the antioxidant Li/PEO-Litfsi of a Li Polymer Battery. journal of the Electrochemical,2003,150: A1385-A1389) by using an alternating current impedance spectroscopy (EIS) method, and a corresponding fitting circuit is established according to the result. Tetsuya Osaka et al (Tetsuya Osaka et al, Proposalof novel equivalent circuit for electrochemical impedance analysis of commercial available lithium ion battery. journal of Power Sources,2012,205: 148A 3-A1486) modeled the system with appropriate equivalent circuits including various diffusion parameters due to different particle sizes of the anode material, solid electrolyte interface of the cathode surface, and electrochemical reaction and conductance portions, studied the residual errors resulting from data fitting for the various equivalent circuits used, analyzed the electrochemical impedance of the industrial lithium ion battery electrodes at different states of charge, and evaluated the proposed circuits. The method can accurately reflect the change of relevant parameters such as internal resistance and the like, so that the generation of the internal lithium dendrite can be predicted, but the method has more relevant parameters, a more complicated analysis process and larger workload during operation.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a lithium ion battery failure analysis method based on an alternating current impedance method, which analyzes the impedance change rule when lithium dendrite is deposited by an alternating current impedance test method, thereby judging the behavior of the ion battery that the ion battery fails due to generation of dendrite and providing a basis and a direction for the performance improvement of the battery at the later stage.
The technical scheme adopted for solving the technical problem is as follows:
1. a lithium ion battery failure analysis method based on an alternating current impedance method comprises the following steps:
1) selecting a brand new lithium ion battery as a sample to be tested, performing normal charge-discharge circulation by adopting a constant-current charge-discharge or constant-current-constant-voltage charge-discharge method after formation, and circulating to n1And (3) ending the cycle, wherein the battery SOC is between 80% and 100%;
2) for circulation to n1The battery of the ring is subjected to EIS test by using a CHI660e electrochemical workstation, and an analog equivalent circuit is constructed on the EIS test result, wherein the circuit is formed by serially connecting solution impedance, interface impedance, charge transfer and Warburg impedance, and the solution resistance is represented by Re; the interface impedance is caused by the solid electrolyte membrane on the surface of the negative electrode and is caused by the capacitance CSEIAnd a resistor RSEIParallel composition, denoted CSEI//RSEI(ii) a The charge transfer part is formed by connecting a charge transfer resistor Rct and Warburg impedance Zw in series and then connecting the charge transfer resistor Rct and Warburg impedance Zw in parallel with a constant phase element CPE, wherein Rct reflects the charge transfer step impedance of the electrode, Zw reflects the diffusion resistance of the electrode diffusion layer, and a resistor R is obtained based on an analog circuit fitting curveSEIN is cycled1The resistance of the ring is denoted RSEI,n1。
3) Continuing to charge and discharge the battery until n2And (3) repeating the step 2) to obtain the resistor RSEI,n2And then recycled to n3And (3) repeating the step 2) to obtain RSEI,n3By the above method, when the battery is subjected to charge-discharge cycle to niWhen enclosing, R is obtainedSEI,n1-RSEI,niA total of i RSEIA resistance value;
4) drawing RSEI,niWith respect to the curve of the number of cycles ni, R is obtainedSEIThe law of variation with cycle number, overall trend, RSEIGradually increases with the number of cycles, but at a certain number of cycles ngAfter, RSEIA sudden decrease, i.e. the cycleNumber of cycles ngAt the time when the short circuit in the dendrite is about to occur, the lithium dendrite in the battery destroys the SEI film.
Further, n1,n2,n3…niIs an arithmetic progression.
Further, the step 1) adopts self-made LiCoO2Coin cell battery of the MCMB system with LiCoO2As a positive electrode active material, MCMB as a negative electrode active material, 80% LiCoO2Mixing 10% of SuperP conductive carbon black and 10% of polyvinylidene fluoride (PVDF) binder, using N-methyl-2-pyrrolidone (NMP) as a solvent, performing ball milling to obtain slurry, and coating the slurry on an aluminum foil to obtain a positive pole piece; the preparation method comprises the steps of taking 90% of MCMB and 10% of PVDF as binders and NMP as solvents, coating the binders on copper foil after ball milling to obtain a negative pole piece, drying the positive pole piece and the negative pole piece, rolling the positive pole piece and the negative pole piece, stamping the positive pole piece and the negative pole piece into pole pieces with the diameter of 10mm, wherein the diaphragm material is a polypropylene diaphragm with the diameter of 16mm, and the electrolyte is 1M LiPF6Dissolving in mixed solvent system of Ethylene Carbonate (EC), diethyl carbonate (DEC) and dimethyl carbonate (DMC), assembling the battery in glove box inert gas environment, and performing formation by small current of C/10 multiplying power for 3 times.
Further, LiCoO is a positive electrode material2The equivalent mass ratio of the metal particles to the negative MCMB microspheres is 1.2:1, 1.3:1 or 1.4: 1.
Further, the overcharge cutoff voltage in the step 3) is 4.4V or 4.6V.
Further, the amplitude of the alternating current signal of the EIS test in the step 2) is 5mV, and the scanning frequency is 100kHz-0.01 Hz.
Compared with the prior art, the invention has the following beneficial effects:
the invention adopts an electrochemical alternating-current impedance test method, analyzes the relation between an alternating-current impedance spectrum signal and the internal environment of the battery, and can analyze the resistance change of the SEI film from the alternating-current impedance spectrum, thereby realizing the rapid and accurate prediction of the short circuit state in the dendritic crystal of the battery under the condition of not damaging the battery, and further evaluating the service life and the safety of the battery.
Drawings
FIG. 1 shows electrochemical impedance spectra (a) and RC simulation circuit (b) obtained from the test of the embodiment.
FIG. 2 is the diffusion resistance R of the 4.4V overcharged cell in example 1SEIIn relation to the number of cycles.
FIG. 3 is an optical microscope and scanning electron microscope image of a battery after being overcharged to 4.4V.
FIG. 4 is the diffusion resistance R of the overcharged cells of 4.4V and 4.6V in example 2SEIIn relation to the number of cycles.
FIG. 5 is the diffusion resistance R at different mass ratios in example 3SEIIn relation to the number of cycles.
Detailed Description
For ease of analysis, embodiments employ self-made LiCoO2Coin cell battery of the MCMB system with LiCoO2As a positive electrode active material, MCMB as a negative electrode active material, 80% LiCoO2Mixing 10% of SuperP conductive carbon black and 10% of polyvinylidene fluoride (PVDF) binder, using N-methyl-2-pyrrolidone (NMP) as a solvent, performing ball milling to obtain slurry, and coating the slurry on an aluminum foil to obtain a positive pole piece; and (3) ball-milling 90% of MCMB and 10% of PVDF binder by using NMP as a solvent, and coating the mixture on a copper foil to obtain a negative pole piece. And drying the positive and negative pole pieces, rolling and stamping to obtain the pole pieces with the diameter of 10 mm. The diaphragm material is a polypropylene diaphragm (Celgard) with the diameter of 16mm, and the electrolyte is 1M LiPF6Dissolving in mixed solvent system of Ethylene Carbonate (EC), diethyl carbonate (DEC) and dimethyl carbonate (DMC). After the cell was assembled in a glove box inert gas atmosphere (95% argon + 5% hydrogen), formation was carried out by 3 cycles of small current at C/10 rate.
Testing the battery by using a battery charge and discharge testing system, and performing an EIS test by using a CHI660e electrochemical workstation, wherein the amplitude of an alternating current signal in the EIS test is 5mV, the scanning frequency is 100kHz-0.01Hz, the EIS test is performed on the overcharged battery in a charging state, and a simulation equivalent circuit (shown in figure 1) is constructed, and is formed by serially connecting three parts of solution impedance, interface impedance, charge transfer and Warburg impedance, and the solution resistance is represented by Re; the interface impedance is mainly caused by the solid electrolyte membrane on the surface of the negative electrode and is caused by the capacitor CSEIAnd a resistor RSEIParallel composition, denoted CSEI//RSEI(ii) a The charge transfer section is connected in series with a Warburg impedance Zw by a charge transfer resistor Rct, which reflects the charge transfer step impedance of the electrode, and then connected in parallel with the constant phase element CPE, and Zw, which reflects the diffusion resistance of the electrode diffusion layer. The influence of the overcharge cycle number, the overcharge voltage and the anode-cathode ratio on the EIS result is respectively analyzed by adopting the analog equivalent circuit.
Example 1
The diffusion resistance R of the overcharged cell is obtained by testing the cell at the rate of 1C and taking 4.4V as the overcharge cut-off voltageSEIThe curve of R under overcharge of 4.4V as shown in FIG. 2SEIThe value increases rapidly with the increase of cycle number, and the surface layer diffusion resistance R is within the first 30 cycles of charge-discharge cycleSEIThe gradual increase from 44.56 omega after 10 weeks to 224.2 omega shows that under the overcharge condition of 4.4V cut-off voltage, the surface structure of the material particles is obviously changed, the SEI film is obviously thickened along with the increase of the cycle number, the film resistance is increased, and when the cycle is up to 40 weeks, RSEIThe value became 157.3 Ω, and suddenly decreased more than 30 weeks, after which RSEIAnd continued to increase to 585.4 omega at 50 weeks.
To verify the prediction, the occurrence of R is verifiedSEIAfter the battery with the inflection point of which the value begins to decrease is disassembled, the negative pole piece (shown in fig. 3, which are pictures taken under different scales) is observed through an optical microscope and a scanning electron microscope, and it can be found that cluster-shaped lithium dendrites appear on the surface of the pole piece, which indicates that the sudden decrease of the RSEI is caused by the lithium dendrites, and the growth of the lithium dendrites causes local damage to the SEI film, so that the diffusion resistance value of lithium ions on the surface layer is reduced. At the moment, the lithium dendrite only occurs in a local area, short circuit in the battery is not directly caused, the SEI film is repaired again in the subsequent cycle, the film resistance continues to increase, but the battery is failed soon afterwards. Thus, RSEIThe appearance of the inflection point suggests that lithium dendrites in the battery damage the SEI film, and the battery is about to generate short circuit in the dendrites.
Example 2
When fixing the positive electrode material LiCoO2When the equivalent mass ratio of the particles to the cathode MCMB microspheres is 1.2:1, the particles are mixed inThe battery is subjected to charge and discharge tests under different cut-off voltages of 4.4V and 4.6V. As a result, as shown in FIG. 4, when the charge cut-off voltage of the battery was set to 4.4V, the surface layer diffusion resistance gradually increased from 25.67. omega. to 74.04. omega. after 10 weeks in the first 30 weeks of the charge-discharge cycle, indicating that the SEI film gradually thickened during the cycle and R during the subsequent cyclesS EIThe value was reduced to 60.55 Ω; when the charge cut-off voltage of the battery is 4.6V, the diffusion impedance of the surface layer is obviously reduced when the battery is cycled for 20 weeks, which shows that the impedance of the lithium ion battery is increased along with the increase of the cut-off voltage in an overcharged state, but R isSEIThe inflection point at which the value begins to decrease occurs earlier, indicating that an internal short circuit has occurred earlier.
Example 3
When the battery charge cut-off voltage was set to 4.4V, LiCoO was added to the positive electrode material, respectively2When the battery is tested with the negative electrode MCMB microsphere equivalent mass ratio of 1.2:1, 1.3:1 and 1.4:1, the diffusion impedance of the surface layer of the battery is gradually increased in the charge-discharge cycle process (as shown in figure 5). When LiCoO is used2When the equivalent mass ratio of the metal oxide to the negative MCMB microspheres is 1.2:1 to 1.3:1, RSEIThe inflection point occurred at 40 weeks; when the mass ratio is 1.4:1, RSEIThe inflection point occurs at 30 weeks. It shows that the internal short circuit problem caused by lithium dendrite is intensified and the internal short circuit time is advanced along with the increase of the excessive proportion of the anode material.
Although exemplary embodiments of the present invention have been described for illustrative purposes, those skilled in the art will appreciate that various modifications, additions, substitutions and the like can be made in form and detail without departing from the scope and spirit of the invention as disclosed in the accompanying claims, all of which are intended to fall within the scope of the claims, and that various steps in the various sections and methods of the claimed product can be combined together in any combination. Therefore, the description of the embodiments disclosed in the present invention is not intended to limit the scope of the present invention, but to describe the present invention. Accordingly, the scope of the present invention is not limited by the above embodiments, but is defined by the claims or their equivalents.
Claims (6)
1. A lithium ion battery failure analysis method based on an alternating current impedance method comprises the following steps:
1) selecting a brand new lithium ion battery as a sample to be tested, performing normal charge-discharge circulation by adopting a constant-current charge-discharge or constant-current-constant-voltage charge-discharge method after formation, and circulating to n1And (3) ending the cycle, wherein the battery SOC is between 80% and 100%;
2) performing EIS test by using CHI660e electrochemical workstation, and constructing an analog equivalent circuit for EIS test results, wherein the circuit is formed by serially connecting solution impedance, interface impedance, charge transfer and Warburg impedance, and the solution resistance is represented by Re; the interface impedance is caused by the solid electrolyte membrane on the surface of the negative electrode and is caused by the capacitance CSEIAnd a resistor RSEIParallel composition, denoted CSEI//RSEI(ii) a The charge transfer part is formed by connecting a charge transfer resistor Rct and Warburg impedance Zw in series and then connecting the charge transfer resistor Rct and Warburg impedance Zw in parallel with a constant phase element CPE, wherein Rct reflects the charge transfer step impedance of the electrode, Zw reflects the diffusion resistance of the electrode diffusion layer, and a resistor R is obtained based on an analog circuit fitting curveSEIN is cycled1The resistance of the ring is denoted RSEI,n1；
3) Continuing to charge and discharge the battery until n2And (3) repeating the step 2) to obtain the resistor RSEI,n2And then recycled to n3And (3) repeating the step 2) to obtain RSEI,n3By the above method, when the battery is subjected to charge-discharge cycle to niWhen enclosing, R is obtainedSEI,n1-RSEI,niA total of i RSEIA resistance value;
4) drawing RSEI,niWith respect to the curve of the number of cycles ni, R is obtainedSEIThe law of variation with cycle number, overall trend, RSEIGradually increases with the number of cycles, but at a certain number of cycles ngAfter, RSEIA sudden decrease, i.e. the number of cycles ngAt the time when the short circuit in the dendrite is about to occur, the lithium dendrite in the battery destroys the SEI film.
2. The method of claim 1, wherein: the step 1) adopts self-made LiCoO2Coin cell battery of the MCMB system with LiCoO2As a positive electrode active material, MCMB as a negative electrode active material, 80% LiCoO2Mixing 10% of SuperP conductive carbon black and 10% of polyvinylidene fluoride (PVDF) binder, using N-methyl-2-pyrrolidone (NMP) as a solvent, performing ball milling to obtain slurry, and coating the slurry on an aluminum foil to obtain a positive pole piece; the preparation method comprises the steps of taking 90% of MCMB and 10% of PVDF as binders and NMP as solvents, coating the binders on copper foil after ball milling to obtain a negative pole piece, drying the positive pole piece and the negative pole piece, rolling the positive pole piece and the negative pole piece, stamping the positive pole piece and the negative pole piece into pole pieces with the diameter of 10mm, wherein the diaphragm material is a polypropylene diaphragm with the diameter of 16mm, and the electrolyte is 1M LiPF6Dissolving in mixed solvent system of Ethylene Carbonate (EC), diethyl carbonate (DEC) and dimethyl carbonate (DMC), assembling the battery in glove box inert gas environment, and performing formation by small current of C/10 multiplying power for 3 times.
3. The method of claim 2, wherein: positive electrode material LiCoO2The equivalent mass ratio of the metal particles to the negative MCMB microspheres is 1.2:1, 1.3:1 or 1.4: 1.
4. A method according to any one of claims 1-3, characterized in that: the overcharge cutoff voltage in the step 3) is 4.4V or 4.6V.
5. A method according to any one of claims 1-3, characterized in that: the amplitude of the alternating current signal tested by the EIS in the step 2) is 5mV, and the scanning frequency is 100kHz-0.01 Hz.
6. The method of claim 1, wherein: n is1,n2,n3…niIs an arithmetic progression.
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